CN109023498A - For observing the metallographic etching agent and its application method of γ ' phase in Ni-based and ferronickel based high-temperature alloy - Google Patents
For observing the metallographic etching agent and its application method of γ ' phase in Ni-based and ferronickel based high-temperature alloy Download PDFInfo
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- CN109023498A CN109023498A CN201810909774.4A CN201810909774A CN109023498A CN 109023498 A CN109023498 A CN 109023498A CN 201810909774 A CN201810909774 A CN 201810909774A CN 109023498 A CN109023498 A CN 109023498A
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- phase
- alloy
- ferronickel
- observing
- etching agent
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
Abstract
The invention discloses a kind of for observing the metallographic etching agent and its application method of γ ' phase in Ni-based and ferronickel based high-temperature alloy, which includes: 30~35% phosphoric acid and 65~70% methanol by volume fraction.Wherein, selected chemical reagent is the pure standard of analysis.Application method of the invention is, electrochemical corrosion is carried out by being placed among prepared corrosive agent by the metallographic sample of mechanical polishing, operating voltage is 5-10V, temperature is 20-25 DEG C, after electrochemical corrosion 10~30 seconds, after the corrosive agent on its metallographic surface is rinsed well, dried with clear water and alcohol, the γ ' in its microscopic structure mutually can be observed and be analyzed by scanning electron microscope.Advantage of the invention is that γ ' phase in the alloy structure for having eroded the matrix in alloy and having obtained, the contrast of imaging is big, pattern is high-visible；Meanwhile also can get the profile and pattern of crystal boundary and the precipitated phases such as grain boundary carbide and transgranular carbide, observation analysis can be carried out to grain size etc..
Description
Technical field
The invention belongs to high-temperature alloy material technical fields, and in particular to one kind is closed for observing Ni-based and nickel iron-based high temp
The metallographic etching agent and its application method of γ ' phase in gold.
Background technique
Ni-based and ferronickel based high-temperature alloy not only has excellent tensile strength, creep rupture strength and fatigue strength, also has
Excellent antioxidant anticorrosive and hot corrosion resistance and high temperature microstructure stability, in aerospace, the energy, petrochemical industry
It is widely used.The mechanical property of these alloys and its institutional framework are closely related, thus analyse to its main hardening constituent
The observation analysis of feature out, performance degradation etc. has great importance after the design and long service for alloying component.
The institutional framework of precipitation strength nickel base superalloy is mainly by matrix γ phase and hardening constituent γ ' phase composition.Alloy
The size of mechanical behavior under high temperature and γ ' phase, pattern and spatial distribution are closely related, it is therefore desirable to the analysis to γ ' phase in alloy
It is furtherd investigate out with Evolution.Traditional high temperature alloy metallographic etching agent is primarily directed to aero-engine and heavy combustion
The microstructure of gas-turbine turbo blade nickel base superalloy images, in corrosion process, usually by alloy γ ' phase corrosion dissolution
Fall, thus cannot show the mutually true pattern of γ ' under a scanning electron microscope.It is rotten that this just needs to develop a kind of novel metallographic
Erosion agent and practical approach are used to observe the γ ' phase in superheater tubes precipitation strength nickel base superalloy.
Summary of the invention
The purpose of the present invention is to provide a kind of for observing the etching pit of γ ' phase in Ni-based and ferronickel based high-temperature alloy
Agent and its application method, to observe the γ ' phase in such nickel-base alloy tissue under a scanning electron microscope.The corrosive agent is matched
Side is simple, and application method is easily operated, for such alloy material gold after original state alloy material and Long-term Aging (military service)
Phase imaging results are significant, and γ ' contrast is clear.
The present invention, which adopts the following technical scheme that, to be achieved:
For observing the metallographic etching agent of γ ' phase in Ni-based and ferronickel based high-temperature alloy, by volume fraction by following component
Be uniformly mixed: 30~35% phosphoric acid and 65~70% methanol；Wherein, selected chemical reagent is the pure mark of analysis
It is quasi-.
