CN101187606A - Metallographic etched process for displaying G Cr15 original austenite grain border - Google Patents

Metallographic etched process for displaying G Cr15 original austenite grain border Download PDF

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Publication number
CN101187606A
CN101187606A CNA200710193134XA CN200710193134A CN101187606A CN 101187606 A CN101187606 A CN 101187606A CN A200710193134X A CNA200710193134X A CN A200710193134XA CN 200710193134 A CN200710193134 A CN 200710193134A CN 101187606 A CN101187606 A CN 101187606A
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Prior art keywords
sample
mordant
polishing
milliliters
alcohol
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CNA200710193134XA
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Chinese (zh)
Inventor
梁华
雷建中
叶健熠
梅亚莉
梁林霞
仇亚军
高元安
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Luoyang Bearing Science and Technology Co Ltd
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Luoyang Bearing Science and Technology Co Ltd
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Priority to CNA200710193134XA priority Critical patent/CN101187606A/en
Publication of CN101187606A publication Critical patent/CN101187606A/en
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Abstract

A metallographic corrosion method for displaying GCr15 original austenitic grain boundaries, which comprises following steps: adding picric acid 5g into distilled water100ml and mixing continuously, then adding sodium dodecyl benzene sulfonate 5ml 50% and mixing, finally adding ferric chloride 2g, and using after placing for 24 hours. A sample is grinded roughly, grinded finely, polished, cleared, blow-dried, immersed into caustic erodent for 2-5 minutes according to a normal method under quenching tempering condition until etched surface is changed into silver grey, washed with flowing water, cleaned with alcohol 95%, and blow-dried. If the sample is over-corroded, polishing paste W0.5-1.0 or metallographic polishing agent 0.5-1.0 is added on silk polishing cloth, the sample is polished slightly with hands, then cleaned with alcohol 95%, and dried. According to practical condition, grain granularity measurement can adopt methods of picture contrast, grid, intercept, quantitative metallography and the like to assess according to relevant standards.

