CN111809128A - Method for rapidly dissolving and deforming Laves phase in high-temperature alloy ingot by pulse current - Google Patents
Method for rapidly dissolving and deforming Laves phase in high-temperature alloy ingot by pulse current Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
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- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
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- C22C19/03—Alloys based on nickel or cobalt based on nickel
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Abstract
The invention discloses a method for rapidly dissolving a Laves phase in a deformed high-temperature alloy ingot by pulse current, which comprises the following steps: carrying out pulse current external field treatment on the deformed high-temperature alloy ingot, wherein the treatment parameters are as follows: the pulse frequency is 25000 to 35000Hz, and the current density is 1A/mm2~100A/mm2The method provided by the invention has the advantages that: the Laves phase in the material can be completely dissolved at a lower temperature in a very short time, the time is short, the temperature is low, the operation is simple, the energy consumption can be greatly reduced, and the requirements of the current industrial green development planning are met. In addition, the plasticity of the alloy can be improved, the alloy can be used for deformation high-temperature alloy treatment, the subsequent cogging and forging processes are facilitated, and a new method is provided for the preparation of the high-temperature alloy turbine disc.
Description
Technical Field
The invention relates to the technical field of wrought superalloy, in particular to a method for rapidly dissolving a Laves phase in a wrought superalloy ingot by pulse current.
Background
The wrought superalloy becomes a key material for parts such as aerospace, ship engines, gas turbine disks and the like due to excellent high temperature resistance, creep resistance, oxidation resistance and the like. The integral blade disc with the integrated disc and blade design is a novel structure of a modern aeroengine and is also the selection trend of an engine with a high thrust-weight ratio, and the diameter of a disc forging is increased by the integration of the disc and the blade of the integral blade disc. However, in order to manufacture large-size parts, large-size ingots must be produced so as to obtain a sufficient deformation ratio, and under the existing conditions, the element segregation degree is further increased by smelting large ingots, so that a Laves phase with higher number density is generated among the ingot dendrites, and adverse effects are generated on the subsequent cogging, forging and heat treatment of the turbine disc.
The Laves phase, which is one of the brittle topologically close-packed phases, has a melting point significantly lower than that of the γ matrix, and is a low-melting phase. During high temperature thermal processing, especially when the temperature is higher than the melting point of the Laves phase, incipient melting and pore formation easily occur. The Laves phase must therefore be completely dissolved. At present, the most effective way for dissolving the low-melting-point phase in the alloy ingot is homogenization heat treatment for obtaining high-quality bars, for example, the Chinese patent with the publication number of CN107523772B discloses a homogenization process for U720Li high-temperature alloy, and the invention is to completely dissolve the low-melting-point phase-Ni in the U720Li alloy ingot5The Zr phase needs to be subjected to heat treatment for 20 hours or more under the high temperature condition of 1080 ℃ to 1120 ℃ respectively. For another example, Chinese patent with application publication No. CN103361585A discloses a homogenization process of high-alloying GH742 high-temperature alloy, which is to keep the temperature at 1050-1100 ℃ for 40h to dissolve low-melting-point phases, namely Laves phase and Ni, existing in the alloy ingot5Ce, and the like.
The GH4169D alloy is a newly developed novel 700-DEG C nickel-based wrought superalloy turbine disc material and 760-DEG C superalloy annular part material, and the successful development of the alloy effectively fills the long-existing blank between the current GH4169 alloy for 650 ℃ and the GH4738 alloy for 750 ℃. However, the most outstanding problem in the GH4169D alloy production process is the generation of a large amount of low-melting-point Laves phase during ingot solidification, which causes a drastic reduction in impact property and plasticity of the material, and is highly likely to cause cracking during ingot cogging and forging. Therefore, the presence of Laves phases is not allowed in the finished material. However, the generation of Laves phases in alloy ingots is inevitable.