A further improvement of the present invention lies in that being uniformly mixed by volume fraction by following component: 33% phosphoric acid and
67% methanol.
A further improvement of the present invention lies in that the object that is directed to of the metallographic etching agent is that γ ' mutually strengthens and at timeliness heat
Ni-based and ferronickel based high-temperature alloy after reason.
It, will be by machinery for observing the application method of the metallographic etching agent of γ ' phase in Ni-based and ferronickel based high-temperature alloy
The sample of polishing, which is placed among prepared metallographic etching agent, carries out electrochemical corrosion, operating voltage 5-10V, and temperature is
After 20-25 DEG C, electrochemical corrosion 10~30 seconds, cleaning, it is dry after, it can be organized by scanning electron microscope in
The observation and analysis of γ ' phase.
A further improvement of the present invention lies in that the alloy after electrochemical corrosion can show the shape of crystal grain and crystal boundary simultaneously
Looks.
A further improvement of the present invention lies in that clear water and alcohol are dry by the corrosive agent flushing on microstructure of the alloy surface when cleaning
Only.
The present invention has following beneficial technical effect:
The present invention for γ/γ ' two-phase is Ni-based and ferronickel based high-temperature alloy, by with corrosive agent to the polishing of such alloy after
Metallographic surface carries out electrochemical corrosion processing, mutually to carry out observation analysis to γ ' in alloy structure, and can observe simultaneously other aobvious
Micro-assembly robot pattern.
Phosphoric acid in the corrosive agent is used for etched the matrix γ phase.In order to slow down to matrix γ phase corrosion rate and convenient for behaviour
Make, joined methanol as organic inhibitor.
Advantage of the invention is that γ ' phase in the alloy structure for having eroded the matrix in alloy and having obtained, pair of imaging
It is bigger than degree, pattern is high-visible；Meanwhile it also can get the profile of crystal boundary and the precipitated phases such as grain boundary carbide and transgranular carbide
And pattern, observation analysis can be carried out to grain size etc..
Detailed description of the invention
Fig. 1 is γ/γ ' institutional framework in IN740H alloy after aging strengthening model that caustic treatment obtains through the invention
Scanning electron microscope pattern photo；
Fig. 2 is γ/γ ' tissue in 282 alloy of Haynes after aging strengthening model that caustic treatment obtains through the invention
The scanning electron microscope pattern photo of structure；
Fig. 3 is crystal boundary structure knot in 282 alloy of Haynes after aging strengthening model that caustic treatment obtains through the invention
The scanning electron microscope pattern photo of structure.
Fig. 4 is γ/γ ' institutional framework in GH2984 alloy after aging strengthening model that caustic treatment obtains through the invention
Scanning electron microscope pattern photo.
Fig. 5 is MC carbide and crystal boundary in GH2984 alloy after aging strengthening model that caustic treatment obtains through the invention
Scanning electron microscope pattern photo.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawings and examples.
Provided by the present invention for observing the metallographic etching agent of γ ' phase in Ni-based and ferronickel based high-temperature alloy, by volume point
Number be uniformly mixed by following component: 30~35% phosphoric acid and 65~70% methanol.Wherein, selected chemical reagent
It is the pure standard of analysis.Its application method is that will be placed among prepared corrosive agent by the metallographic sample of mechanical polishing
Carry out electrochemical corrosion, operating voltage 5-10V, after temperature is 20-25 DEG C, electrochemical corrosion 10~30 seconds, with clear water and
It, can be by scanning electron microscope in its microscopic structure after the corrosive agent on its metallographic surface is rinsed well, dried by alcohol
γ ' mutually observed.
Wherein, the Ni-based and ferronickel based high-temperature alloy of the corrosive agent mutually strengthened for object for γ ', is suitable at timeliness
Ni-based and ferronickel based high-temperature alloy metallographic sample after reason, formula is simple, and operation is same simple and easy.
