CN108611675A - A kind of electrolytic etching method of nickel-base high-temperature single crystal alloy - Google Patents
A kind of electrolytic etching method of nickel-base high-temperature single crystal alloy Download PDFInfo
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- CN108611675A CN108611675A CN201810413778.3A CN201810413778A CN108611675A CN 108611675 A CN108611675 A CN 108611675A CN 201810413778 A CN201810413778 A CN 201810413778A CN 108611675 A CN108611675 A CN 108611675A
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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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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/52—Alloys
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
Abstract
The invention discloses a kind of electrolytic etching method of nickel-base high-temperature single crystal alloy, this method includes：One, as cast condition nickel-base high-temperature single crystal alloy is ground, polished, cleaned and dried successively；Two, using nickel-base high-temperature single crystal alloy after drying as anode, carbon-point connects DC power supply and carries out electrolytic etching as cathode；Step 3: the nickel-base high-temperature single crystal alloy after electrolytic etching is cleaned successively and is dried, microexamination is then carried out.The present invention uses H3PO4Solution, HNO3Solution and H2SO4The electrolytic etching agent that solution is formulated, the nickel-base high-temperature single crystal alloy of C will be added to, or the γ matrixes phase and γ ' hardening constituents being added in the nickel-base high-temperature single crystal alloy of C and B erode, make the carbide being precipitated in alloy and boride is clearer displays, avoid the interference of other phases, be conducive to subsequent microexamination, shorten the time of corrosion, improves the uniformity of nickel-base high-temperature single crystal alloy specimen surface corrosion.
Description
Technical field
The invention belongs to Metallographic Analysis technical fields, and in particular to a kind of electrolytic etching side of nickel-base high-temperature single crystal alloy
Method.
Background technology
Nickel-base high-temperature single crystal alloy is the preferred material of current novel advanced aero engine blade, and trace element is to nickel
The influence of based single-crystal high-temperature alloy organization and performance is the hot spot studied at present.With the increase of Trace Elements, close
Some cenotypes are understood in Jin Zhonghui precipitations.For example, the addition of trace element C and B can make that a large amount of carbide and boronation are precipitated in alloy
Object phase.Studies have shown that carbide and boride are precipitated around eutectic structure in nickel-base high-temperature single crystal alloy, and pattern phase
Seemingly, so to research differentiate alloy in carbide and boride cause difficulty.And in nickel-base high-temperature single crystal alloy, carbonization
The precipitation pattern of object and boride can also influence the raising of alloy mechanical property.Therefore, it is necessary to carbon to being precipitated in alloy
Compound and boride mutually carry out observation discriminating, and control the analysis of carbide and boride by C in optimized alloy, B content
Go out quantity and pattern, and then improves the mechanical property of alloy.
In the research process to the microstructure observation of nickel-base high-temperature single crystal alloy, the selection direct relation of caustic solution
To the observing effect of alloy microscopic structure.Nickel-base high-temperature single crystal alloy corrosion at present mostly uses immersion corrosion method, immersion corrosion method
It is divided into as shallow corrosion and deep etch.It is shallow to corrode the arborescent structure being mainly used in research nickel-base high-temperature single crystal alloy, eutectic structure
With γ ' phases, shallow corrosive liquid is generally formed by nitric acid, hydrofluoric acid and glycerol；Deep etch is mainly used for studying to be carbonized in alloy
The precipitation pattern of object and boride, deep etch liquid are generally formulated by hydrogen peroxide and hydrochloric acid.Either shallow corrosion is still deep
Corrosion all has the following problems：(1) selected nitric acid, hydrofluoric acid and hydrochloric acid are volatile when corrosive liquid is prepared, corrosive liquid
Concentration is not easy to control；(2) corrode and take longer, especially deep etch, the general corrosion time is 40min~50min；(3) corrode
Uneven, corrosive effect is poor, often will appear and corrodes less than or corrode too deep phenomenon, is unfavorable for the sight of later stage microscopic structure
It examines and studies.
