CN104593775B - For observing δ-Ni in ferronickel based high-temperature alloy tissue3the metallographic etching agent of Nb phase and using method thereof - Google Patents
For observing δ-Ni in ferronickel based high-temperature alloy tissue3the metallographic etching agent of Nb phase and using method thereof Download PDFInfo
- Publication number
- CN104593775B CN104593775B CN201510071208.7A CN201510071208A CN104593775B CN 104593775 B CN104593775 B CN 104593775B CN 201510071208 A CN201510071208 A CN 201510071208A CN 104593775 B CN104593775 B CN 104593775B
- Authority
- CN
- China
- Prior art keywords
- based high
- metallographic
- temperature alloy
- etching agent
- phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention discloses a kind of for observing δ Ni in ferronickel based high-temperature alloy tissue3The metallographic etching agent of Nb phase and using method thereof, this metallographic etching agent by volume mark includes: 26～the Fluohydric acid. of the nitric acid of the hydrochloric acid of 33%, 30～37%, 13～18% and 12～the ethanol of 31%, and containing 2g oxalic acid and 1g copper sulfate in every this metallographic etching agent of 100mL；Wherein, hydrochloric acid mass percentage concentration is 36%, and nitric acid mass percentage concentration is 68%, and Fluohydric acid. mass percentage concentration is 40%, and copper sulfate reagent is anhydrous cupric sulfate, and ethanol is dehydrated alcohol, selected by be that chemical reagent is analytical pure standard；The metallographic etching agent prepared is coated on the metallographic surface of ferronickel based high-temperature alloy sample by its using method, chemical attack 5～after 8 seconds, the caustic on its metallographic surface is rinsed well, after drying with clear water and ethanol, can be by optical microscope and scanning electron microscope to the δ Ni in its microscopic structure3Nb phase is observed.
Description
Technical field
The invention belongs to high-temperature alloy material field, be specifically related to a kind of for observing δ-Ni in ferronickel based high-temperature alloy tissue3The metallographic etching agent of Nb phase and using method thereof.
Background technology
Ferronickel based high-temperature alloy has preferable elevated temperature strength, preferable processability and economy, has important application at Aero-Space, the energy, the high-temperature component of petrochemical field.The microstructure of alloy is closely related with the performance of alloy, separates out its phase and the observation analysis of microstructure Evolution feature, has great importance for performance degradation after the design of alloying component, long service etc..
The matrix of ferronickel based high-temperature alloy is austenite γ phase, and " as the hardening constituent that it is main, γ is " often to δ (Ni after long service with γ to utilize γ '3Nb) inversion of phases, δ phase is as γ after long service, and " stable state of phase, its pattern, distribution and quantity affect the mechanical behavior under high temperature of ni-fe-based alloy, especially at Long-term Aging (military service) δ-Ni afterwards3The change that Nb phase occurs directly affects the change of performance, it is therefore desirable to precipitation and Evolution to alloy δ phase are furtherd investigate.Traditional high temperature alloy metallographic etching agent is primarily directed to the microstructure imaging of nickel base superalloy, if corrosivity is stronger, easily being fallen by the δ phase corrosion dissolution in ni-fe-based alloy, if corrosivity is more weak, then δ phase can not image under optical microscope and scanning electron microscope.Use electrolytic etching, usually occur that the uniformity of matrix corrosion is poor.
Summary of the invention
It is an object of the invention to provide a kind of for observing δ-Ni in ferronickel based high-temperature alloy tissue3The metallographic etching agent of Nb phase and using method thereof, to observe such ni-fe-based alloy in-house δ-Ni under optical microscope and scanning electron microscope3Nb phase, this caustic formula is simple, and notable for such alloy material metallographic imaging results after original state alloy material and Long-term Aging (military service), δ contrast is clear.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that and is achieved:
For observing δ-Ni in ferronickel based high-temperature alloy tissue3The metallographic etching agent of Nb phase, by volume mark includes: 26～the Fluohydric acid. of the nitric acid of the hydrochloric acid of 33%, 30～37%, 13～18% and 12～the ethanol of 31%, and containing 2g oxalic acid and 1g copper sulfate in every this metallographic etching agent of 100mL；Wherein, hydrochloric acid mass percentage concentration is 36%, and nitric acid mass percentage concentration is 68%, and Fluohydric acid. mass percentage concentration is 40%, and copper sulfate reagent is anhydrous cupric sulfate, and ethanol is dehydrated alcohol, selected by be that chemical reagent is analytical pure standard.