Description

A kind of etching pit method that shows GCr15 original austenite grains border
Technical field
The invention belongs to the heat treatment technics field, specially refer to the etching pit method on a kind of GCr15 of demonstration original austenite grains border.
Background technology
The austenite crystal refinement of steel can improve the intensity of steel effectively.Crystal grain is more tiny, to be subjected to the inhibition of crystal boundary bigger in the expansion of plastic yield under the effect of external force, therefore help improving the intensity of steel, on the other hand, because grain refinement can make wide-angle and low-angle crystal boundary increase again, crackle passes through the energy that crystal boundary consumes to be increased, the propagation rate of crack is slowed down, and simultaneously, austenite grain size also directly has influence on martensitic form, substructure and toughness.The austenite crystal refinement, the also corresponding raising of its toughness.
For many years, thermal treatment worker and scientific research personnel have done a large amount of work for GCr15 bearing steel original austenite grains degree to intensity, toughness and the Fatigue Life of steel both at home and abroad, many achievements in research have also been obtained, but to adopting which kind of etching pit method to show that GCr15 bearing steel original austenite grains border studies not enough, the caustic solution that has can not clearly show crystal boundary, the method that has is too loaded down with trivial details and lose time, the heating that then needs that has could show, and the result is also very undesirable sometimes.Therefore, brought inconvenience and difficult for the refinement of GCr15 bearing steel original austenite grains.
Summary of the invention
At the problems referred to above, the invention provides the etching pit method on a kind of GCr15 of demonstration original austenite grains border, the caustic solution that is adopted can realize showing well at normal temperatures the GCr15 bearing steel original austenite grains border after the tempering of quenching, test condition for the grain refinement treatment process of research bearing steel is provided convenience also provides good foundation for later bearing steel thermal treatment standard revise simultaneously.
For achieving the above object, the present invention has adopted following technical scheme:
The etching pit method on described demonstration GCr15 original austenite grains border comprises mordant prescription, mordant preparation and etching pit three steps, and each step is as follows:
I, mordant prescription
100 milliliters of picric acid 5 grams, 5 milliliters of neopelex 50%W, ferric trichloride 2 grams, distilled water;
II, mordant preparation
1) in 100 milliliters distilled water, adds the picric acid of 5 grams and constantly stirring;
2) neopelex that adds 5 milliliters 50%W in picric solution also constantly stirs;
3) in picric acid that configures and neopelex solution, add 2 ferric trichlorides that restrain;
4) mordant that configures is placed after 24 hours and is used;
III, etching pit
1) sample is roughly ground, fine grinding, polishing, is cleaned and dry up according to conventional method under the Annealed Strip of quenching;
2) sample for preparing is immersed in the mordant, corrode 2~5 minutes, the erosional surface of sample should be placed up and constantly stir or with the continuous wiping of cotton, so that corrosion is even, till erosional surface becomes silver gray;
3) sample that will corrode washes with circulating water, and dries up with 95% alcohol wash;
4) if the sample excessive corrosion can add the antiscuffing paste of W0.5~1.0 or 0.5~1.0 metallurgical polishing agent and carry out slight polishing with hand, and then dry up with the cleaning of 95% alcohol on the real silk polishing cloth;
5) mensuration of grain size can select to adopt methods such as picture pairing comparision, gridding method, intercept method and quantitative metallography to evaluate according to relevant criterion according to actual conditions.
Because adopt aforesaid technical scheme, the present invention has following superiority:
1, do not need heating, can carry out at normal temperatures;
2, not only economy but also save time;
3, can clearly demonstrate the border of GCr15 bearing steel original austenite grains under the Annealed Strip of quenching;
4, reappearance is preferably arranged.
Embodiment
The etching pit method on demonstration GCr15 original austenite grains of the present invention border comprises mordant prescription, mordant preparation and etching pit three steps, and each step is as follows:
I, mordant prescription
100 milliliters of picric acid 5 grams, 5 milliliters of dodecylbenzene sulfonic acid 50%W, ferric trichloride 2 grams, distilled water;
II, mordant preparation
1) in 100 milliliters distilled water, adds the picric acid of 5 grams and constantly stirring;
2) neopelex that adds 5 milliliters 50%W in picric solution also constantly stirs;
3) in picric acid that configures and neopelex solution, add 2 ferric trichlorides that restrain;
4) mordant that configures is placed after 24 hours and is used;
III, etching pit are divided into following 3 kinds of embodiment:
Embodiment 1
1) sample is roughly ground, fine grinding, polishing, is cleaned and dry up according to conventional method under the Annealed Strip of quenching;
2) sample for preparing is immersed in the mordant, corrode 2 minutes, the erosional surface of sample should be placed up and constantly stir or with the continuous wiping of cotton, so that corrosion is even, till erosional surface becomes silver gray;
3) sample that will corrode washes with circulating water, and dries up with 95% alcohol wash;
4) if the sample excessive corrosion can add the antiscuffing paste of W0.5~1.0 or the metallurgical polishing agent of W0.5~1.0 and carry out slight polishing with hand, and then dry up with the cleaning of 95% alcohol on the real silk polishing cloth;
5) mensuration of grain size can select to adopt methods such as picture pairing comparision, gridding method, intercept method and quantitative metallography to evaluate according to relevant criterion according to actual conditions.
This caustic solution has fast, the advantages of simple operation of corrosion speed, may exist austenite grain boundary to manifest incomplete situation, is not suitable for metallographic and takes pictures, but can not have influence on evaluation result.
Embodiment 2
1) sample is roughly ground, fine grinding, polishing, is cleaned and dry up according to conventional method under the Annealed Strip of quenching;
2) sample for preparing is immersed in the mordant, corrode 3~4 minutes, the erosional surface of sample should be placed up and constantly stir or with the continuous wiping of cotton, so that corrosion is even, till erosional surface becomes silver gray;
3) sample that will corrode washes with circulating water, and dries up with 95% alcohol wash;
4) if the sample excessive corrosion can add the antiscuffing paste of W0.5~1.0 or the metallurgical polishing agent of W0.5~1.0 and carry out slight polishing with hand, and then dry up with the cleaning of 95% alcohol on the real silk polishing cloth;
5) mensuration of grain size can select to adopt methods such as picture pairing comparision, gridding method, intercept method and quantitative metallography to evaluate according to relevant criterion according to actual conditions.
This caustic solution has the moderate advantage of corrosion speed, and austenite grain boundary can show fully that suitable metallographic is taken pictures and graded.
Embodiment 3
1) sample is roughly ground, fine grinding, polishing, is cleaned and dry up according to conventional method under the Annealed Strip of quenching;
2) sample for preparing is immersed in the mordant, corrode 5 minutes, the erosional surface of sample should be placed up and constantly stir or with the continuous wiping of cotton, so that corrosion is even, till erosional surface becomes silver gray;
3) sample that will corrode washes with circulating water, and dries up with 95% alcohol wash;
4) if the sample excessive corrosion can add the antiscuffing paste of W0.5~1.0 or the metallurgical polishing agent of W0.5~1.0 and carry out slight polishing with hand, and then dry up with the cleaning of 95% alcohol on the real silk polishing cloth;
5) mensuration of grain size can select to adopt methods such as picture pairing comparision, gridding method, intercept method and quantitative metallography to evaluate according to relevant criterion according to actual conditions.
The suitable austenite crystal of this caustic solution is tiny, the difficult sample to differentiate of crystal boundary.

Claims (1)

1. etching pit method that shows GCr15 original austenite grains border is characterized in that: this method comprises mordant prescription, mordant preparation and etching pit three steps, and each step is as follows:
I, mordant prescription
100 milliliters of picric acid 5 grams, 5 milliliters of neopelex 50%W, ferric trichloride 2 grams, distilled water;
II, mordant preparation
1) in 100 milliliters distilled water, adds the picric acid of 5 grams and constantly stirring;
2) neopelex that adds 5 milliliters 50%W in picric solution also constantly stirs;
3) in picric acid that configures and neopelex solution, add 2 ferric trichlorides that restrain;
4) mordant that configures is placed after 24 hours and is used;
III, etching pit
1) sample is roughly ground, fine grinding, polishing, is cleaned and dry up according to conventional method under the Annealed Strip of quenching;
2) sample for preparing is immersed in the mordant, corrode 2~5 minutes, the erosional surface of sample should be placed up and constantly stir or with the continuous wiping of cotton, so that corrosion is even, till erosional surface becomes silver gray;
3) sample that will corrode washes with circulating water, and dries up with 95% alcohol wash;
4) if the sample excessive corrosion can add the antiscuffing paste of W0.5~1.0 or 0.5~1.0 metallurgical polishing agent and carry out slight polishing with hand, and then dry up with the cleaning of 95% alcohol on the real silk polishing cloth;
5) mensuration of grain size can select to adopt methods such as picture pairing comparision, gridding method, intercept method and quantitative metallography to evaluate according to relevant criterion according to actual conditions.
CNA200710193134XA 2007-11-30 2007-11-30 Metallographic etched process for displaying G Cr15 original austenite grain border Pending CN101187606A (en)

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Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100594372C (en) * 2008-08-26 2010-03-17 武汉钢铁(集团)公司 Display and quantitative detection method of residual austenite or island-form martensite-austenite in TRIP steel
CN101880881A (en) * 2010-06-13 2010-11-10 西南大学 High aluminum zinc alloy etching agent and use method thereof
CN102095623A (en) * 2011-01-16 2011-06-15 首钢总公司 Preparation method for silicon steel metallographic sample
CN102103051A (en) * 2011-01-13 2011-06-22 马鞍山钢铁股份有限公司 Medium-high carbon steel actual grain size developer and developing method
CN102183402A (en) * 2011-04-01 2011-09-14 天津万立鑫晟新材料技术研究院有限公司 Method for preparing grain size test sample of high-chromium cast iron
CN101672738B (en) * 2009-09-15 2011-10-05 西部金属材料股份有限公司 Sample processing method for observing nuclear silver-indium-cadmium control rod metallographic structure
CN102517586A (en) * 2011-12-26 2012-06-27 上海锅炉厂有限公司 Corrosive agent for displaying 9% Cr steel original austenite grain boundary and application thereof
CN103344532A (en) * 2013-06-19 2013-10-09 武汉理工大学 Rapid metallographic determination method for grain size of GCr15 steel bearing assembly
CN103499480A (en) * 2013-09-30 2014-01-08 南昌航空大学 Metallographic phase corrosion method displaying austenitic stainless steel grain boundary
CN103512792A (en) * 2013-10-15 2014-01-15 北京科技大学 Method for displaying GCr15SiMn steel original austenite crystal grains in pearlite state
CN103592170A (en) * 2013-11-04 2014-02-19 南京钢铁股份有限公司 Detection etching solution and detection method for steel austenite grain size and dendrite segregation
CN103614662A (en) * 2013-11-26 2014-03-05 南京钢铁股份有限公司 Preparation method of austenite actual grain size detection sample of wear-resistant steel
CN103698192A (en) * 2013-12-21 2014-04-02 哈尔滨锅炉厂有限责任公司 Chemical etching liquid and method for displaying raw stainless steel austenite grain boundary
CN103712844A (en) * 2013-12-16 2014-04-09 贵州安大航空锻造有限责任公司 Corrosion method for displaying Cr13-type martensitic stainless steel grain size
CN104535399A (en) * 2014-12-23 2015-04-22 北京科技大学 Method for displaying original austenite grains in steel for bearing ring of shield tunneling machine
CN106017760A (en) * 2016-05-10 2016-10-12 攀钢集团研究院有限公司 Method for detecting residual stress of steel rail
CN106370499A (en) * 2016-08-25 2017-02-01 鹰普(中国)有限公司 Austenite crystal boundary corrosion method after carburizing and quenching
CN107621398A (en) * 2017-08-23 2018-01-23 包头钢铁(集团)有限责任公司 A kind of method for showing weather resisting steel Q450NQR1 original austenite crystal boundaries
CN107761100A (en) * 2016-08-18 2018-03-06 宝山钢铁股份有限公司 Medium high carbon high-strength steel prior austenite grain size visualizingre agent and its application method
CN108535080A (en) * 2018-03-27 2018-09-14 华电国际电力股份有限公司技术服务中心 A kind of metallurgical polishing method for making sample
CN110118779A (en) * 2019-05-13 2019-08-13 中天钢铁集团有限公司 A kind of the dendrite corrosive agent and display methods of the heat resisting steel containing chromium
CN110132962A (en) * 2019-04-24 2019-08-16 东方电气集团东方锅炉股份有限公司 A kind of original austenite crystal prevention display methods of boiler and pressure vessel tempering bainite steel
CN112195471A (en) * 2020-09-16 2021-01-08 上海交通大学 Corrosive agent for lath martensite steel original austenite grain boundary, preparation method and corrosion method
CN112629983A (en) * 2020-12-16 2021-04-09 本钢板材股份有限公司 Medium carbon steel actual grain size corrosive agent and corrosion experiment method
CN113063707A (en) * 2021-03-12 2021-07-02 浙江美力科技股份有限公司 Corrosion method for prior austenite grain size of tempered troostite and martensite structure
WO2021135226A1 (en) * 2019-12-31 2021-07-08 北京科技大学 Method for displaying austenite grains of spring steel

Cited By (31)