Invention content
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, provide a kind of nickel-based monocrystal
The electrolytic etching method of high temperature alloy.This method uses volume ratio for 13:42:46 H3PO4Solution, HNO3Solution and H2SO4It is molten
The electrolyte that liquid is formulated will be added to the nickel-base high-temperature single crystal alloy of C, or be added to the nickel-based monocrystal high temperature conjunction of C and B
γ matrixes phase and γ ' hardening constituents in gold erode, and make the carbide being precipitated in nickel-base high-temperature single crystal alloy alloy, or be precipitated
Carbide and boride is clearer displays, shorten the time of corrosion, improve nickel-base high-temperature single crystal alloy sample
The uniformity of surface corrosion.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of electrolysis of nickel-base high-temperature single crystal alloy
Caustic solution, which is characterized in that this approach includes the following steps：
Step 1: as cast condition nickel-base high-temperature single crystal alloy is ground successively, polished, cleaned and is dried；The as cast condition nickel
The mass content of C is that the mass content of C in 0.085% or as cast condition nickel-base high-temperature single crystal alloy is in based single-crystal high-temperature alloy
The mass content that the mass content of 0.072%, B are C in 0.005% or as cast condition nickel-base high-temperature single crystal alloy is 0.085%, B
Mass content be C in 0.010% or as cast condition nickel-base high-temperature single crystal alloy mass content be 0.078%, B quality contain
Amount is 0.014%；
Step 2: using nickel-base high-temperature single crystal alloy after drying in step 1 as anode, carbon-point is connected as cathode
DC power supply carries out electrolytic etching, waits for that the surface of nickel-base high-temperature single crystal alloy loses metallic luster and one layer of fine and close silvery white occurs
Stop electrolytic etching after corrosion layer；The electrolytic etching agent that the electrolytic etching uses is by H3PO4Solution, HNO3Solution and H2SO4It is molten
Liquid is according to 13:42:46 volume ratio is formulated, the H3PO4Solution, HNO3Solution and H2SO4The mass concentration of solution is distinguished
It is 65%, 15% and 20%；
Step 3: the nickel-base high-temperature single crystal alloy in step 2 after electrolytic etching is cleaned and is dried successively, so
After carry out microexamination.
The electrolytic etching method of above-mentioned a kind of nickel-base high-temperature single crystal alloy, which is characterized in that be electrolysed described in step 2
The voltage of corrosion is 5V~6V, and the time is 10s~12s.
A kind of electrolytic etching method of above-mentioned nickel-base high-temperature single crystal alloy, which is characterized in that the electricity of the electrolytic etching
Pressure is 5V, time 12s.
Compared with the prior art, the present invention has the following advantages：
1, the electrolytic etching agent that the present invention uses can will be added to the nickel-base high-temperature single crystal alloy of C, or be added to C and B
Nickel-base high-temperature single crystal alloy in γ matrixes phase and γ ' hardening constituents erode, make the carbide being precipitated in alloy, or be precipitated
Carbide and boride is clearer displays, avoid the interference of other phases, be conducive to subsequent microexamination, shorten
The time of corrosion improves the uniformity of nickel-base high-temperature single crystal alloy specimen surface corrosion.
2, the present invention uses H3PO4Solution, HNO3Solution and H2SO4The electrolytic etching liquid that solution is configured to, overcomes tradition
The corrosion of immersion corrosion method is uneven and takes long disadvantage, and the corrosion layer on nickel-base high-temperature single crystal alloy surface is uniform after corrosion, does not have
Have and do not erode to and corrode too deep phenomenon, corrosive effect is preferable, is easy to observe, and in combination with scanning electron microscope power spectrum point
Analysis, determines the ingredient of each precipitated phase in nickel-base high-temperature single crystal alloy, by compare carbide and boride precipitation feature and at
Dtex point, further determined the classification of precipitated phase in alloy.
3, method of the invention is simple, and device is easy to get, it is only necessary to which DC power supply and carbon-point make electrode, and corrosive liquid is easy to
It prepares, corrosion process is controllable, flexible and convenient operation.
Below by drawings and examples, the present invention is described in further detail.
Description of the drawings
Fig. 1 is the micro-organization chart of the precipitated phase of 1 nickel-base high-temperature single crystal alloy of the embodiment of the present invention.
Fig. 2 is the EDS energy spectrum diagrams of the precipitated phase of 1 nickel-base high-temperature single crystal alloy of the embodiment of the present invention.
Fig. 3 is the micro-organization chart of the precipitated phase of 2 nickel-base high-temperature single crystal alloy of the embodiment of the present invention.
Fig. 4 is the EDS energy spectrum diagrams of the precipitated phase 1 of 2 nickel-base high-temperature single crystal alloy of the embodiment of the present invention.
Fig. 5 is the EDS energy spectrum diagrams of the precipitated phase 2 of 2 nickel-base high-temperature single crystal alloy of the embodiment of the present invention.
