CN116814968A - Method for preparing high-purity ordered gradient superalloy by electron beam refining casting technology - Google Patents
Method for preparing high-purity ordered gradient superalloy by electron beam refining casting technology Download PDFInfo
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- 238000010894 electron beam technology Methods 0.000 title claims abstract description 93
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 84
- 238000007670 refining Methods 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000005266 casting Methods 0.000 title claims abstract description 38
- 238000005516 engineering process Methods 0.000 title claims abstract description 22
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000000956 alloy Substances 0.000 claims abstract description 42
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 41
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000000746 purification Methods 0.000 claims abstract description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 41
- 229910052802 copper Inorganic materials 0.000 claims description 41
- 239000010949 copper Substances 0.000 claims description 41
- 238000003723 Smelting Methods 0.000 claims description 37
- 239000012535 impurity Substances 0.000 claims description 35
- 238000002844 melting Methods 0.000 claims description 22
- 230000008018 melting Effects 0.000 claims description 22
- 238000004140 cleaning Methods 0.000 claims description 16
- 239000000155 melt Substances 0.000 claims description 14
- 238000007711 solidification Methods 0.000 claims description 14
- 230000008023 solidification Effects 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- 239000002893 slag Substances 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000005498 polishing Methods 0.000 claims description 8
- 239000000498 cooling water Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229920000742 Cotton Polymers 0.000 claims description 6
- 239000000428 dust Substances 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000011109 contamination Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 9
- 238000005204 segregation Methods 0.000 abstract description 6
- 238000007781 pre-processing Methods 0.000 abstract 1
- 230000006698 induction Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000013014 purified material Substances 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/22—Remelting metals with heating by wave energy or particle radiation
- C22B9/228—Remelting metals with heating by wave energy or particle radiation by particle radiation, e.g. electron beams
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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Abstract
The invention provides a method for preparing high-purity ordered gradient superalloy by an electron beam refining casting technology, which comprises the following steps: s1, preprocessing raw materials; s2, refining by electron beam high purification; s3, alloy casting. The invention realizes the preparation of the high-purity ordered gradient structure of the nickel-cobalt-based superalloy, and the prepared high-purity easily-deformable cast ingot has few inclusions, low segregation degree and ordered structure, and can further improve the performance of the superalloy.
Description
Technical Field
The invention relates to a method for preparing high-purity ordered gradient superalloy by an electron beam refining casting technology.
Background
The high-temperature alloy is very important in materials for the turbine disk of the industrial gas turbine, the working environment is in high temperature, stress and corrosion environment, coarsening of the structure and precipitation of harmful phases are easy to occur, cracking is easy to occur in an inclusion or defect enrichment area, and the corresponding interface is easy to become a channel for crack propagation.
The traditional preparation methods of the current deformed nickel-cobalt-based superalloy comprise a high-vacuum induction smelting method, a vacuum consumable smelting method and the like. In the methods, the alloy is smelted integrally according to the components, and inclusions or impurity elements can not be decomposed or removed in a targeted manner in the smelting process, and the segregation degree is high. Difficult to deform and easy to crack.
The electron beam refining casting and induced solidification technology is to bombard the surface of material with high energy electron beam, and is one smelting mode for smelting refractory metal and its alloy, titanium and titanium alloy and smelting purified material. In the invention, during electron beam refining, parameters such as the size of electron beam current, the size of electron beam spot, an electron beam scanning mode and the like are adjusted to ensure that the surface of the high-temperature alloy melt is kept at a higher smelting temperature, and impurities in the high-temperature alloy are decomposed under a high-vacuum and high-superheat environment, so that impurity elements can be effectively removed. And after refining, removing surface impurities through slag absorption, and then pouring the refined high-temperature alloy melt into a water-cooled copper crucible stably. And controlling the gradient and the rate of the solidification front of the ingot by using an electron beam, and obtaining the nickel-cobalt-based superalloy ingot with a gradient ordered structure after the nickel-cobalt-based superalloy in the water-cooled copper crucible is completely solidified.