The present invention is further improved by: by volume mark includes: the hydrochloric acid of 30%, the nitric acid of 35%, the Fluohydric acid. of 15% and the ethanol of 20%.
The present invention is further improved by: this metallographic etching agent is ferronickel based high-temperature alloy for object, ferronickel based high-temperature alloy metallographic sample after being applicable to Ageing Treatment or after life-time service, wherein, in ferronickel based high-temperature alloy, the mass fraction of contained Fe element is 17～35%, and Nb element mass fraction is 3.5～5.5%.
For observing δ-Ni in ferronickel based high-temperature alloy tissue3The using method of the metallographic etching agent of Nb phase, by this metallographic etching agent etch ferronickel based high-temperature alloy metallographic surface, chemical attack 5～8 seconds, clean, dried, under optical microscope or scanning electron microscope, demonstrate the δ-Ni in alloy microscopic structure3The pattern of Nb phase.
The present invention is further improved by: the ferronickel based high-temperature alloy after this metallographic etching agent after etching shows the pattern of crystal grain and crystal boundary simultaneously.
The present invention is further improved by: during cleaning, the caustic on ferronickel based high-temperature alloy metallographic surface is rinsed well by clear water and ethanol.
Compared with prior art, (γ ") three-phase ferronickel based high-temperature alloy carries out chemical attack process, with to δ-Ni in alloy structure by metallographic surface after polishing such alloy with caustic to the present invention is directed to γ/γ '/δ3Nb phase carries out observation analysis, and can observe other displaing micro tissue topography simultaneously.
Hydrochloric acid, copper sulfate and nitric acid are used for corroding γ matrix, but copper sulfate is unsuitable many, answers control corrosion rate speed；It is equal that nitric acid is used for corroding γ ' as acid with strong oxidizing property；Owing to the chemical stability of Nb and (between metal) compound thereof is good, outside dehydrogenation fluoric acid not with other mineral acid or alkali effect, also insoluble in chloroazotic acid, in order to slow down δ-Ni3Nb phase corrosion rate, adds oxalic acid and ethanol as organic inhibitor.
Ni (γ matrix)+H2SO4+HNO3→NiSO4+2NO2↑+H2O
Fe (γ matrix)+2H+→Fe2++H2↑
Nb (in δ phase)+HF+5HNO3→NbO2F+5NO2↑+3H2O
The present invention's it is a technical advantage that obtain alloy structure in δ-Ni3The contrast of Nb phase (crystal grain) matrix imaging relatively is relatively big, pattern is clear, to undersized, all can observe it under optical microscope and Scanning Electron microscope；Meanwhile, crystal boundary and the profile of carbide precipitate carbonization and pattern can be obtained, grain size etc. can be carried out observation analysis.
Accompanying drawing explanation
Fig. 1 is to be processed after long-term (military service) use obtained δ-Ni in GH4169 alloy structure by metallographic etching agent of the present invention3The optical microscope pattern photo of Nb phase；
Fig. 2 is to be processed after long-term (military service) use obtained δ-Ni in GH4169 alloy structure by metallographic etching agent of the present invention3The scanning electron microscope pattern photo of Nb phase；
Fig. 3 is to process after the low temperature aging that obtains processes δ-Ni in IN718 alloy structure by metallographic etching agent of the present invention3The scanning electron microscope pattern photo of Nb phase.
Detailed description of the invention
The present invention is further illustrated with detailed description of the invention below in conjunction with the accompanying drawings.
The present invention is used for observing δ-Ni in ferronickel based high-temperature alloy tissue3The metallographic etching agent of Nb phase, by volume mark includes: 26～the Fluohydric acid. of the nitric acid of the hydrochloric acid of 33%, 30～37%, 13～18% and 12～the ethanol of 31%, and containing 2g oxalic acid and 1g copper sulfate in every this metallographic etching agent of 100mL；Wherein, hydrochloric acid mass percentage concentration is 36%, and nitric acid mass percentage concentration is 68%, and Fluohydric acid. mass percentage concentration is 40%, and copper sulfate reagent is anhydrous cupric sulfate, and ethanol is dehydrated alcohol, selected by be that chemical reagent is analytical pure standard.