Fig. 6 is the micro-organization chart of the precipitated phase of 3 nickel-base high-temperature single crystal alloy of the embodiment of the present invention.
Fig. 7 is the EDS energy spectrum diagrams of the precipitated phase 1 of 3 nickel-base high-temperature single crystal alloy of the embodiment of the present invention.
Fig. 8 is the EDS energy spectrum diagrams of the precipitated phase 2 of 3 nickel-base high-temperature single crystal alloy of the embodiment of the present invention.
Fig. 9 is the micro-organization chart of the precipitated phase of 4 nickel-base high-temperature single crystal alloy of the embodiment of the present invention.
Figure 10 is the EDS energy spectrum diagrams of the precipitated phase 1 of 4 nickel-base high-temperature single crystal alloy of the embodiment of the present invention.
Figure 11 is the EDS energy spectrum diagrams of the precipitated phase 2 of 4 nickel-base high-temperature single crystal alloy of the embodiment of the present invention.
Specific implementation mode
Embodiment 1
The present embodiment includes the following steps：
Step 1: as cast condition nickel-base high-temperature single crystal alloy is ground successively, polished, cleaned and is dried；The as cast condition nickel
C content in based single-crystal high-temperature alloy is 0.085%；
Step 2: using nickel-base high-temperature single crystal alloy after drying in step 1 as anode, carbon-point is connected as cathode
DC power supply carries out electrolytic etching, waits for that the surface of nickel-base high-temperature single crystal alloy loses metallic luster and one layer of fine and close silvery white occurs
Stop electrolytic etching after corrosion layer；The electrolytic etching agent that the electrolytic etching uses is by H3PO4Solution, HNO3Solution and H2SO4It is molten
Liquid is according to 13:42:46 volume ratio is formulated, the H3PO4Solution, HNO3Solution and H2SO4The mass concentration of solution is distinguished
It is 65%, 15% and 20%；The voltage of the electrolytic etching is 5V, time 11s；
Step 3: the nickel-base high-temperature single crystal alloy in step 2 after electrolytic etching is cleaned and is dried successively, so
Hitachi's S-4800 field emission scanning electron microscopes are used to carry out microexamination to the precipitated phase in nickel-base high-temperature single crystal alloy afterwards.
Fig. 1 is the micro-organization chart of the precipitated phase of the present embodiment nickel-base high-temperature single crystal alloy, as can be seen from Figure 1 this implementation
Occurs apparent blocky white precipitated phase in the microscopic structure of the nickel-base high-temperature single crystal alloy of example.
Fig. 2 is the EDS energy spectrum diagrams of the precipitated phase of the present embodiment nickel-base high-temperature single crystal alloy.
Fig. 1 and Fig. 2 binding analysis is obtained into the chemical composition of precipitated phase, as a result as shown in table 1 below.
The ingredient of the precipitated phase of the nickel-base high-temperature single crystal alloy of 1 embodiment 1 of table
As shown in Table 1, Ta content highests in the precipitated phase of the nickel-base high-temperature single crystal alloy of the present embodiment, mass fraction are super
50% has been crossed, has been Carbide Phases by precipitated phase 1 known to the ingredient of the precipitated phase.
Embodiment 2
The present embodiment includes the following steps：
Step 1: as cast condition nickel-base high-temperature single crystal alloy is ground successively, polished, cleaned and is dried；The as cast condition nickel
C content in based single-crystal high-temperature alloy is 0.072%, B content 0.005%；
Step 2: using nickel-base high-temperature single crystal alloy after drying in step 1 as anode, carbon-point is connected as cathode
DC power supply carries out electrolytic etching, waits for that the surface of nickel-base high-temperature single crystal alloy loses metallic luster and one layer of fine and close silvery white occurs
Stop electrolytic etching after corrosion layer；The electrolytic etching agent that the electrolytic etching uses is by H3PO4Solution, HNO3Solution and H2SO4It is molten
Liquid is according to 13:42:46 volume ratio is formulated, the H3PO4Solution, HNO3Solution and H2SO4The mass concentration of solution is distinguished
It is 65%, 15% and 20%；The voltage of the electrolytic etching is 6V, time 10s；
Step 3: the nickel-base high-temperature single crystal alloy in step 2 after electrolytic etching is cleaned and is dried successively, so
Hitachi's S-4800 field emission scanning electron microscopes are used to carry out microexamination to the precipitated phase in nickel-base high-temperature single crystal alloy afterwards.