The present invention is used to observe the application method of the metallographic etching agent of γ ' phase in Ni-based and ferronickel based high-temperature alloy tissue,
Electrochemical corrosion is carried out by being placed among prepared metallographic etching agent by the sample of mechanical polishing, operating voltage 5-
10V after temperature is 20-25 DEG C, electrochemical corrosion 10~30 seconds, is rinsed the corrosive agent on its metallographic surface with clear water and alcohol
Completely, after dry, i.e., the pattern of the γ ' phase in alloy microscopic structure is shown under a scanning electron microscope.In addition, through the gold
Ni-based and ferronickel based high-temperature alloy after phase corrosive agent after etching shows the pattern of crystal grain and crystal boundary simultaneously.
Embodiment 1:
Electrochemical corrosion processing has been carried out to nickel base superalloy IN740H.The alloy is equally mutually strong as high temperature using γ '
Change phase, Ni content is 50.8% (mass fraction) in alloy, and Cr content is 25% (mass fraction).The alloy passes through timeliness heat
Handle the γ ' phase obtained.Fig. 1 is the metallographic after being mechanically polished using the IN740H alloy after the corrosive agent aging strengthening model
Surface carries out the tissue topography after electrochemical corrosion, and the γ ' of transgranular square therein is mutually high-visible under scanning electron microscope.
Embodiment 2:
Electrochemical corrosion processing has been carried out to nickel base superalloy Haynes 282.The alloy is mutually strong as high temperature using γ '
Change phase, Ni content is 57% (mass fraction) in alloy, and Cr content is 20% (mass fraction).Alloy passes through aging strengthening model
γ ' the phase of acquisition.Fig. 2 and Fig. 3 is respectively that 282 alloy of Haynes after using the corrosive agent aging strengthening model carries out mechanical throwing
Metallographic surface after light carries out the tissue topography after electrochemical corrosion, and wherein the spherical γ ' of intra-die is mutually being scanned with crystal boundary
It is high-visible under Electronic Speculum.
Embodiment 3:
Electrochemical corrosion has been carried out to ferronickel based high-temperature alloy GH2984 alloy.The alloy is using γ ' mutually as High-Temperature Strengthening
Phase, Ni content is 40~42% (mass fractions) in alloy, and Fe content is 32~34% (mass fractions).GH2984 alloy is low
After warm hardening processing, γ ' phase is precipitated in intra-die, since γ ' phase amount of precipitation is few, size is small, and is distributed in crystal boundary, is very unlikely to
It observes.After metallographic surface after mechanically polishing using the corrosive agent to it carries out electrochemical corrosion, pass through scanning electron
Microscope can be clearly observed the γ ' of the intra-die of the distribution mutually grain boundary structure with MC carbide and alloy, respectively
As shown in Figure 4 and Figure 5.
Claims (6)
1. for observing the metallographic etching agent of γ ' phase in Ni-based and ferronickel based high-temperature alloy, which is characterized in that by volume fraction by
Following component is uniformly mixed: 30~35% phosphoric acid and 65~70% methanol；Wherein, selected chemical reagent is
Analyze pure standard.
2. it is according to claim 1 for observing the metallographic etching agent of γ ' phase in Ni-based and ferronickel based high-temperature alloy, it is special
Sign is, is uniformly mixed by volume fraction by following component: 33% phosphoric acid and 67% methanol.
3. it is according to claim 1 or 2 for observing the metallographic etching agent of γ ' phase in Ni-based and ferronickel based high-temperature alloy,
It is characterized in that, the metallographic etching agent is that γ ' mutually strengthens and the Ni-based and ferronickel base height after aging strengthening model for object
Temperature alloy.
4. for observing the etching pit of γ ' phase in Ni-based and ferronickel based high-temperature alloy described in any one of claims 1 to 3
The application method of agent, which is characterized in that carried out being placed among prepared metallographic etching agent by the sample of mechanical polishing
Electrochemical corrosion, operating voltage 5-10V, after temperature is 20-25 DEG C, electrochemical corrosion 10~30 seconds, after cleaning, drying,
The observation and analysis of γ ' phase in being organized by scanning electron microscope to it.
5. according to claim 4 for observing making for the metallographic etching agent of γ ' phase in Ni-based and ferronickel based high-temperature alloy
With method, which is characterized in that the alloy after electrochemical corrosion can show the pattern of crystal grain and crystal boundary simultaneously.
6. according to claim 4 for observing making for the metallographic etching agent of γ ' phase in Ni-based and ferronickel based high-temperature alloy
With method, which is characterized in that rinsed well the corrosive agent on microstructure of the alloy surface with clear water and alcohol when cleaning.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110438553A (en) * | 2019-09-04 | 2019-11-12 | 内蒙古工业大学 | For observing the metallographic etching agent and caustic solution of γ ' phase in the high-quality GH4738 alloy after secondary forging |
| CN110455605A (en) * | 2019-08-23 | 2019-11-15 | 中国航发北京航空材料研究院 | A kind of clear metallographic etching agent and application method for showing δ phase in GH4169 alloy |
| CN110672393A (en) * | 2019-10-31 | 2020-01-10 | 西安欧中材料科技有限公司 | Sample preparation method for fracture analysis of powder high-temperature alloy durable sample |
| CN111504753A (en) * | 2020-06-11 | 2020-08-07 | 中国航发成都发动机有限公司 | General corrosive agent and corrosion method for gamma' phase and depletion layer metallographic structure of corrosion-resistant high-temperature alloy |
| CN112593278A (en) * | 2020-11-27 | 2021-04-02 | 西安工业大学 | Electrochemical corrosive agent for high-temperature alloy precipitation strengthening phase and use method thereof |
| CN112763523A (en) * | 2020-12-30 | 2021-05-07 | 上海大学 | Three-dimensional etching characterization method for high-nickel maraging steel nonmetallic inclusions |
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| CN106198592A (en) * | 2016-07-01 | 2016-12-07 | 北京北冶功能材料有限公司 | The measuring method of precipitate volume fraction in a kind of nickel base superalloy |
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| CN106198592A (en) * | 2016-07-01 | 2016-12-07 | 北京北冶功能材料有限公司 | The measuring method of precipitate volume fraction in a kind of nickel base superalloy |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110455605A (en) * | 2019-08-23 | 2019-11-15 | 中国航发北京航空材料研究院 | A kind of clear metallographic etching agent and application method for showing δ phase in GH4169 alloy |
| CN110438553A (en) * | 2019-09-04 | 2019-11-12 | 内蒙古工业大学 | For observing the metallographic etching agent and caustic solution of γ ' phase in the high-quality GH4738 alloy after secondary forging |
| CN110438553B (en) * | 2019-09-04 | 2020-09-08 | 内蒙古工业大学 | Metallographic corrosive agent and corrosion method for observing gamma' phase in high-quality GH4738 alloy subjected to secondary forging |
| CN110672393A (en) * | 2019-10-31 | 2020-01-10 | 西安欧中材料科技有限公司 | Sample preparation method for fracture analysis of powder high-temperature alloy durable sample |
| CN111504753A (en) * | 2020-06-11 | 2020-08-07 | 中国航发成都发动机有限公司 | General corrosive agent and corrosion method for gamma' phase and depletion layer metallographic structure of corrosion-resistant high-temperature alloy |
| CN112593278A (en) * | 2020-11-27 | 2021-04-02 | 西安工业大学 | Electrochemical corrosive agent for high-temperature alloy precipitation strengthening phase and use method thereof |
| CN112593278B (en) * | 2020-11-27 | 2022-02-08 | 西安工业大学 | Electrochemical corrosive agent for high-temperature alloy precipitation strengthening phase and use method thereof |
| CN112763523A (en) * | 2020-12-30 | 2021-05-07 | 上海大学 | Three-dimensional etching characterization method for high-nickel maraging steel nonmetallic inclusions |
| CN112763523B (en) * | 2020-12-30 | 2022-10-11 | 上海大学 | Three-dimensional etching characterization method for high-nickel maraging steel nonmetallic inclusions |
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Application publication date: 20181218 |