Further, this metallographic etching agent by volume mark includes: the hydrochloric acid of 30%, the nitric acid of 35%, the Fluohydric acid. of 15% and the ethanol of 20%, and containing 2g oxalic acid and 1g copper sulfate in the metallographic etching agent of every 100mL.
Wherein, this metallographic etching agent is ferronickel based high-temperature alloy for object, it is adaptable to the ferronickel based high-temperature alloy metallographic sample after Ageing Treatment or after life-time service, wherein, in ferronickel based high-temperature alloy, the mass fraction of contained Fe element is 17～35%, and Nb element mass fraction is 3.5～5.5%.
The present invention is used for observing δ-Ni in ferronickel based high-temperature alloy tissue3The using method of the metallographic etching agent of Nb phase, by this metallographic etching agent etch ferronickel based high-temperature alloy metallographic surface, chemical attack 5～8 seconds, the caustic on ferronickel based high-temperature alloy metallographic surface is rinsed well, after drying with clear water and ethanol, under optical microscope or scanning electron microscope, i.e. demonstrate the δ-Ni in alloy microscopic structure3The pattern of Nb phase.Additionally, the ferronickel based high-temperature alloy after this metallographic etching agent after etching shows the pattern of crystal grain and crystal boundary simultaneously.
Embodiment 1:
Ferronickel based high-temperature alloy GH4169 alloy is corroded."/δ phase is as High-Temperature Strengthening phase, and in its alloy, Fe content is 18～19% (mass fraction), and Nb content is 5.0～5.5% (mass fraction) with γ using γ ' for this alloy.The γ "-Ni obtained by Ageing Treatment3Nb is converted into its thermodynamic (al) stable state δ-Ni during long-term (military service) uses3Nb phase, and agglomeration.Fig. 1 and Fig. 2 is the tissue topography after using this caustic to corrode the metallographic surface after (military service) use GH4169 alloy mechanically polishes for a long time, wherein (grows) δ-Ni of needle-like3Nb phase is high-visible；Simultaneously intracrystalline spherical gamma ' mutually and crystal boundary carbide precipitate is also high-visible under scanning electron microscope.
Embodiment 2:
IN718 alloy is carried out corrosion treatmentCorrosion Science, as shown in Figure 3.After IN718 alloy (chemical composition is basically identical with GH4169 alloy) low temperature aging processes, separate out a small amount of δ-Ni at crystal boundary3Nb phase, due to δ-Ni3Nb phase amount of precipitation is few, size is little, and is distributed in crystal boundary, is very unlikely to observe.After metallographic surface after using this caustic to mechanically polish it is corroded, a small amount of (short) needle-like δ-Ni being perpendicular to crystal boundary distribution can be clearly observed by scanning electron microscope3Nb phase.
Claims (6)
1. it is used for observing δ-Ni in ferronickel based high-temperature alloy tissue3The metallographic etching agent of Nb phase, it is characterised in that: by volume mark
Including: 26～the Fluohydric acid. of the nitric acid of the hydrochloric acid of 33%, 30～37%, 13～18% and 12～the ethanol of 31%, and every 100mL
Containing 2g oxalic acid and 1g copper sulfate in this metallographic etching agent；Wherein, hydrochloric acid mass percentage concentration is 36%, nitric acid percent mass
Concentration is 68%, and Fluohydric acid. mass percentage concentration is 40%, and copper sulfate reagent is anhydrous cupric sulfate, and ethanol is dehydrated alcohol, institute
Selection is that chemical reagent is analytical pure standard；
During use, by this metallographic etching agent etch ferronickel based high-temperature alloy metallographic surface, chemical attack 5～8 seconds, with clear water and
The caustic on ferronickel based high-temperature alloy metallographic surface rinsed well by ethanol, after drying, i.e. show at optical microscope or scanning electron
δ-the Ni in alloy microscopic structure is demonstrated under micro mirror3The pattern of Nb phase.