Fig. 3 is the micro-organization chart of the precipitated phase of the present embodiment nickel-base high-temperature single crystal alloy, as can be seen from Figure 3 this implementation
There is the precipitated phase of two kinds of different-shapes in the microscopic structure of the nickel-base high-temperature single crystal alloy of example, precipitated phase 1 is that size is larger
Grey massive phase, precipitated phase 2 is the smaller grey corynebacterium phase of size.
Fig. 4 is the EDS energy spectrum diagrams of the precipitated phase 1 of the present embodiment nickel-base high-temperature single crystal alloy, and Fig. 5 is the Ni-based of the present embodiment
The EDS energy spectrum diagrams of the precipitated phase 2 of single crystal super alloy.
Fig. 3, Fig. 4 and Fig. 5 binding analysis are obtained into the chemical composition of precipitated phase, as a result as shown in table 2 below.
The ingredient of the precipitated phase of the nickel-base high-temperature single crystal alloy of 2 embodiment 2 of table
As shown in Table 2, it is rich in Ta in the precipitated phase 1 of the nickel-base high-temperature single crystal alloy of the present embodiment, is rich in precipitated phase 2
Cr by the constituent analysis to precipitated phase 1 and precipitated phase 2 in the alloy, and combines its that pattern is precipitated, it is known that precipitated phase 1 is
Carbide Phases, precipitated phase 2 are boride phase.
Embodiment 3
The present embodiment includes the following steps：
Step 1: as cast condition nickel-base high-temperature single crystal alloy is ground successively, polished, cleaned and is dried；The as cast condition nickel
C content in based single-crystal high-temperature alloy is 0.085%, B content 0.010%；
Step 2: using nickel-base high-temperature single crystal alloy after drying in step 1 as anode, carbon-point is connected as cathode
DC power supply carries out electrolytic etching, waits for that the surface of nickel-base high-temperature single crystal alloy loses metallic luster and one layer of fine and close silvery white occurs
Stop electrolytic etching after corrosion layer；The electrolytic etching agent that the electrolytic etching uses is by H3PO4Solution, HNO3Solution and H2SO4It is molten
Liquid is according to 13:42:46 volume ratio is formulated, the H3PO4Solution, HNO3Solution and H2SO4The mass concentration of solution is distinguished
It is 65%, 15% and 20%；The voltage of the electrolytic etching is 5.5V, time 10s；
Step 3: the nickel-base high-temperature single crystal alloy in step 2 after electrolytic etching is cleaned and is dried successively, so
Hitachi's S-4800 field emission scanning electron microscopes are used to carry out microexamination to the precipitated phase in nickel-base high-temperature single crystal alloy afterwards.
Fig. 6 is the micro-organization chart of the precipitated phase of the present embodiment nickel-base high-temperature single crystal alloy, from fig. 6, it can be seen that this reality
The precipitated phase for occurring two kinds of different-shapes in the microscopic structure of the nickel-base high-temperature single crystal alloy of example is applied, precipitated phase 1 is brilliant white
The massive phase of hexahedron type, precipitated phase 2 are the smaller grey corynebacterium phases of size.
Fig. 7 is the EDS energy spectrum diagrams of the precipitated phase 1 of the present embodiment nickel-base high-temperature single crystal alloy, and Fig. 8 is the Ni-based of the present embodiment
The EDS energy spectrum diagrams of the precipitated phase 2 of single crystal super alloy.
Fig. 6, Fig. 7 and Fig. 8 binding analysis are obtained into the chemical composition of precipitated phase, as a result as shown in table 3 below.
The ingredient of the precipitated phase of the nickel-base high-temperature single crystal alloy of 3 embodiment 3 of table
As shown in Table 3, it is rich in Ta in the precipitated phase 1 of the nickel-base high-temperature single crystal alloy of the present embodiment, is rich in precipitated phase 2
Cr by the constituent analysis to precipitated phase 1 and precipitated phase 2 in the alloy, and combines its that pattern is precipitated, it is known that precipitated phase 1 is
Carbide Phases, precipitated phase 2 are boride phase.