In order to realize the complete re-dissolution of the Laves phase in the GH4169D alloy ingot and simultaneously avoid the situation that the initial melting of the Laves phase hinders the diffusion of segregation element atoms, the Laves phase can be completely eliminated only by placing the ingot in a muffle furnace for continuously preserving the temperature for more than 20 hours at the temperature of more than 1100 ℃. However, although the Laves phase can be well dissolved by the method, the conventional homogenization process has high treatment temperature, long treatment time and complicated flow. Therefore, it is very important to explore a method with low energy consumption and high efficiency to realize the Laves phase redissolution in the alloy ingot.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for rapidly dissolving a Laves phase in a deformed high-temperature alloy ingot by pulse current, which has the advantages that the deformed high-temperature alloy is treated by the pulse current, the Laves phase formed in the solidification final stage of the deformed high-temperature alloy can be completely dissolved in a very short time, the time is short, the operation is simple, and favorable conditions are created for cogging and forging in the later period.
In order to achieve the purpose, the invention provides the following technical scheme: a method for rapidly dissolving and deforming Laves phase in a high-temperature alloy ingot by pulse current comprises the following steps: carrying out pulse current external field treatment on the deformed high-temperature alloy ingot, wherein the treatment parameters are as follows: the pulse frequency is 25000 to 35000Hz, and the current density is 1A/mm2～100A/mm2。
By adopting the technical scheme, based on the electrochemical property difference between the Laves phase and the strengthening phase in the deformed high-temperature alloy ingot and the matrix, under the action of directionally flowing drift electrons, the method breaks the thermal diffusion limit of atoms in the traditional heat treatment, and can realize the complete dissolution of the Laves phase in the deformed high-temperature alloy in a short time. Compared with the traditional heat treatment which needs more than 20 hours, the method adopting the pulse current can realize the complete dissolution of the Laves phase only by 30 minutes, and greatly shortens the time needed by the complete dissolution of the Laves phase in the ingot.
In addition, the pulse current external field parameters provided by the invention are adopted to process the deformed high-temperature alloy ingot, the working condition temperature of the pulse current external field is reduced by at least 100 ℃ compared with the traditional heat treatment process, and the complete dissolution of the Laves phase can be realized at 1000 ℃.
Moreover, after the deformed high-temperature alloy is subjected to the pulse current treatment, the obtained high-temperature alloy has better plasticity, and can improve micro defects such as microcracks, holes and the like in the high-temperature alloy.
Compared with the traditional heat treatment, the method provided by the invention can realize complete dissolution of the Laves phase in a very short time at a lower temperature, and the obtained high-temperature alloy has good plasticity, is more beneficial to the subsequent cogging and forging processes of the high-temperature alloy, so that the energy consumption in the whole process is sharply reduced, the method meets the current concept and requirement of green development, can bring huge economic benefits, and has a wide development space.
The invention is further configured to: the pulse current treatment time is 5 min-10 h.
The invention is further configured to: the specific operation steps of the pulse current external field treatment are as follows:
s1, connecting the high-temperature alloy to two ends of a pulse power supply through a pure copper wire and a pure copper clamp;
and S2, switching on a pulse power supply after setting parameters, continuously applying pulses for 5min to 10h, and air-cooling to room temperature after switching off the power supply.
The invention is further configured to: the pulsed current external field treatment is carried out at room temperature.
The invention is further configured to: the deformed high-temperature alloy ingot is a nickel-based high-temperature alloy ingot.
The invention is further configured to: the nickel-based high-temperature alloy cast ingot can be obtained by a two-combined smelting process or a three-combined smelting process, and is preferably prepared by the nickel-based high-temperature alloy cast ingot by the three-combined smelting process.
The invention is further configured to: the nickel-based superalloy ingot is a GH4169D novel nickel-based superalloy ingot.
By adopting the technical scheme, the method provided by the invention is applied to the GH4169D novel nickel-based high-temperature alloy cast ingot, and the problems that the impact property and plasticity of an alloy material are sharply reduced and cracking is easily caused in the processes of cogging and forging of the cast ingot due to the generation of a large amount of low-melting-point Laves phases in the solidification process of the GH4169D alloy cast ingot are solved, so that the cracking problem in the processes of cogging and forging of the GH4169D novel nickel-based high-temperature alloy is solved, and the alloy forging meeting the conditions is obtained.