The most according to claim 1 for observing δ-Ni in ferronickel based high-temperature alloy tissue3The metallographic etching agent of Nb phase, its
It is characterised by: by volume mark includes: the hydrochloric acid of 30%, the nitric acid of 35%, the Fluohydric acid. of 15% and the ethanol of 20%.
The most according to claim 1 and 2 for observing δ-Ni in ferronickel based high-temperature alloy tissue3The metallographic etching agent of Nb phase,
It is characterized in that: this metallographic etching agent is ferronickel based high-temperature alloy for object, it is adaptable to after Ageing Treatment or after life-time service
Ferronickel based high-temperature alloy metallographic sample, wherein, in ferronickel based high-temperature alloy, the mass fraction of contained Fe element is 17～35%,
Nb element mass fraction is 3.5～5.5%.
4. δ-Ni during being used for described in claim 1 or 2 observes ferronickel based high-temperature alloy tissue3Making of the metallographic etching agent of Nb phase
By method, it is characterised in that: by this metallographic etching agent etch ferronickel based high-temperature alloy metallographic surface, chemical attack 5～8 seconds,
Clean, dried, under optical microscope or scanning electron microscope, demonstrate the δ-Ni in alloy microscopic structure3The shape of Nb phase
Looks.
The most according to claim 4 for observing δ-Ni in ferronickel based high-temperature alloy tissue3The metallographic etching agent of Nb phase
Using method, it is characterised in that: the ferronickel based high-temperature alloy after this metallographic etching agent after etching shows crystal grain and crystal boundary simultaneously
Pattern.
The most according to claim 4 for observing δ-Ni in ferronickel based high-temperature alloy tissue3The metallographic etching agent of Nb phase
Using method, it is characterised in that: during cleaning, the caustic on ferronickel based high-temperature alloy metallographic surface is rinsed well by clear water and ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510071208.7A CN104593775B (en) | 2015-02-10 | 2015-02-10 | For observing δ-Ni in ferronickel based high-temperature alloy tissue3the metallographic etching agent of Nb phase and using method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510071208.7A CN104593775B (en) | 2015-02-10 | 2015-02-10 | For observing δ-Ni in ferronickel based high-temperature alloy tissue3the metallographic etching agent of Nb phase and using method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104593775A CN104593775A (en) | 2015-05-06 |
| CN104593775B true CN104593775B (en) | 2016-11-16 |
Family
ID=53119820
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510071208.7A Active CN104593775B (en) | 2015-02-10 | 2015-02-10 | For observing δ-Ni in ferronickel based high-temperature alloy tissue3the metallographic etching agent of Nb phase and using method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104593775B (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107747095B (en) * | 2017-10-17 | 2019-11-22 | 中国华能集团公司 | A kind of ni-fe-based alloy weld joint samples metallographic etching agent and application method |
| CN107576554A (en) * | 2017-11-07 | 2018-01-12 | 中国民航大学 | IN718 alloys δ phases corrosive liquid and the preparation method of corrosive liquid and sample |
| CN107991160B (en) * | 2017-11-16 | 2020-12-04 | 中国航发沈阳黎明航空发动机有限责任公司 | Macroscopic inspection method for surface defects of iron-based high-temperature alloy disc |
| CN108760452B (en) * | 2018-05-30 | 2019-05-14 | 山东大学 | Nickel base superalloy γ ' phase show and quantitative evaluation method |
| 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 |
| CN112725800A (en) * | 2020-12-29 | 2021-04-30 | 西安赛尔电子材料科技有限公司 | Corrosive agent for Inconel X-750 alloy metallographic detection and preparation method and corrosion method thereof |
| CN113702379B (en) * | 2021-08-27 | 2023-09-01 | 华能国际电力股份有限公司 | Metallographic corrosion method for displaying homogenized structure of high-alloyed nickel-based alloy |
| CN113758784A (en) * | 2021-09-06 | 2021-12-07 | 湘潭大学 | Metallographic corrosive liquid and corrosive method applied to iron-based matrix nickel-based coating |
| CN114112608B (en) * | 2021-11-19 | 2024-03-12 | 华能国际电力股份有限公司 | Multistage corrosion process for observing metallographic structure of high-temperature alloy in original state and solid solution state |
