CN111575619A - Method for rapidly eliminating dendrite segregation in deformed high-temperature alloy ingot by pulse current - Google Patents
Method for rapidly eliminating dendrite segregation in deformed high-temperature alloy ingot by pulse current Download PDFInfo
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Abstract
The invention relates to the technical field of turbine disk preparation, and provides a method for rapidly eliminating dendritic crystal segregation (mainly aiming at the second stage of traditional homogenization heat treatment) in a nickel-based wrought superalloy ingot for a turbine disk by using pulse current. The diffusion capacity of segregation element atoms under the action of coupling of pulse current and joule heat is greatly enhanced, and further dendritic crystal segregation under the action of pulse current external field is rapidly eliminated. The parameter range of the pulse external field treatment of the invention is as follows: the frequency is 30000Hz, the voltage is 0.1V-100V, and the current density is 1A/mm2～150A/mm2The treatment time is 5 min-20 h. Compared with the traditional long-time high-temperature treatment with a single thermal field, the method can quickly eliminate dendritic crystal segregation under proper pulse parameters, realize the uniform distribution of segregation elements, and the treated high-temperature alloy has lower strength and is more beneficial to the subsequent cogging forging process. Moreover, the technical means of the invention is green and energy-savingThe novel method accords with the current concept and requirement of green development and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of high-temperature alloy turbine disk preparation, and particularly relates to a novel method for rapidly eliminating dendritic crystal segregation in a nickel-based deformed high-temperature alloy ingot for a turbine disk by a pulse current external field.
Technical Field
Since the birth of high-temperature alloy in the last century, the huge demand of high-temperature materials for hot-end parts of aeroengines continuously pushes the rapid development of high-temperature alloy. Among the three major types of superalloys, wrought, cast and powdered, wrought superalloys are most widely used. The deformed high-temperature alloy is mainly used for manufacturing high-temperature components such as turbine discs, combustion chambers and the like of aircraft engines. The turbine disk is an important part in an engine, the working temperature is high, and the stress condition of each part is extremely complex. Therefore, high temperature alloys for turbine disks are required to have high strength, plasticity, long life, creep resistance, corrosion resistance, oxidation resistance, long-term structure stability, and the like. However, the wrought superalloy has a high degree of alloying and contains a large amount of insoluble elements. In the final stage of solidification of the high-temperature alloy, serious dendrite segregation is easy to generate, so that the structure and the mechanical property are uneven, and the performance of the turbine disk is often not in line with the service requirement. Therefore, dendrite segregation is not allowed to exist in the final material.
Under the existing smelting conditions, the existence of dendritic crystal segregation in the deformed high-temperature alloy ingot is inevitable. In order to obtain a good quality bar and improve the quality of the turbine disk, dendritic segregation in the alloy ingot should be completely eliminated. Currently, the most effective way to eliminate dendrite segregation is homogenization heat treatment. The patent (CN 107523772B) discloses a homogenization process of U720Li high-temperature alloy, and in order to solve the problem of element segregation, the whole homogenization process flow needs to continuously keep the temperature of an alloy ingot at 1200 ℃ for 72 hours. The patent (CN 103276333A) discloses a homogenizing treatment method of a GH4738 nickel-base superalloy ingot, and in order to solve the problem that a great amount of cast dendritic structures exist in the GH4738 ingot, the ingot needs to be placed in an annealing furnace to be continuously annealed for 20-50 h under the high-temperature condition of 1160-1200 ℃.