Embodiment 4
The present embodiment includes the following steps：
Step 1: as cast condition nickel-base high-temperature single crystal alloy is ground successively, polished, cleaned and is dried；The as cast condition nickel
C content in based single-crystal high-temperature alloy is 0.078%, B content 0.014%；
Step 2: using nickel-base high-temperature single crystal alloy after drying in step 1 as anode, carbon-point is connected as cathode
DC power supply carries out electrolytic etching, waits for that the surface of nickel-base high-temperature single crystal alloy loses metallic luster and one layer of fine and close silvery white occurs
Stop electrolytic etching after corrosion layer；The electrolytic etching agent that the electrolytic etching uses is by H3PO4Solution, HNO3Solution and H2SO4It is molten
Liquid is according to 13:42:46 volume ratio is formulated, the H3PO4Solution, HNO3Solution and H2SO4The mass concentration of solution is distinguished
It is 65%, 15% and 20%；The voltage of the electrolytic etching is 5V, time 12s；
Step 3: the nickel-base high-temperature single crystal alloy in step 2 after electrolytic etching is cleaned and is dried successively, so
Hitachi's S-4800 field emission scanning electron microscopes are used to carry out microexamination to the precipitated phase in nickel-base high-temperature single crystal alloy afterwards.
Fig. 9 is the micro-organization chart of the precipitated phase of the present embodiment nickel-base high-temperature single crystal alloy, as can be seen from Figure 9 this implementation
There is the precipitated phase of two kinds of different-shapes in the microscopic structure of the nickel-base high-temperature single crystal alloy of example, precipitated phase 1 is that size is larger
Massive phase, and the smaller thin rod shape precipitated phase 2 of size has been precipitated around precipitated phase 1.
Figure 10 is the EDS energy spectrum diagrams of the precipitated phase 1 of the present embodiment nickel-base high-temperature single crystal alloy, and Figure 11 is that the present embodiment is Ni-based
The EDS energy spectrum diagrams of the precipitated phase 2 of single crystal super alloy.
Fig. 9, Figure 10 and Figure 11 binding analysis are obtained into the chemical composition of precipitated phase, as a result as shown in table 4 below.
The ingredient of the precipitated phase of the nickel-base high-temperature single crystal alloy of 4 embodiment 4 of table
As shown in Table 4, Ta, thin bar are rich in the large scale bulk precipitated phase 1 of the nickel-base high-temperature single crystal alloy of the present embodiment
It is rich in Cr in the precipitated phase 2 of shape, is carbide by precipitated phase 1 known to the ingredient and pattern of precipitated phase, precipitated phase 2 is boronation
Object.
The above is only presently preferred embodiments of the present invention, is not imposed any restrictions to the present invention.It is every according to invention skill
Art essence still falls within technical solution of the present invention to any simple modification, change and equivalence change made by above example
Protection domain in.
Claims (3)
1. a kind of electrolytic etching method of nickel-base high-temperature single crystal alloy, which is characterized in that this approach includes the following steps：
Step 1: as cast condition nickel-base high-temperature single crystal alloy is ground successively, polished, cleaned and is dried；The Ni-based list of as cast condition
The mass content of C is that the mass content of C in 0.085% or as cast condition nickel-base high-temperature single crystal alloy is in brilliant high temperature alloy
The mass content that the mass content of 0.072%, B are C in 0.005% or as cast condition nickel-base high-temperature single crystal alloy is 0.085%, B
Mass content be C in 0.010% or as cast condition nickel-base high-temperature single crystal alloy mass content be 0.078%, B quality contain
Amount is 0.014%；
Step 2: using nickel-base high-temperature single crystal alloy after drying in step 1 as anode, carbon-point connects direct current as cathode
Power supply carries out electrolytic etching, waits for that the surface of nickel-base high-temperature single crystal alloy loses metallic luster and one layer of fine and close silvery white corrosion occurs
Stop electrolytic etching after layer；The electrolytic etching agent that the electrolytic etching uses is by H3PO4Solution, HNO3Solution and H2SO4Solution is pressed
According to 13:42:46 volume ratio is formulated, the H3PO4Solution, HNO3Solution and H2SO4The mass concentration of solution is respectively
65%, 15% and 20%；
Step 3: cleaned and dried successively the nickel-base high-temperature single crystal alloy in step 2 after electrolytic etching, then into
Row microexamination.
2. a kind of electrolytic etching method of nickel-base high-temperature single crystal alloy according to claim 1, which is characterized in that step 2
Described in electrolytic etching voltage be 5V~6V, the time be 10s~12s.
3. a kind of electrolytic etching method of nickel-base high-temperature single crystal alloy according to claim 2, which is characterized in that the electricity
The voltage of solution corrosion is 5V, time 12s.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109738263A (en) * | 2018-12-18 | 2019-05-10 | 海洋石油工程股份有限公司 | The detection method of corrosion resistant alloy welding point macroscopic view metallographic |
| 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 |
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| 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 |
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