| CN114264656A (en) * | 2021-12-30 | 2022-04-01 | 西安汉唐分析检测有限公司 | Corrosion observation method for metallographic structure of Nb-Ta-Hf alloy |
| CN114606496A (en) * | 2022-03-28 | 2022-06-10 | 西安热工研究院有限公司 | Metallographic corrosive agent for 800H alloy welded joint sample, preparation method and metallographic display method |
| CN114672808A (en) * | 2022-03-30 | 2022-06-28 | 西安热工研究院有限公司 | Corrosive agent for gamma' phase metallographic phase in nickel-based alloy, preparation method and corrosion method |
| CN115323378B (en) * | 2022-08-18 | 2024-04-26 | 西安热工研究院有限公司 | Metallographic corrosive agent for displaying sliding band of austenitic material, and preparation method and use method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4071397A (en) * | 1973-07-02 | 1978-01-31 | Motorola, Inc. | Silicon metallographic etch |
| CN103196733B (en) * | 2013-04-01 | 2015-03-11 | 东方电气集团东方汽轮机有限公司 | Etchant for displaying metallographic structure of nickel-based high temperature alloy and method |
| CN103822817A (en) * | 2014-02-28 | 2014-05-28 | 金川集团股份有限公司 | Pure nickel chemical polishing etching solution and application method |
-
2015
- 2015-02-10 CN CN201510071208.7A patent/CN104593775B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104593775A (en) | 2015-05-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104593775B (en) | For observing δ-Ni in ferronickel based high-temperature alloy tissue3the metallographic etching agent of Nb phase and using method thereof | |
| Xu et al. | Effect of quasicrystalline phase on improving the corrosion resistance of a duplex structured Mg–Li alloy | |
| CN109457245B (en) | Machining-state wrought aluminum alloy grain boundary corrosive agent and preparation method and application thereof | |
| CN104677715B (en) | A kind of method for being used for record in situ and observing magnesium alloy microstructures corrosion behavior | |
| CN103792128A (en) | Method for displaying two-phase grain boundary of duplex stainless steel | |
| CN108896378A (en) | A kind of the electrobrightening corrosive agent and its application method of high temperature alloy | |
| CN106702383A (en) | Metallographic-phase corrosion liquid of beta titanium alloy and corrosion method | |
| CN107761160B (en) | A kind of electrolytic etching agent of high-strength invar microscopic structure and caustic solution | |
| CN104762622A (en) | A treatment method for brightening surfaces of copper nickel alloy tubes | |
| CN110438553B (en) | Metallographic corrosive agent and corrosion method for observing gamma' phase in high-quality GH4738 alloy subjected to secondary forging | |
| CN103163003A (en) | Metallographic phase display method used for different microstructure conditions of wrought magnesium alloy | |
| CN111579325A (en) | Metallographic corrosion method of high-strength beta titanium alloy | |
| CN110749718A (en) | Dendritic crystal corrosive agent and corrosion method for maraging stainless steel | |
| CN113916634B (en) | Method for rapidly representing grain size of nickel-based and nickel-iron-based alloy | |
| LI et al. | Corrosion action and passivation mechanism of magnesium alloy in fluoride solution | |
| CN107478486B (en) | Method for displaying original grain boundary of Fe-Mn-Al-C low-density steel | |
| CN109385633A (en) | The metallographic etchant and its caustic solution of one Albatra metal | |
| CN111139379A (en) | Degradable aluminum alloy and heat treatment method thereof, aluminum alloy and application thereof | |
| CN107988599A (en) | A kind of metallographic etching agent for distinguishing titanium alloy condition of heat treatment | |
| CN110608937A (en) | Metallographic corrosive agent for stainless steel high-temperature quenching structure and corrosion method thereof | |
| Wang et al. | Effect of crystal orientation on the corrosion behavior of as-cast pure aluminum anodes in air batteries | |
| KR101122698B1 (en) | Etchant composition of nickle-based superalloy and method of etching the alloy | |
| CN113403621B (en) | Metallographic corrosive agent for austenitic Fe-Mn-Al-C series low-density high-strength steel and preparation method and application thereof | |
| CN113049347B (en) | Metallographic corrosive agent for precipitation strengthening of high-temperature alloy and use method thereof | |
| KR20200038027A (en) | Etching solution for observation of austenite crystal grain and etching method using the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |