CN104593775A - Metallographical corrosive for observing delta-Ni3Nb phase in ferronickel-based superalloy structure and using method of metallographical corrosive - Google Patents
Metallographical corrosive for observing delta-Ni3Nb phase in ferronickel-based superalloy structure and using method of metallographical corrosive Download PDFInfo
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Abstract
The invention discloses a metallographical corrosive for observing delta-Ni3Nb phase in a ferronickel-based superalloy structure and a using method of the metallographical corrosive. The metallographical corrosive comprises the following components by volume fraction: 26-33% of hydrochloric acid, 30-37% of nitric acid, 13-18% of hydrofluoric acid and 12-31% of ethyl alcohol; every 100 mL of the metallographical corrosive contains 2g of oxalic acid and 1g of copper sulfate; the mass percentage concentration of the hydrochloric acid is 36%; the mass percentage concentration of the nitric acid is 68%; the mass percentage concentration of the hydrofluoric acid is 40%; the copper sulfate is anhydrous copper sulfate; the ethyl alcohol is anhydrous ethyl alcohol; and the selected chemical reagents are analytical reagents. The using method comprises the following steps: coating the prepared metallographical corrosive on the metallographical surface of a ferronickel-based superalloy sample; chemically corroding for 5-8 seconds; washing and drying the metallographical corrosive on the metallographical surface by clear water and alcohol; and observing the delta-Ni3Nb phase in the microscopic structure through an optical microscope and a scanning electron microscope.
Description
Technical field
The invention belongs to high temperature alloy field, being specifically related to a kind of for observing δ-Ni in ferronickel based high-temperature alloy tissue
3the metallographic etching agent of Nb phase and using method thereof.
Background technology
Ferronickel based high-temperature alloy has good hot strength, preferably processibility and economy, has important application at the high-temperature component of aerospace, the energy, petrochemical field.The microstructure of alloy is closely related with the performance of alloy, separates out and the observation analysis of microstructure Evolution feature its phase, has great importance for performance degradation after the design of alloying constituent, long service etc.
The matrix of ferronickel based high-temperature alloy is austenite γ phase, utilizes γ ' and γ " as the strengthening phase that it is main, γ " often to δ (Ni after long service
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 afterwards
3the change that Nb phase occurs directly affects the change of performance, therefore needs the precipitation of alloy δ phase and Evolution to further investigate.Traditional superalloy metallographic etching agent is mainly for the microtexture video picture of nickel base superalloy, if corrodibility is stronger, easily fallen by the δ phase corrosion dissolution in ni-fe-based alloy, if corrodibility is more weak, then δ phase can not video picture under opticmicroscope and scanning electronic microscope.Adopt electrolytic corrosion, usually occur that the homogeneity of matrix corrosion is poor.
Summary of the invention
The object of the present invention is to provide a kind of for observing δ-Ni in ferronickel based high-temperature alloy tissue
3the metallographic etching agent of Nb phase and using method thereof, to observe the in-house δ of such ni-fe-based alloy-Ni under opticmicroscope and scanning electronic microscope
3nb phase, this etching reagent formula is simple, and remarkable for such alloy material metallographic imaging results after original state alloy material and Long-term Aging (military service), δ contrast is clear.
For achieving the above object, the present invention adopts following technical scheme to be achieved:
For observing δ-Ni in ferronickel based high-temperature alloy tissue
3the metallographic etching agent of Nb phase, by volume mark comprises: the hydrochloric acid of 26 ~ 33%, the nitric acid of 30 ~ 37%, the hydrofluoric acid of 13 ~ 18% and the ethanol of 12 ~ 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 hydrofluoric 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 further improves and is: by volume mark comprises: the hydrochloric acid of 30%, the nitric acid of 35%, the hydrofluoric acid of 15% and the ethanol of 20%.
The present invention further improves and is: this metallographic etching agent be 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 massfraction of contained Fe element is 17 ~ 35%, Nb element massfraction is 3.5 ~ 5.5%.
For observing δ-Ni in ferronickel based high-temperature alloy tissue
3the using method of the metallographic etching agent of Nb phase, by this metallographic etching agent etch ferronickel based high-temperature alloy metallographic surface, chemical corrosion 5 ~ 8 second, after cleaning, drying, demonstrates the δ-Ni in alloy microscopic structure under opticmicroscope or scanning electronic microscope
3the pattern of Nb phase.