Disclosure of Invention
The traditional preparation methods of the deformed nickel-cobalt-based superalloy provided by the above include a high-vacuum induction smelting method, a vacuum consumable smelting method and the like, wherein the methods are to carry out integral smelting on the alloy according to components, inclusions or impurity elements can not be decomposed or removed in a targeted manner in the smelting process, and the segregation degree is high; the technical problems of difficult deformation and easy cracking are solved, and the method for preparing the high-purity ordered gradient superalloy by using the electron beam refining casting technology is provided. The invention provides a method for preparing high-purity ordered gradient superalloy by combining electron beam high-purification refining and induced solidification, which comprises the steps of inducing inclusion to be enriched at the edge of the alloy at the end of electron beam refining and carrying out slag absorption treatment, melting and pouring pure melt without inclusion into a water-cooled copper crucible, and achieving the purpose of preparing high-purity deformable nickel-cobalt-based superalloy by electron beam induced solidification.
The invention adopts the following technical means:
a method for preparing high-purity ordered gradient superalloy by electron beam refining casting technology comprises the following steps:
s1, pretreatment of raw materials:
s11, using a rod-shaped nickel-cobalt-based superalloy as a raw material;
s12, cutting, polishing, cleaning and drying the nickel-cobalt-based superalloy bar for later use;
s2, high purification and refining by electron beams:
s21, cleaning the inside of a furnace body of the electron beam smelting furnace, and polishing and cleaning two water-cooled copper crucibles;
s22, placing the pretreated nickel-cobalt-based superalloy raw material in the middle of a No. 1 water-cooled copper crucible, treating and cleaning the periphery of the crucible by using cotton cloth stained with alcohol, and closing a furnace door after confirming that the smelting environment is pollution-free;
s23, turning on a power switch of the cooling water, the air compressor and the electron beam melting equipment, and vacuumizing a melting chamber and an electron gun chamber to reach a target vacuum degree;
s24, after the vacuum degree of the smelting chamber and the electron gun chamber meets the requirement, starting a No. 1 electron gun to melt the nickel-cobalt-based superalloy;
s25, after the nickel-cobalt-based superalloy is completely melted, carrying out electron beam high-purification refining treatment;
s26, refining and purifying for 10min, removing impurities on the surface of the melt by utilizing an electron beam, and obtaining a high-purity melt to be poured after refining;
s3, alloy casting:
s31, after all inclusions on the alloy surface in the step S26 are removed, starting a crucible dumping device, pouring high-purity melt in a No. 1 water-cooled crucible into a No. 2 water-cooled copper crucible, and starting a No. 2 electron gun to apply electron beams to the melt in the No. 2 water-cooled copper crucible to obtain an ingot casting structure;
s32, after pouring, recovering the No. 1 water-cooled crucible to the original position; closing the high voltage of the two electron guns, reducing the beam current to 0mA, and closing the two electron guns;
s33, after the electron beam melting furnace is cooled for 60min, argon is introduced twice to continuously cool the furnace body, and after the furnace body is completely cooled, the high-purity ordered gradient superalloy cast ingot is taken out.
Further, in the step S11, the diameter of the rod-shaped nickel-cobalt-based superalloy is 20-50mm;
the specific steps of the step S12 are as follows:
s121, cutting the nickel-cobalt-based superalloy bar into small cylinders with phi of 100mm multiplied by 8mm, and polishing the surfaces of the small cylinders by a grinder to remove stains and oxide skin on the surfaces;
s122, cleaning the polished nickel-cobalt-based superalloy with deionized water and alcohol respectively, cleaning the polished nickel-cobalt-based superalloy with an ultrasonic cleaner, drying the cleaned nickel-cobalt-based superalloy with a blower, and smelting the nickel-cobalt-based superalloy with an electron beam.
Further, in step S21, the surfaces of the two water-cooled copper crucibles are polished to be smooth by using 2000# sand paper, the polished dust is removed by using a powerful dust collector, the polished surface is cleaned by using alcohol, and the polished surface is wiped clean by using cotton cloth, so that the two water-cooled copper crucibles are free from impurity pollution.
