CN110118779A - A kind of the dendrite corrosive agent and display methods of the heat resisting steel containing chromium - Google Patents

A kind of the dendrite corrosive agent and display methods of the heat resisting steel containing chromium Download PDF

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Publication number
CN110118779A
CN110118779A CN201910392766.1A CN201910392766A CN110118779A CN 110118779 A CN110118779 A CN 110118779A CN 201910392766 A CN201910392766 A CN 201910392766A CN 110118779 A CN110118779 A CN 110118779A
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CN
China
Prior art keywords
heat resisting
resisting steel
metallographic
dendrite
chromium
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Pending
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CN201910392766.1A
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Chinese (zh)
Inventor
万文华
戴林荣
许加陆
屈志东
孙宏飞
仲红刚
李仁兴
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Changzhou Bangyi Iron And Steel Co Ltd
Zenith Steel Group Co Ltd
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Changzhou Bangyi Iron And Steel Co Ltd
Zenith Steel Group Co Ltd
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Application filed by Changzhou Bangyi Iron And Steel Co Ltd, Zenith Steel Group Co Ltd filed Critical Changzhou Bangyi Iron And Steel Co Ltd
Priority to CN201910392766.1A priority Critical patent/CN110118779A/en
Publication of CN110118779A publication Critical patent/CN110118779A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84Systems specially adapted for particular applications
    • G01N21/88Investigating the presence of flaws or contamination
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2866Grinding or homogeneising

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Investigating And Analyzing Materials By Characteristic Methods (AREA)

Abstract

The present invention provides the dendrite corrosive agent and display methods of a kind of heat resisting steel containing chromium, including heat resisting steel metallographic specimen to carry out mechanical lapping, mechanical polishing, dendrite burn into flushing drying and micro- sem observation etc..Metallographic etching agent of the invention is the mixed solution for being saturated bitter taste aqueous acid and iron chloride solvent, the iron chloride aqueous solvent that the metallographic etching agent is 20%~30% by saturation bitter taste aqueous acid, mass percent is 10:1 according to volume ratio, the mixed liquor that total volume is 100ml is configured, along with neopelex configures.The arborescent structure of the heat resisting steel metallographic specimen containing 9% chromium can be clearly showed that using arborescent structure display methods of the invention, and then is conducive to the growth length of measurement dendrite.