The present invention further improves and is: the ferronickel based high-temperature alloy after this metallographic etching agent after etching shows the pattern of grain and grain boundary simultaneously.
The present invention further improves and is: during cleaning, the etching reagent on ferronickel based high-temperature alloy metallographic surface is rinsed well by clear water and alcohol.
Compared with prior art, (γ ") three-phase ferronickel based high-temperature alloy, by carrying out chemical corrosion process, with δ-Ni in alloy tissue with etching reagent to metallographic surface after such alloy polishing to the present invention is directed to γ/γ '/δ
3nb phase carries out observation analysis, and can observe other displaing micro tissue topography simultaneously.
Hydrochloric acid, copper sulfate and nitric acid are for corroding γ matrix, but copper sulfate is unsuitable many, answers control corrosion rate speed; Nitric acid is equal for corroding γ ' as acid with strong oxidizing property; Because the chemical stability of Nb and (intermetallic) compound thereof is good, except hydrofluoric acid not with other mineral acid or alkali effect, be also insoluble to chloroazotic acid, in order to slow down δ-Ni
3nb phase erosion rate, adds oxalic acid and ethanol as organic inhibitor.
Ni (γ matrix)+H
2sO
4+ HNO
3→ NiSO
4+ 2NO
2↑+H
2o
Fe (γ matrix)+2H
+→ Fe
2++ H
2↑
Nb (in δ phase)+HF+5HNO
3→ NbO
2f+5NO
2↑+3H
2o
Technical superiority of the present invention is δ-Ni in the alloy structure obtained
3the contrast gradient of relative (crystal grain) matrix imaging of Nb phase is comparatively large, pattern is clear, to undersized, all can observe it under opticmicroscope and Scanning Electron microscope; Meanwhile, profile and the pattern of crystal boundary and carbide precipitate carbonization can be obtained, observation analysis can be carried out to grain fineness number etc.
Accompanying drawing explanation
Fig. 1 is that long-term (military service) obtained by metallographic etching agent process of the present invention uses δ-Ni in rear GH4169 alloy structure
3the opticmicroscope pattern photo of Nb phase;
Fig. 2 is that long-term (military service) obtained by metallographic etching agent process of the present invention uses δ-Ni in rear GH4169 alloy structure
3the scanning electronic microscope pattern photo of Nb phase;
Fig. 3 is δ-Ni in IN718 alloy structure after the low temperature aging process obtained by metallographic etching agent process of the present invention
3the scanning electronic microscope pattern photo of Nb phase.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated.
The present invention is for observing δ-Ni in ferronickel based high-temperature alloy tissue
3the metallographic etching agent of Nb phase, by volume mark comprises: the hydrochloric acid of 26 ~ 33%, the nitric acid of 30 ~ 37%, the hydrofluoric acid of 13 ~ 18% and the ethanol of 12 ~ 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 hydrofluoric 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 comprises: the hydrochloric acid of 30%, the nitric acid of 35%, the hydrofluoric 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 be ferronickel based high-temperature alloy for object, the 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 massfraction of contained Fe element is 17 ~ 35%, Nb element massfraction is 3.5 ~ 5.5%.
The present invention is for observing δ-Ni in ferronickel based high-temperature alloy tissue
3the using method of the metallographic etching agent of Nb phase, by this metallographic etching agent etch ferronickel based high-temperature alloy metallographic surface, chemical corrosion 5 ~ 8 second, the etching reagent on ferronickel based high-temperature alloy metallographic surface is rinsed well with clear water and alcohol, after drying, under opticmicroscope or scanning electronic microscope, namely demonstrates the δ-Ni in alloy microscopic structure
3the pattern of Nb phase.In addition, the ferronickel based high-temperature alloy after this metallographic etching agent after etching shows the pattern of grain and grain 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% (massfractions), and Nb content is 5.0 ~ 5.5% (massfractions) with γ using γ ' for this alloy.The γ "-Ni obtained by ageing treatment
3nb is converted into its thermodynamic (al) stable state δ-Ni in long-term (military service) use procedure
3nb phase, and agglomeration.Tissue topography after Fig. 1 and Fig. 2 corrodes for the metallographic after using this etching reagent to use GH4169 alloy to carry out mechanical polishing to long-term (militarys service) is surperficial, the wherein δ-Ni of (length) needle-like
3nb phase is high-visible; Simultaneously intracrystalline spherical gamma ' mutually and crystal boundary carbide precipitate also high-visible under scanning electron microscope.