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Publication number Priority date Publication date Assignee Title
CN100594372C (en) * 2008-08-26 2010-03-17 武汉钢铁(集团)公司 Display and quantitative detection method of residual austenite or island-form martensite-austenite in TRIP steel
CN101672738B (en) * 2009-09-15 2011-10-05 西部金属材料股份有限公司 Sample processing method for observing nuclear silver-indium-cadmium control rod metallographic structure
CN101880881A (en) * 2010-06-13 2010-11-10 西南大学 High aluminum zinc alloy etching agent and use method thereof
CN102103051A (en) * 2011-01-13 2011-06-22 马鞍山钢铁股份有限公司 Medium-high carbon steel actual grain size developer and developing method
CN102095623A (en) * 2011-01-16 2011-06-15 首钢总公司 Preparation method for silicon steel metallographic sample
CN102183402A (en) * 2011-04-01 2011-09-14 天津万立鑫晟新材料技术研究院有限公司 Method for preparing grain size test sample of high-chromium cast iron
CN102183402B (en) * 2011-04-01 2013-01-16 天津万立鑫晟新材料技术研究院有限公司 Method for preparing grain size test sample of high-chromium cast iron
CN102517586B (en) * 2011-12-26 2013-11-27 上海锅炉厂有限公司 Corrosive agent for displaying 9% Cr steel original austenite grain boundary and application thereof
CN102517586A (en) * 2011-12-26 2012-06-27 上海锅炉厂有限公司 Corrosive agent for displaying 9% Cr steel original austenite grain boundary and application thereof
CN103344532A (en) * 2013-06-19 2013-10-09 武汉理工大学 Rapid metallographic determination method for grain size of GCr15 steel bearing assembly
CN103499480A (en) * 2013-09-30 2014-01-08 南昌航空大学 Metallographic phase corrosion method displaying austenitic stainless steel grain boundary
CN103499480B (en) * 2013-09-30 2016-03-30 南昌航空大学 A kind of etching pit method showing austenitic stainless steel grain boundary
CN103512792A (en) * 2013-10-15 2014-01-15 北京科技大学 Method for displaying GCr15SiMn steel original austenite crystal grains in pearlite state
CN103512792B (en) * 2013-10-15 2015-12-02 北京科技大学 The method of the GCr15SiMn steel original austenite grains of display pearlite state
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CN103592170B (en) * 2013-11-04 2016-01-20 南京钢铁股份有限公司 The autstenitic grain size of steel and dendritic segregation detect etching solution and detection method
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CN103698192A (en) * 2013-12-21 2014-04-02 哈尔滨锅炉厂有限责任公司 Chemical etching liquid and method for displaying raw stainless steel austenite grain boundary
CN104535399A (en) * 2014-12-23 2015-04-22 北京科技大学 Method for displaying original austenite grains in steel for bearing ring of shield tunneling machine
CN106017760A (en) * 2016-05-10 2016-10-12 攀钢集团研究院有限公司 Method for detecting residual stress of steel rail
CN107761100A (en) * 2016-08-18 2018-03-06 宝山钢铁股份有限公司 Medium high carbon high-strength steel prior austenite grain size visualizingre agent and its application method
CN106370499A (en) * 2016-08-25 2017-02-01 鹰普(中国)有限公司 Austenite crystal boundary corrosion method after carburizing and quenching
CN107621398A (en) * 2017-08-23 2018-01-23 包头钢铁(集团)有限责任公司 A kind of method for showing weather resisting steel Q450NQR1 original austenite crystal boundaries
CN108535080A (en) * 2018-03-27 2018-09-14 华电国际电力股份有限公司技术服务中心 A kind of metallurgical polishing method for making sample
CN110132962A (en) * 2019-04-24 2019-08-16 东方电气集团东方锅炉股份有限公司 A kind of original austenite crystal prevention display methods of boiler and pressure vessel tempering bainite steel
CN110118779A (en) * 2019-05-13 2019-08-13 中天钢铁集团有限公司 A kind of the dendrite corrosive agent and display methods of the heat resisting steel containing chromium
WO2021135226A1 (en) * 2019-12-31 2021-07-08 北京科技大学 Method for displaying austenite grains of spring steel
CN112195471A (en) * 2020-09-16 2021-01-08 上海交通大学 Corrosive agent for lath martensite steel original austenite grain boundary, preparation method and corrosion method
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CN113063707A (en) * 2021-03-12 2021-07-02 浙江美力科技股份有限公司 Corrosion method for prior austenite grain size of tempered troostite and martensite structure

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