In conclusion, the invention has the following beneficial effects:
1. the pulse current external field provided by the invention can realize the dissolution of the Laves phase in the deformed high-temperature alloy, and can realize the purpose in a very short time and at a lower temperature, and moreover, the high-temperature alloy obtained by the invention has better plasticity, is more beneficial to the subsequent cogging and forging process of the high-temperature alloy, so that the energy consumption in the whole process is sharply reduced, meets the current concept and requirements of green development, can bring huge economic benefits, and has a wide development space;
2. according to the invention, the Laves phase in the deformed high-temperature alloy can be completely dissolved in a short time by utilizing the electrochemical property difference of the Laves phase and the strengthening phase and the matrix under the action of the pulse current external field. Compared with the traditional heat treatment, the time for dissolving the Laves phase can be reduced to 0.5h from 20h by adopting a pulse current method;
3. the pulse current external field parameters provided by the invention are adopted to process the deformed high-temperature alloy cast ingot, the working condition temperature of the pulse current external field is reduced by at least 100 ℃ compared with the traditional heat treatment process, and the complete dissolution of the Laves phase can be realized at 1000 ℃;
4. after the deformed high-temperature alloy is subjected to the pulse current treatment, the obtained high-temperature alloy has better plasticity, can improve micro defects such as microcracks, holes and the like in the high-temperature alloy, and is more beneficial to the subsequent cogging and forging processes;
5. the method provided by the invention is applied to the GH4169D novel nickel-based high-temperature alloy cast ingot, and solves the problems that impact property and plasticity of an alloy material are sharply reduced and cracking is easily caused in the processes of cogging and forging of the cast ingot due to the generation of a large amount of low-melting-point Laves phases in the solidification process of the GH4169D alloy cast ingot, so that the problem that the GH4169D novel nickel-based high-temperature alloy is easy to crack in the processes of cogging and forging is solved, and finally, the alloy forging meeting the high-temperature use at 700 ℃ is obtained.
Drawings
FIG. 1 is a diagram showing a gold phase diagram, wherein (a) is a Laves phase distribution gold phase diagram in an as-cast superalloy, (b) is a Laves phase distribution gold phase diagram in example 2, (c) is a Laves phase distribution gold phase diagram in comparative example 2, and (d) is a Laves phase distribution gold phase diagram in comparative example 3;
FIG. 2 shows the results of room temperature plasticity of the high temperature alloys of examples 1-2 and comparative examples 1-3 of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and those not specifically noted in the examples are carried out according to conventional conditions or conditions suggested by the manufacturer.
The invention provides a method for rapidly dissolving a Laves phase in a deformed high-temperature alloy ingot by pulse current, which comprises the following steps: carrying out pulse current external field treatment on the deformed high-temperature alloy ingot, wherein the treatment parameters are as follows: the pulse frequency is 25000 to 35000Hz, and the current density is 1A/mm2～100A/mm2The invention is further configured to: the pulse current processing time is 5 min-10 h, and the specific operation steps are as follows:
s1, connecting the high-temperature alloy to two ends of a pulse power supply through a pure copper wire and a pure copper clamp;
and S2, setting pulse frequency, current and voltage parameters, switching on a pulse power supply, continuously applying pulses for 5 min-10 h, and switching off the power supply and then cooling to room temperature in air.
Wherein, in the step S2, the current density is ensured to be constant and reach 1A/mm by two parameters of current and voltage2～100A/mm2And (4) finishing.
The method provides a scheme for dissolving the Laves phase in the high-temperature alloy ingot by a more efficient and energy-saving method, and the mechanism is that the Laves phase dissolution is promoted mainly by means of the difference of the electrochemical properties of the Laves phase in the deformed high-temperature alloy and the strengthening phase and the matrix, so that the method can not only be applied to the nickel-based high-temperature alloy, but also be used for dissolving the Laves phase as long as the Laves phase exists in the alloy and the Laves phase in the alloy has the difference of the electrochemical properties of the strengthening phase and the matrix, and the effect of completely dissolving the Laves phase is achieved by adjusting the pulse frequency and the current density. The wrought superalloy in the following examples and comparative examples is prepared by taking GH4169D novel nickel-based wrought superalloy as an example, and the chemical composition of the GH4169D novel nickel-based superalloy is as follows: zr: 0.001 to 0.1 wt%, C: less than or equal to 0.1 wt%, Cr: 12-20 wt%, Mo: 4 wt% or less, W: less than or equal to 6 wt%, Co: 5-12 wt%, Fe: not more than 14 wt%, Nb: 4-8 wt%, Al: 0.6-2.6 wt%, Ti: 0.4-1.4 wt%, P: 0.003 to 0.03 wt%, B: 0.003 to 0.015 wt%, and the balance being Ni.