Embodiment 2:
Corrosion treatment is carried out to IN718 alloy, as shown in Figure 3.After IN718 alloy (chemical composition and GH4169 alloy basically identical) low temperature aging process, separate out a small amount of δ-Ni at crystal boundary
3nb phase, due to δ-Ni
3nb phase amount of precipitation is few, size is little, and is distributed in crystal boundary, and pole is not easy to observe.After using this etching reagent to corrode the metallographic surface after it carries out mechanical polishing, clearly can observe a small amount of (short) needle-like δ-Ni perpendicular to crystal boundary distribution by scanning electronic microscope
3nb phase.
Claims (6)
1. for observing δ-Ni in ferronickel based high-temperature alloy tissue
3the metallographic etching agent of Nb phase, is characterized in that: by volume mark comprises: the hydrochloric acid of 26 ~ 33%, the nitric acid of 30 ~ 37%, the hydrofluoric acid of 13 ~ 18% and the ethanol of 12 ~ 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 hydrofluoric 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.
2. according to claim 1 for observing δ-Ni in ferronickel based high-temperature alloy tissue
3the metallographic etching agent of Nb phase, is characterized in that: by volume mark comprises: the hydrochloric acid of 30%, the nitric acid of 35%, the hydrofluoric acid of 15% and the ethanol of 20%.
3. according to claim 1 and 2 for observing δ-Ni in ferronickel based high-temperature alloy tissue
3the metallographic etching agent of Nb phase, it is characterized in that: this metallographic etching agent be 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 massfraction of contained Fe element is 17 ~ 35%, Nb element massfraction is 3.5 ~ 5.5%.
4. according to any one of claims 1 to 3 for observing δ-Ni in ferronickel based high-temperature alloy tissue
3the using method of the metallographic etching agent of Nb phase, it is characterized in that: by this metallographic etching agent etch ferronickel based high-temperature alloy metallographic surface, chemical corrosion 5 ~ 8 second, after cleaning, drying, under opticmicroscope or scanning electronic microscope, demonstrate the δ-Ni in alloy microscopic structure
3the pattern of Nb phase.
5. according to claim 4 for observing δ-Ni in ferronickel based high-temperature alloy tissue
3the using method of the metallographic etching agent of Nb phase, is characterized in that: the ferronickel based high-temperature alloy after this metallographic etching agent after etching shows the pattern of grain and grain boundary simultaneously.
6. according to claim 4 for observing δ-Ni in ferronickel based high-temperature alloy tissue
3the using method of the metallographic etching agent of Nb phase, is characterized in that: during cleaning, the etching reagent on ferronickel based high-temperature alloy metallographic surface is rinsed well by clear water and alcohol.
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Cited By (13)
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| 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 |
| CN107747095A (en) * | 2017-10-17 | 2018-03-02 | 中国华能集团公司 | A kind of ni-fe-based alloy weld joint samples metallographic etching agent and application method |
| CN107991160A (en) * | 2017-11-16 | 2018-05-04 | 中国航发沈阳黎明航空发动机有限责任公司 | A kind of iron-base superalloy diskware surface defect macro inspection method |
| CN108760452A (en) * | 2018-05-30 | 2018-11-06 | 山东大学 | Nickel base superalloy γ ' phases show and quantitative evaluation method |
| 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 |
| 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 |
| CN113702379A (en) * | 2021-08-27 | 2021-11-26 | 华能国际电力股份有限公司 | Metallographic corrosion method for displaying homogenized structure of high-alloying 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 |
| CN114112608A (en) * | 2021-11-19 | 2022-03-01 | 华能国际电力股份有限公司 | Multistage corrosion process for metallographic structure observation 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 |
| CN115323378A (en) * | 2022-08-18 | 2022-11-11 | 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 application method thereof |
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| CN107747095A (en) * | 2017-10-17 | 2018-03-02 | 中国华能集团公司 | A kind of ni-fe-based alloy weld joint samples metallographic etching agent and application method |
| 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 |
| CN107991160A (en) * | 2017-11-16 | 2018-05-04 | 中国航发沈阳黎明航空发动机有限责任公司 | A kind of iron-base superalloy diskware surface defect macro inspection method |
| 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 |
| CN108760452A (en) * | 2018-05-30 | 2018-11-06 | 山东大学 | Nickel base superalloy γ ' phases 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 |
| 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 |
| 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 |
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| 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 |
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| 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 |
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| 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 |
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| 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 |
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