Description

A kind of the dendrite corrosive agent and display methods of the heat resisting steel containing chromium
Technical field
The present invention relates to a kind of dendrite of steel to observe experimental technique, more particularly to is the heat resisting steel of 9% chromium containing mass fraction Corrosive agent, the caustic solution of metallographic specimen and the display methods of dendrite of metallographic specimen dendrite observation.
Technical background
The material properties such as the internal organizational structure and hardness, intensity, ductility of metal material have direct and close connection System, and the dendritic growth form of metal material can be directly acquainted with metal from the sequence for being molten to solidification, the enrichment of element, hot tearing The generation etc. of line.Metallographic refers to physical state and chemical state of the various composition of metal or alloy inside metal or alloy. Metallography microscope observation can be carried out to the tissue of different metal or alloy, dendrite etc. using metallography microscope display methods.Wherein, right Dendrite, which is observed, to be first had to using chemical erosion method, and branch when solidifying metal or alloy using suitable metallographic etching agent Crystalline substance is shown, then observes its direction of growth, and so as to carry out subsequent research, including but not limited to power spectrum, electronics is visited The analysis means such as needle or in-situ metal observation detection elements segregation.
However, comparing in the prior art the effect for carrying out the micro- display of dendrite containing the heat resisting steel that mass fraction is 9% chromium Difference, and its method is comparatively laborious with step, and corrosive agent has strong acid solution.If chromium is added to inside steel, greatly enhance The corrosion resistance of steel, which results in the overlong time of corrosion, many using the affected factor of electrolytic etching, and corrodes The more difficult grasp of degree.It is harsh to heat strong acid etching condition, etching time is long, is unfavorable for clearly showing dendrite, is unfavorable for advising greatly Mould industrial application.
Therefore, suitable dendrite corrosive agent how is selected, how the corrosion containing the heat resisting steel that mass fraction is 9% chromium is imitated Fruit reaches more preferably, and clear dendrite how to be allowed to show, just seems very necessary to facilitate subsequent research.
Summary of the invention
What the purpose of the present invention is to provide a kind of corrosive effect, good and etching time was accurately controlled is containing mass fraction Dendrite corrosive agent, sample caustic solution and the dendrite display methods of the heat resisting steel of 9% chromium.
The purpose of the present invention is achieved through the following technical solutions: a kind of method for displaying metallographic structure, comprising: is provided and is contained matter Measure the heat resisting steel metallographic specimen that score is 9% chromium;Mechanical lapping is carried out to the metallographic specimen;To grinding metallographic specimen just into Row mechanical polishing;Metallographic specimen after polishing is immersed into metallographic etching agent, and Heating Water corrodes in 85 DEG C of water-bath furnace, institute Stating metallographic etching agent is the mixed solution for being saturated picric acid and iron chloride, additional a small amount of neopelex;After corroding Metallographic specimen rinse, drying;It is finally putting into the dendrite of sample described in optical microphotograph sem observation.
Further, saturation picric acid solution and quality hundred of the metallographic etching agent by mass percent for 4%~5% Dividing than the ferric chloride solution for 20%~30% is 10:1 according to volume ratio, and additional 3g neopelex is formulated.
Further, the metallographic specimen immerses in the metallographic etching agent, and corrosion is heated in 85 DEG C of water-bath furnace 60s~80s.
Further, it needs to rinse 3s~5s with circulating water after the metallographic specimen corrosion.
Further, dry with alcohol hydro-peening after the metallographic specimen rinses, it is repeated 3 times.
Compared with prior art, the present invention has the effect that using above-mentioned technical method, available to contain mass fraction For the caustic solution of the heat resisting steel dendrite of 9% chromium, and corrosion efficiency is high, and Corrosion results are good, and repeatability is high.
Detailed description of the invention
Fig. 1 is the metallographic specimen photo containing the heat resisting steel that mass fraction is 9% chromium before corrosion;
Fig. 2 is to use the corrosion of 1 corrosive agent of embodiment containing mass fraction for the dendrite morphology figure after the heat resisting steel of 9% chromium;
Fig. 3 is to use the corrosion of 1 corrosive agent of comparative example containing mass fraction for the dendrite morphology figure after the heat resisting steel of 9% chromium.
Specific embodiment
In order to enable those skilled in the art to better understand the present invention, below with reference to specific embodiment to of the invention Technical solution is described in detail.
Embodiment 1
It is saturation picric acid solution and mass percent that metallographic etching agent in the present embodiment, which is 100ml by mass percent, It according to volume ratio is 10:1 for 20%~30% ferric chloride solution, the mixed liquor that configuration total volume is 100ml, additional 3g 12 Sodium alkyl benzene sulfonate is formulated.Using the metallographic etching agent to the heat resisting steel metallographic specimen for containing mass percent being 9% chromium The corrosion for carrying out pine-tree structure can greatly improve corrosion efficiency and corrosion display effect.Corrosive agent configuration is simple, utilizes water Bath heating corrosion, corrosive agent volatile quantity is few, and one group of corrodible sample size of corrosive agent is more.
The metallographic specimen containing the heat resisting steel that mass fraction is 9% chromium is provided, as shown in Figure 1, the metallographic specimen has carried out Mechanical lapping, mechanical polishing.Then, the metallographic specimen after mechanical polishing is immersed into above-mentioned metallographic etching agent, and is put into 85 DEG C of water Corrode 65s in liquid furnace, take out sample, rinses 5s with circulating water, it is then dry with alcohol hydro-peening, it is repeated 5 times to get after corrosion It is the heat resisting steel dendrite sample of 9% chromium containing mass fraction, finally reuses optical microscopy and carry out microexamination, it can be observed that The pine-tree structure of Fig. 2.So can clearly show that containing mass fraction be the heat-resisting of 9% chromium with technical solution of the present invention The pine-tree structure of steel, so as to carry out subsequent research, including but not limited to power spectrum, the analysis means such as electron probe.
Comparative example 1
The configuration method with embodiment 1 of the corrosive agent compared with Example 1 of comparative example 1 is consistent, but it is molten that picric acid is added The mass percent of liquid is 2%, i.e. unsaturation picric acid solution, other ingredients are identical.
In order to compare the effect of above-mentioned corrosive agent, provide same as Example 1 containing the heat resisting steel that mass fraction is 9% chromium Metallographic specimen re-starts mechanical lapping, mechanical polishing.Then sample is immersed in 1 corrosive agent of comparative example, and is put into 85 DEG C of water Corrode 65s in liquid furnace, take out sample, rinses 5s with circulating water, it is then dry with alcohol hydro-peening, it is repeated 5 times, it is aobvious to reuse optics Micro mirror carries out microexamination.The etch figures observed are as shown in Figure 3.If can be seen that the picric acid in corrosive agent is unsaturation Solution, sample dendrite corrosive effect be it is unconspicuous, what can only be obscured sees a dendrite, and secondary dendrite show it is fuzzy, no Conducive to dendrite length, gap etc. is for statistical analysis.
The foregoing is merely some embodiments of the invention, the embodiment being not all of, ordinary skill people Any equivalent variation that member takes the technology of the present invention method by reading description of the invention, is right of the invention It is required that being covered.