The above process is illustrated below with reference to specific examples.
Example 1
A method for rapidly dissolving and deforming Laves phase in a high-temperature alloy ingot by pulse current comprises the following steps: the pulse current external field treatment is carried out on the deformed high-temperature alloy cast ingot, and the specific operation steps are as follows:
s1, sequentially polishing the surfaces of the GH4169D novel nickel-based high-temperature alloy cast ingots by 180-mesh, 600-mesh, 1000-mesh, 1500-mesh and 2000-mesh abrasive papers until no visible defects exist, and then connecting the GH4169D alloy cast ingots to two ends of a pulse power supply through a pure copper lead and a pure copper clamp;
s2, setting the pulse frequency to be 30000Hz, and setting the current and voltage parameters to ensure that the current density is 16.35A/mm2And continuously performing pulse treatment for 30min at room temperature, then cutting off the power supply, and then cooling to room temperature in air. In the whole treatment process, the surface temperature of the superalloy after the application of the pulsed external field was measured by a K-type thermocouple to be 900 ℃.
Example 2
A method for rapidly dissolving and deforming Laves phase in a superalloy ingot by pulse current selects GH4169D novel nickel-based superalloy ingot with the same structural state and mechanical property as those in example 1, and is carried out according to the method in example 1, except that,
the pulse current external field treatment is carried out on the deformed high-temperature alloy cast ingot, and the specific operation steps are as follows:
s1, sequentially polishing the surfaces of the GH4169D novel nickel-based high-temperature alloy cast ingots by 180-mesh, 600-mesh, 1000-mesh, 1500-mesh and 2000-mesh abrasive paper until no visible defects exist, and then connecting the GH4169D alloy rectangular cast ingots to two ends of a pulse power supply through a pure copper lead and a pure copper clamp;
s2, setting the pulse frequency to be 30000Hz, and setting the current and voltage parameters to ensure that the current density is 18.5A/mm2And continuing pulse treatment at room temperature for 30min, and then cutting off the power supply to cool to room temperature. In the whole treatment process, the surface temperature of the superalloy after application of the pulsed external field was measured by a K-type thermocouple to be 1000 ℃.
Example 3
A method for rapidly dissolving and deforming Laves phase in a superalloy ingot by pulse current selects GH4169D novel nickel-based superalloy ingot with the same structural state and mechanical property as those in example 2, and is carried out according to the method in example 2, wherein the difference is that the pulse current processing parameters in step S2 are as follows:
setting the current and voltage parameters so that the current density is 1A/mm2The pulse processing time was 10 h.
Example 4
A method for rapidly dissolving and deforming Laves phase in a superalloy ingot by pulse current selects GH4169D novel nickel-based superalloy ingot with the same structural state and mechanical property as those in example 2, and is carried out according to the method in example 2, wherein the difference is that the pulse current processing parameters in step S2 are as follows:
setting the current and voltage parameters so that the current density is 100A/mm2The pulse treatment time was 5 min.
Example 5
A method for rapidly dissolving a Laves phase in a deformed high-temperature alloy ingot by pulse current is carried out according to the method in the embodiment 2 by selecting a GH4169D novel nickel-based high-temperature alloy ingot with the same structural state and mechanical property as those in the embodiment 2, and the difference is that the pulse frequency in the pulse current processing parameters in the step S2 is 35000 Hz.
Example 6
A method for rapidly dissolving a Laves phase in a deformed high-temperature alloy ingot by pulse current is carried out according to the method in the embodiment 2 by selecting a GH4169D novel nickel-based high-temperature alloy ingot with the same structural state and mechanical property as those in the embodiment 2, and the difference is that the pulse frequency in the pulse current processing parameters in the step S2 is 25000 Hz.
Comparative example 1
In the comparative example, a GH4169D novel nickel-based superalloy ingot with the same structural state and mechanical property as those in example 1 is selected and subjected to heat treatment in a muffle furnace, wherein the heat treatment parameters are as follows: heating to 900 deg.C at a rate of 5 deg.C/min, and maintaining for 30 min.
Comparative example 2
In the comparative example, a GH4169D novel nickel-based superalloy ingot with the same structural state and mechanical property as those in example 1 is selected and subjected to heat treatment in a muffle furnace, wherein the heat treatment parameters are as follows: heating to 1000 deg.C at a rate of 5 deg.C/min, maintaining for 30min, and air cooling to room temperature.
Comparative example 3
In the comparative example, a GH4169D novel nickel-based superalloy ingot with the same structural state and mechanical property as those in example 1 is selected and subjected to heat treatment in a muffle furnace, wherein the heat treatment parameters are as follows: heating to 1100 deg.C at a rate of 5 deg.C/min, maintaining for 24 hr, and air cooling to room temperature.
Performance detection
1. Observation of Laves phase redissolution
The pulsed current treated GH4169D alloy ingots of examples 1-6 and the heat treated GH4169D alloy ingots of comparative examples 1-3 were observed for Laves phase re-dissolution, specifically, the Laves phase re-dissolution of the ingots treated by examples and comparative examples was observed by OLYMPUS GX71 metallographic optical microscope: taking the as-cast state and the pulse respectivelyPunching the high-temperature alloy in a processing state and a heat treatment state, sequentially grinding the surface of the high-temperature alloy by 180-mesh, 600-mesh, 1000-mesh, 1500-mesh and 2000-mesh abrasive paper until the scratch direction is consistent, and carrying out electrolytic corrosion after mechanical polishing: the corrosive liquid is 16g of CrO3+10ml H2SO4+170ml H3PO4(ii) a The direct current voltage is 5V, and the electrolytic corrosion time is 5-7 seconds. And observing the Laves phase distribution in the cast state, the embodiment and the high-temperature alloy in the comparative example through a metallographic microscope.
It can be observed that the Laves phase in the ingot subjected to the pulse treatment in the example of the present invention is dissolved, and referring to fig. 1 again, (a) in fig. 1 is the Laves phase distribution in the as-cast ingot in the example and the comparative example, (b) is the Laves phase distribution in the ingot subjected to the pulse current treatment (1000 ℃/30min) in the example 2, (c) is the Laves phase distribution in the ingot subjected to the conventional heat treatment (1000 ℃/30min) in the comparative example 2, and (d) is the Laves phase distribution in the ingot subjected to the conventional heat treatment (1100 ℃/24h) in the comparative example 3, wherein the heat treatment parameters in the comparative example 3 are the heat treatment parameters commonly used in the GH4169D nickel-based superalloy industry, it can be seen that, in the pulse parameters (pulse frequency 30000Hz, current density 18.5A/mm)2) The effect obtained by the next treatment for 30min can be comparable with the effect obtained by the heat treatment process commonly used in the industry in the field.
2. Plasticity detection
The room temperature plasticity tests were carried out at room temperature (23 ℃) on the as-cast ingots of the novel nickel-base superalloys of the examples and comparative examples GH 4169D. The elongation a of the ingot before treatment was 12%. Also, the pulsed current-treated ingots and the heat-treated ingots obtained in examples 1 to 2 and comparative examples 1 to 3 were subjected to a room temperature plasticity test at room temperature (23 ℃). Plasticity test the elongation A is detected by a tensile test according to GB/T228.1-2010 metal material room temperature tensile test method, and the detection results are shown in the following table 1.