The nickel-based wrought superalloy material used in the invention has a grade GH 4169D. GH4169D cast ingot obtained by triple smelting has a large amount of low-melting-point brittle phase and typical dendritic segregation. The traditional homogenization method is divided into two stages: stage one, keeping the temperature above 1100 ℃ for at least 20h to eliminate the low-melting brittle Laves phase; and in the second stage, the temperature is kept above 1160 ℃ for at least 70h to eliminate the interdendritic element segregation. In order to show the positive significance of the pulse current intervention means on the elimination of dendrite segregation in alloy ingots, the raw materials of the invention are subjected to a phase treatment of the traditional homogenization process to eliminate low-melting-point phases (collectively referred to as a phase homogenization heat treatment state). At present, in order to completely eliminate dendritic segregation in GH4169D alloy ingots, high-temperature heat treatment with the temperature of more than 1100 ℃ and the time of more than 70 hours is generally adopted in the industry. Through the method, dendritic crystal segregation can be well eliminated, but the traditional heat treatment method is high in treatment temperature, long in treatment time, complex in flow and high in energy consumption, and does not meet the requirements of current industrial green development planning. Therefore, there is a need to find a new treatment method to eliminate dendrite segregation with high efficiency and low energy consumption.
Disclosure of Invention
After dissolving the low-melting-point brittle phase in the GH4169D alloy ingot, the traditional heat treatment needs to be carried out for a long time of heat preservation for 70-80 hours at high temperature to completely eliminate the dendrite element segregation. The technical means used by the invention, namely pulse current, is an instantaneous high-energy input mode. Different from the traditional heat treatment single thermal field, the pulse current external field accelerates the diffusion rate of segregation element atoms due to the coupling effect of pulse current and joule heat, breaks the thermal diffusion limit, and obviously accelerates the elimination of dendritic crystal segregation in the ingot, which is a novel treatment means completely different from the heat treatment.
Aiming at the defects existing in the process of eliminating dendrite segregation by traditional heat treatment, the invention provides a brand new technical means for quickly eliminating dendrite segregation in the ingot under the non-traditional pulse current external field. By adopting the technical scheme of the invention, under the appropriate pulse parameters, the complete elimination of dendrite segregation can be realized only by 30 min. In addition, after the pulse current external field is applied, the electron wind power brought by high-speed drift electrons can not only accelerate the diffusion rate of segregation element atoms, but also improve the mobility of defects in the metal material, thereby realizing the improvement of the plasticity of the material. Therefore, compared with the traditional homogenization heat treatment, the homogenization material obtained by the technical means of the invention has lower room temperature yield strength. In consideration of the integrity of the process, the high-temperature alloy treated by the pulse current external field is more beneficial to the subsequent cogging and forging processes. The invention carries out pulse external field treatment on the small-size high-temperature alloy material subjected to one-stage homogenization heat treatment. For the ingots with different sizes, the pulse external field treatment effect same as that of the small-size high-temperature alloy material can be achieved only by correspondingly adjusting two parameters of voltage and current to ensure constant current density in the ingots.
The technical scheme of the invention is as follows:
the method carries out pulse current treatment on the nickel-based wrought superalloy ingot which is subjected to the traditional one-stage homogenization heat treatment (namely, the low-melting-point phase is eliminated, but serious element segregation still exists), and the method greatly shortens the time required for thoroughly eliminating the dendrite segregation in the ingot; the pulse processing parameters are as follows: the frequency is 30000Hz, the voltage is 0.1V-100V, and the current density is 1A/mm2～150A/mm2The treatment time is 5 min-20 h. In order to show the positive effect of the pulse external field on dendrite segregation elimination, the temperature is measured by a K-type thermocouple welded in the center of the surface of the high-temperature alloy, and equivalent heat treatment is carried out in a muffle furnace.
The method for rapidly eliminating dendrite segregation in the deformed high-temperature alloy ingot by the pulse current comprises the following specific steps:
(1) the nickel-based deformed superalloy material is fixed by a pure copper clamp and then connected to two ends of a pulse power supply through a pure copper wire;
(2) after setting parameters, switching on a pulse power supply, and enabling the temperature of the central area of the high-temperature alloy to reach the expected treatment temperature within 10 s; continuously applying pulses for 5 min-20 h, and air-cooling to room temperature after the power supply is cut off.
Further, the nickel-based wrought superalloy is a GH4169D alloy cast ingot, and is obtained by a triple smelting process: vacuum induction melting, electroslag remelting and vacuum consumable remelting, and a first stage of homogenization heat treatment is carried out to re-dissolve the low-melting brittle phase.
Furthermore, the pulse current output device is a high-frequency pulse power supply, and different processing effects can be obtained by adjusting voltage and current.
Further, the whole process of the pulsed current external field treatment is carried out under the condition of room temperature.
Further, the temperature rise by the generated joule heat is considered to be uniform over the section of the superalloy material when the pulse current is applied.
Further, after the pulse current is applied, the rapid elimination of dendrite segregation benefits from the coupling effect of the pulse current and the joule heat; compared with a pure thermal field, the pulse current has a remarkable advantage in eliminating dendritic segregation in the alloy ingot.
Further, the size of the high-temperature alloy in the pulse current external field treatment state for analyzing the dendrite segregation elimination condition is 30 × 4 × 1.5.5 mm3The rectangular deformation zone of the high-temperature alloy in the pulse current external field treatment state for testing the tensile strength at room temperature is 20 × 4 × 1.5.5 mm3。
Further, because the copper is fast in heat dissipation, the temperature of the clamping end parts on the two sides of the high-temperature alloy is lower than the processing temperature, and therefore, in the subsequent structure observation process, the elimination condition of dendritic crystal segregation in the central region of the high-temperature alloy in the pulse current external field processing state is mainly concerned.
Compared with the traditional heat treatment, the invention has the following beneficial effects:
1. the time required for eliminating dendrite segregation is greatly shortened. In order to diffuse the segregation elements in the alloy ingot to be uniformly distributed, the traditional heat treatment needs to keep the temperature for about 100 hours at a high temperature in two stages. Compared with the traditional heat treatment means, the pulse current breaks the thermal diffusion limit of the segregation element atoms, and the same effect can be achieved only by treating for 30min under proper parameters. Therefore, the pulse current external field has obvious promotion effect on elimination of dendrite segregation.
2. The temperature required to eliminate dendrite segregation is reduced. The complete elimination of dendrite segregation can be realized when a pulse external field is applied under the condition of 1050 ℃. Compared with the traditional heat treatment means, the pulse current external field treatment reduces the working condition temperature by over 100 ℃.
3. The simplification of the treatment process, the shortening of the treatment time and the reduction of the treatment temperature greatly reduce the energy consumption required by the whole process and bring unpredictable economic benefits.
4. The high-temperature alloy obtained by adopting the technical scheme of the invention has lower strength than that of the high-temperature alloy treated by the traditional homogenization method, and is more beneficial to the subsequent cogging and forging processes.
Drawings
Fig. 1 shows a metallographic photograph. Wherein, (a) is a metallographic photograph of dendritic crystal distribution in a high-temperature alloy in a stage of homogenization heat treatment state, (b) is a metallographic photograph of dendritic crystal distribution in example 3, (c) is a metallographic photograph of dendritic crystal distribution in comparative example 3, and (d) is a metallographic photograph of dendritic crystal distribution in an industrial heat treatment example.
FIG. 2 shows the results of room temperature tensile strength of the as-cast, one-stage homogenization heat treatment, and industrial heat treatment examples, examples 1 to 3, and comparative examples 1 to 3.
Detailed Description
The following describes embodiments 1 to 3 of the present invention in detail with reference to the drawings, and the present invention is further described, but not limited thereto. Meanwhile, in order to verify the positive effect of the pulse current, equivalent heat treatment is carried out in a muffle furnace, which is specifically shown in comparative examples 1-3.
The following describes that the high temperature alloy materials used in examples 1 to 3, comparative examples 1 to 3, and industrial heat treatment examples are obtained by heat-treating a low melting point brittle phase (collectively referred to as a one-stage homogenization heat treatment state), in which a non-negligible dendritic structure still exists, as shown in fig. 1 (a). The industrial heat treatment example is to keep the temperature of the high-temperature alloy in the one-stage homogenization heat treatment state in a muffle furnace under the high-temperature condition to eliminate the dendritic structure.
The pulse parameters described in examples 1-3 below are for analysis of dendrite elimination with a size of 30 × 4 × 1.5mm3The rectangular deformation zone of the high-temperature alloy in the pulse current external field treatment state for the room-temperature tensile strength test is 20 × 4 × 1.5.5 mm3The same pulse external field treatment effect as that used for the tissue analysis sample can be achieved only by correspondingly adjusting two parameters of voltage and current to ensure constant current density.
Example 1
In this embodiment, the pulse parameters are set to 30000Hz, 1.2V and 14.721A/mm2. The temperature measured by a type K thermocouple at this parameter was 850 ℃. The pulse was continued for 30min and then air cooled to room temperature. The method comprises the following specific steps:
(1) taking a rectangular deformation zone 20 × 4 × 1.5.5 mm3The surface of the material in the heat treatment state is ground by 180-mesh, 600-mesh, 1000-mesh, 1500-mesh and 2000-mesh abrasive paper in sequence until no visible defects exist, so that good contact with the pulse electrode is ensured.
(2) And (5) carrying out pulsed current external field treatment. And (3) fixing the high-temperature alloy polished in the step (1) at two ends of a pulse power supply by using copper clamps. The pulse treatment is continued for 30min at room temperature, and the surface temperature of the high-temperature alloy after the pulse current external field is applied is measured by a K-type thermocouple to be 850 ℃.
(3) The treated tensile specimens were tested for room temperature tensile strength at room temperature (23 ℃).
Comparative example 1
The comparative example heat treatment process was carried out in a muffle furnace. Heating to 850 deg.C at a rate of 5 deg.C/min, maintaining for 30min, and air cooling to room temperature. The treated tensile specimens were tested for room temperature tensile strength at room temperature (23 ℃).
Example 2
In this embodiment, the pulse parameters are set to 30000Hz, 1.45V and 17.570A/mm2. Under the parameter, the temperature is measured by a K-type thermocouple, and the temperature is 950 ℃. The pulse was continued for 30min and then air cooled to room temperature.
(1) Taking a rectangular deformation zone 20 × 4 × 1.5.5 mm3The surface of the material is 180 meshes and 600 meshesAnd sequentially polishing 1000-mesh, 1500-mesh and 2000-mesh sandpaper until no visible defects exist so as to ensure good contact with the pulse electrode.
(2) And (5) carrying out pulsed current external field treatment. And (3) fixing the high-temperature alloy polished in the step (1) at two ends of a pulse power supply by using copper clamps. The pulse treatment was continued for 30min at room temperature while the surface temperature of the superalloy after application of the pulsed current external field was measured by a K-type thermocouple to be 950 ℃.
(3) The treated tensile specimens were tested for room temperature tensile strength at room temperature (23 ℃).
Comparative example 2
The comparative example heat treatment process was carried out in a muffle furnace. Heating to 950 deg.C at a rate of 5 deg.C/min, maintaining for 30min, and air cooling to room temperature. The treated tensile specimens were tested for room temperature tensile strength at room temperature (23 ℃).
Example 3
In this embodiment, the pulse parameters are set to 30000Hz, 1.6V and 19.676A/mm2. Under the parameter, the temperature is measured by a K-type thermocouple and is 1050 ℃. The pulse was continued for 30min and then air cooled to room temperature. The method comprises the following specific steps:
(1) taking 30 × 4 × 1.5.5 mm3With rectangular deformation zone 20 × 4 × 1.5.5 mm3The surface of the material is sequentially polished by 180-mesh, 600-mesh, 1000-mesh, 1500-mesh and 2000-mesh abrasive paper until no visible defects exist, and good contact with the pulse electrode is ensured.
(2) And (5) carrying out pulsed current external field treatment. And (3) fixing the high-temperature alloy polished in the step (1) at two ends of a pulse power supply by using copper clamps. The pulse treatment is continued for 30min at room temperature, and the surface temperature of the high-temperature alloy after the pulse current external field is applied is measured by a K-type thermocouple to be 1050 ℃.
(3) The treated tensile specimens were tested for room temperature tensile strength at room temperature (23 ℃).
(4) The dendrite distribution was observed by means of an OLYMPUS GX71 metallographic optical microscope. Respectively taking a stage of high-temperature alloy in a homogenized heat treatment state and a pulse current external field treatment state, and sequentially polishing the surface by 180-mesh, 600-mesh, 1000-mesh, 1500-mesh and 2000-mesh abrasive paper until the scratch direction is consistent. And (3) carrying out electrolytic corrosion after mechanical polishing: the corrosive liquid is 16g of CrO3+10mLH2SO4+170mL H3PO4(ii) a The direct current voltage is 5V, and the electrolytic corrosion time is 5-7 seconds. And observing the homogenization heat treatment state in one stage and the distribution of dendrites in the high-temperature alloy in the embodiment through a metallographic microscope. The metallurgical results are shown in (a) and (b) of the attached figure 1.
Comparative example 3
The comparative example heat treatment process was carried out in a muffle furnace. Heating to 1050 deg.C at a rate of 5 deg.C/min, and holding for 30 min. For the elimination of dendrite segregation, the observation was performed by a metallographic optical microscope, and the sample preparation method was as shown in example 3. The metallographic results are shown in FIG. 1 (c). The treated tensile specimens were tested for room temperature tensile strength at room temperature (23 ℃).
Example of Industrial Heat treatment
The whole heat treatment process is completed in a muffle furnace, the temperature is raised to 1190 ℃, heat preservation is continued for 72 hours, and then air cooling is carried out to the room temperature. For the elimination of dendrite segregation, the observation was performed by a metallographic optical microscope, and the sample preparation method was as shown in example 3. The metallographic results are shown in FIG. 1 (d). The treated tensile specimens were tested for room temperature tensile strength at room temperature (23 ℃).
The elimination of dendrites in the one-stage homogenized heat-treated superalloy, example 3, comparative example 3, and industrial heat treatment example was observed by a metallographic optical microscope, and the results are shown in fig. 1. FIG. 1 shows that: the pulse current external field greatly accelerates the diffusion rate of the segregation element atoms and breaks the thermal diffusion limit of the atoms. At appropriate pulse parameters (30000Hz, 1.6V, 19.676A/mm)2) And the effect of industrial long-time high-temperature heat treatment can be achieved only by treating for 30 min.
The samples in the as-cast state, the one-stage homogenization heat treatment state, the industrial heat treatment examples, examples 1 to 3 and comparative examples 1 to 3 were subjected to room temperature stretching, and the results of the high-temperature alloy yield strength test in each state were obtained, as shown in fig. 2. The results show that: compared with the traditional heat treatment, the method has the advantages that the pulse parameters are proper (30000Hz, 1.6V, 19.676A/mm)2) The lower treatment is carried out for 30min, the yield strength of the high-temperature alloy reaches 283MPa, the strength is goodIs significantly lower than 386MPa after industrial heat treatment. Cogging forging after homogenization to avoid cracking, a lower strength of the superalloy is desired. Therefore, the method is beneficial to the subsequent cogging and forging processes while realizing elimination of dendrite segregation.
The above description is only an embodiment of the present invention for eliminating dendrite segregation in a ni-based wrought superalloy ingot, and the above examples are only exemplary and should not be taken as limiting the scope of the present invention. The invention is not limited to the above embodiments, and any person skilled in the art can substitute similar materials, devices or adjust related technical parameters within the technical scope of the invention.
Claims (9)
1. A method for rapidly eliminating dendrite segregation in a deformed high-temperature alloy ingot by pulse current is characterized in that the method carries out pulse current treatment on a nickel-based deformed high-temperature alloy ingot which is only subjected to the traditional one-stage homogenization heat treatment, and the method greatly shortens the time required for eliminating the dendrite segregation in the ingot; the pulse processing parameters are as follows: the frequency is 30000Hz, the voltage is 0.1V-100V, and the current density is 1A/mm2～150A/mm2The treatment time is 5min to 20 h; the conventional uniform stage is to eliminate the low melting point phase, but a severe element segregation stage still exists.
2. The method for rapidly eliminating dendritic segregation in a deformed high-temperature alloy ingot by using pulse current as claimed in claim 1, which is characterized by comprising the following specific steps of:
(1) the nickel-based deformed superalloy material is fixed by a pure copper clamp and then connected to two ends of a pulse power supply through a pure copper wire;
(2) after setting parameters, switching on a pulse power supply, and enabling the temperature of the central area of the high-temperature alloy to reach the expected treatment temperature within 10 s; continuously applying pulses for 5 min-20 h, and air-cooling to room temperature after the power supply is cut off.
3. The method for rapidly eliminating dendritic segregation in a wrought superalloy ingot by pulse current according to claim 2, wherein the nickel-based wrought superalloy is an GH4169D alloy ingot and is obtained by a triple smelting process: vacuum induction melting, electroslag remelting and vacuum consumable remelting, and a first stage of homogenization heat treatment is carried out to re-dissolve the low-melting brittle phase.
4. The method for rapidly eliminating dendrite segregation in a deformed high-temperature alloy ingot by using pulse current according to claim 2, wherein the pulse current output equipment is a high-frequency pulse power supply, and different treatment effects can be obtained by adjusting voltage and current.
5. The method for rapidly eliminating dendrite segregation in a deformed superalloy ingot by pulsed current according to claim 2, wherein the pulsed current external field treatment is performed at room temperature.
6. The method of claim 2 wherein the temperature rise due to joule heating generated when the pulse current is applied is considered uniform across the superalloy material.
7. The method of claim 2, wherein the rapid elimination of dendrite segregation is facilitated by the coupling of pulse current and joule heating after the pulse current is applied; compared with a pure thermal field, the pulse current has a remarkable advantage in eliminating dendritic segregation in the alloy ingot.
8. The method for rapidly eliminating dendrite segregation in a deformed superalloy ingot by using pulsed current according to claim 2, wherein the pulsed current external field treatment is used for analyzing dendrite segregation elimination situationThe size of the alloy is 30 × 4 × 1.5.5 mm3The rectangular deformation zone of the high-temperature alloy in the pulse current external field treatment state for testing the tensile strength at room temperature is 20 × 4 × 1.5.5 mm3。
9. The method of claim 2, wherein the temperature of the clamping end portions on both sides of the superalloy is lower than the processing temperature due to the rapid heat dissipation of copper, so that the elimination of dendrite segregation in the central region of the superalloy in the pulsed current external field processing state is mainly concerned in the subsequent structure observation process.
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| CN114058992A (en) * | 2021-11-22 | 2022-02-18 | 北京航空航天大学 | Method for prolonging service time of single crystal high-temperature alloy blade material for aircraft engine |
| CN114058992B (en) * | 2021-11-22 | 2022-06-14 | 北京航空航天大学 | Method for prolonging service time of single crystal high-temperature alloy blade material for aircraft engine |
| CN115740491A (en) * | 2022-11-03 | 2023-03-07 | 燕山大学 | Method for preparing 3D printing heterogeneous material with excellent interface performance based on pulse current |
| CN116145061A (en) * | 2022-12-26 | 2023-05-23 | 大连理工大学 | Multi-field coupling heat treatment process for manufacturing GH4099 large-sized structural member by additive material |
| CN116145061B (en) * | 2022-12-26 | 2024-04-02 | 大连理工大学 | Multi-field coupling heat treatment process for manufacturing GH4099 large-sized structural member by additive material |
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