Claims (6)

1. a kind of dendrite corrosive agent of heat resisting steel containing chromium, it is characterised in that: the metallographic etching agent by saturation bitter taste aqueous acid, The iron chloride aqueous solvent that mass percent is 20%~30% is 10:1 mixing according to volume ratio, then ten are added into mixed liquor Dialkyl benzene sulfonic acids sodium configures.
2. the dendrite corrosive agent of the heat resisting steel containing chromium described in claim 1, it is characterised in that: neopelex additional amount is 3g is added in every 100mL mixed liquor.
3. the dendrite corrosive agent of the heat resisting steel containing chromium described in claim 1, it is characterised in that: the chrome-bearing steel is containing mass fraction The heat resisting steel of 9% chromium.
4. a kind of arborescent structure display methods of heat resisting steel containing chromium, which is characterized in that provide the heat resisting steel metallographic containing 9% chromium and try Sample carries out mechanical lapping to the metallographic specimen, the metallographic specimen after grinding is mechanically polished;By the metallographic examination after polishing Sample immerses the described in any item corrosive agent of claim 1-3 and carries out etching pit, and the metallographic specimen after corrosion is rinsed drying, is used The arborescent structure of metallographic specimen described in optical microphotograph sem observation.
5. the arborescent structure display methods of the heat resisting steel containing chromium as claimed in claim 4, which is characterized in that the metallographic specimen immerses In the metallographic etching agent, and heating water bath corrodes 60s~80s in 85 DEG C of water-bath furnace.
6. the arborescent structure display methods of the heat resisting steel containing chromium as claimed in claim 4, which is characterized in that the metallographic specimen corrosion After need to rinse 3s~5s with flowing clear water, it is dry with alcohol hydro-peening after flushing, be repeated 3 times.
CN201910392766.1A 2019-05-13 2019-05-13 A kind of the dendrite corrosive agent and display methods of the heat resisting steel containing chromium Pending CN110118779A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114855168A (en) * 2022-05-24 2022-08-05 洛阳金鹭硬质合金工具有限公司 Corrosive agent for displaying undissolved high alloy phase in steel and metallographic phase display method

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101187606A (en) * 2007-11-30 2008-05-28 洛阳轴研科技股份有限公司 Metallographic etched process for displaying G Cr15 original austenite grain border
CN103454187A (en) * 2013-08-27 2013-12-18 宁夏共享集团有限责任公司 Method for displaying original austenite grain boundary of tempering bainite structure at room temperature
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
CN105547796A (en) * 2015-12-21 2016-05-04 中车戚墅堰机车车辆工艺研究所有限公司 A metallographic phase corrosive used for displaying a tempered sorbite tissue austenite crystal boundary and a corroding method
CN107236955A (en) * 2017-06-16 2017-10-10 马鞍山钢铁股份有限公司 A kind of metallographic etching agent and the metallographic phase display method for showing crackle microscopic structure
CN107523833A (en) * 2017-08-22 2017-12-29 河南科技大学 A kind of metallographic etching agent and its application in terms of carbide, crystal boundary in showing steel
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
CN109612809A (en) * 2018-11-22 2019-04-12 包头钢铁(集团)有限责任公司 A method of display high corrosion resistant type weathering steel S450EW original austenite crystal boundary

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101187606A (en) * 2007-11-30 2008-05-28 洛阳轴研科技股份有限公司 Metallographic etched process for displaying G Cr15 original austenite grain border
CN103454187A (en) * 2013-08-27 2013-12-18 宁夏共享集团有限责任公司 Method for displaying original austenite grain boundary of tempering bainite structure at room temperature
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
CN105547796A (en) * 2015-12-21 2016-05-04 中车戚墅堰机车车辆工艺研究所有限公司 A metallographic phase corrosive used for displaying a tempered sorbite tissue austenite crystal boundary and a corroding method
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
CN107236955A (en) * 2017-06-16 2017-10-10 马鞍山钢铁股份有限公司 A kind of metallographic etching agent and the metallographic phase display method for showing crackle microscopic structure
CN107523833A (en) * 2017-08-22 2017-12-29 河南科技大学 A kind of metallographic etching agent and its application in terms of carbide, crystal boundary in showing steel
CN109612809A (en) * 2018-11-22 2019-04-12 包头钢铁(集团)有限责任公司 A method of display high corrosion resistant type weathering steel S450EW original austenite crystal boundary

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刘哲: "《金属材料基础实验指导书》", 30 April 2015, 天津大学出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114855168A (en) * 2022-05-24 2022-08-05 洛阳金鹭硬质合金工具有限公司 Corrosive agent for displaying undissolved high alloy phase in steel and metallographic phase display method
CN114855168B (en) * 2022-05-24 2024-04-16 洛阳金鹭硬质合金工具有限公司 Corrosive agent for displaying undissolved high alloy phase in steel and metallographic display method

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Application publication date: 20190813