Table 1:
by plotting Table 1 above, and referring to FIG. 2, the plasticity of the ingot after pulse treatment can be seenIs remarkably improved. As a result of examination with reference to example 2 and comparative examples 2 and 3, it was found that the pulsed current treatment (pulse frequency 30000Hz, current density 18.5A/mm) was performed in comparison with the conventional heat treatment2) The elongation of the post-alloy cast ingot is 44.5 percent, the alloy plasticity is highest and is 37 percent higher than that of the alloy subjected to the common industrial heat treatment in the prior field, and the post-alloy cast ingot is more beneficial to the post-alloy cogging and forging processes.
In summary, compared to the conventional thermal treatment that dissolves the Laves phase in the wrought high temperature alloy only by increasing the atomic diffusion rate under high temperature conditions, the pulsed current treatment facilitates the dissolution of the Laves phase by virtue of the electrochemical property difference between the Laves phase and the strengthening phase and the matrix in the wrought high temperature alloy. The method provided by the invention can realize the complete dissolution of the Laves phase in the ingot casting only by 30min, and the treatment temperature is reduced, namely the complete dissolution of the Laves phase is realized at 1000 ℃. Moreover, the high-temperature alloy obtained by the treatment of the invention has better plasticity, and is more beneficial to the subsequent cogging and forging process of the high-temperature alloy, so that the problem that the GH4169D novel nickel-based high-temperature alloy is easy to crack in cogging and forging is solved, and the alloy forging meeting the use requirement under the high-temperature condition of 700 ℃ is finally obtained. The energy consumption in the whole process is sharply reduced, the current concept and requirements of green development are met, and the method can bring huge economic benefits and has wide development space.
The above description is only a specific embodiment of the present invention for dissolving the Laves phase in a certain nickel-based wrought superalloy ingot. The method is also suitable for other metal ingots and ingots with other sizes, and only corresponding parameters are required to be adjusted. The scope of the present invention is not limited thereto, and any person skilled in the art can substitute similar materials, devices or adjust related technical parameters within the technical scope of the present invention, according to the technical solution of the present invention and the inventive concept thereof, and shall fall within the scope of the present invention.
Claims (7)
1. A method for rapidly dissolving a Laves phase in a deformed high-temperature alloy ingot by using pulse current is characterized by comprising the following steps: pulse current external field is carried out on the deformed high-temperature alloy ingotThe processing parameters are as follows: the pulse frequency is 25000 to 35000Hz, and the current density is 1A/mm2~100A/mm2。
2. The method for rapidly dissolving the Laves phase in the deformed high-temperature alloy ingot by the pulse current according to claim 1, wherein the pulse current treatment time is 5 min-10 h.
3. The method for rapidly dissolving the Laves phase in the deformed high-temperature alloy ingot by the pulse current according to claim 1, wherein the pulse current external field treatment comprises the following specific operation steps:
s1, connecting the high-temperature alloy to two ends of a pulse power supply through a pure copper wire and a pure copper clamp;
and S2, switching on a pulse power supply after setting parameters, continuously applying pulses for 5 min-10 h, and air-cooling to room temperature after switching off the power supply.
4. The method for rapidly dissolving the Laves phase in the deformed high-temperature alloy ingot by the pulse current according to claim 1, wherein the pulse current external field treatment is carried out at room temperature.
5. The method of claim 1, wherein the wrought superalloy ingot is a nickel-based superalloy ingot.
6. The method for rapidly dissolving the Laves phase in the wrought superalloy ingot by the pulse current according to claim 5, wherein the nickel-based superalloy ingot is produced by a triple smelting process.
7. The method for rapidly dissolving the Laves phase in the wrought superalloy ingot by the pulse current as claimed in claim 5, wherein the nickel-base superalloy ingot is a GH4169D new nickel-base superalloy ingot.
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| CN110747420A (en) * | 2019-11-29 | 2020-02-04 | 北京科技大学 | Method for rapidly repairing nickel-based superalloy turbine disc at last service stage |
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| CN101311277A (en) * | 2007-05-25 | 2008-11-26 | 丹阳市精密合金厂 | Homogenization treatment process for high-temperature alloyed steel ingot |
| CN106077647A (en) * | 2016-07-27 | 2016-11-09 | 湖南大学 | A kind of laser gain material controls the method for fragility Laves phase during manufacturing nickel base superalloy |
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