Further, in the step S23, the target vacuum degree is: the vacuum degree of the smelting chamber is required to be less than 5 multiplied by 10 -2 Pa～8×10 -2 Pa, vacuum degree of electron gun chamber is less than 8×10 -3 Pa～9×10 -3 Pa。
Further, the specific steps of the step S24 are as follows:
after the vacuum degree of the smelting chamber and the electron gun chamber reaches the requirement, starting the high voltage of the 1# electron gun, slowly increasing the beam current to 200mA after the voltage reaches 20kV and is stable for 1min, and focusing 118mA downwards; the smelting power is kept unchanged, and the nickel-cobalt-based superalloy raw material is gradually melted in a spiral line scanning mode.
Further, the specific steps of the step S25 are as follows:
after the nickel-cobalt-based superalloy is completely melted and filled in the crucible, slowly increasing the beam current to 600mA, and after the beam current is stable, carrying out electron beam high-purification refining treatment on the melted alloy.
Further, in the step S26, after refining and purifying for 10min, the impurities are driven to concentrate toward the crucible edge by adopting an electron beam spiral scanning mode and are collected to a slag taking area, and the impurities on the surface of the melt are removed by a slag sucking system.
Further, the specific steps of the step S31 are as follows:
after all impurities on the alloy surface are removed in the step S26, starting a crucible dumping device, pouring the high-purity melt in the No. 1 water-cooling crucible into the No. 2 water-cooling copper crucible at the speed of 150g/min, starting a No. 2 electron gun, performing induced solidification on the melt in the No. 2 water-cooling copper crucible, adjusting the beam current of the No. 2 electron gun, and reducing the beam current from 600mA to 0mA within 5min to obtain an ingot casting structure with a columnar crystal-equiaxed crystal-columnar crystal multi-size structure.
Further, during the casting process, the electron beam uniformly scanned the melt surface in the # 1 water-cooled crucible.
Further, in the step S32, after the pouring is completed, the solidified alloy containing a large amount of impurities in the deep arc-receiving area is still left in the 1# water-cooled copper crucible, so that the high-purity melt and the impurities are effectively separated.
Compared with the prior art, the invention has the following advantages:
1. the method for preparing the high-purity ordered gradient superalloy by using the electron beam refining casting technology provided by the invention prepares the high-purity ordered gradient superalloy by combining electron beam high-purity refining with induced solidification, induces impurities to be enriched at the edge of the alloy at the end of electron beam refining and carries out slag suction treatment, melts and casts pure melt without impurities into a water-cooled copper crucible, and achieves the aim of preparing the high-purity easily-deformable nickel-cobalt-based superalloy by using electron beam induced solidification.
2. According to the method for preparing the high-purity ordered gradient superalloy by the electron beam refining casting technology, in the electron beam refining process, parameters such as the size of electron beam current, the size of electron beam spots, an electron beam scanning mode and the like are adjusted to enable the surface of a superalloy melt to be kept at a higher smelting temperature, and impurities in the superalloy are decomposed under a high-vacuum and high-superheat environment, so that impurity elements can be effectively removed. And after refining, removing surface impurities through slag absorption, and then pouring the refined high-temperature alloy melt into a water-cooled copper crucible stably. And controlling the gradient and the rate of the solidification front of the ingot by using an electron beam, and obtaining the nickel-cobalt-based superalloy ingot with a gradient ordered structure after the nickel-cobalt-based superalloy in the water-cooled copper crucible is completely solidified.
3. The method for preparing the high-purity ordered gradient superalloy by the electron beam refining casting technology combines with casting on the basis of electron beam refining of the nickel-cobalt-based superalloy, realizes effective separation of the superalloy and impurities, shortens the production period of a high-purity easily-deformable ingot, and further improves the purity and the hot working window of the ingot. The preparation yield of the alloy is improved to more than 85% from the traditional 60%.
4. The method for preparing the high-purity ordered gradient superalloy by the electron beam refining casting technology provided by the invention realizes the preparation of the high-purity ordered gradient structure of the nickel-cobalt-based superalloy, and the prepared high-purity easily-deformable ingot has few inclusions, low segregation degree and ordered structure, and can further improve the performance of the superalloy.
In summary, the technical scheme of the invention can solve the problems that the traditional preparation methods of the deformed nickel-cobalt-based superalloy comprise a high-vacuum induction smelting method, a vacuum consumable smelting method and the like, and the methods are all to carry out integral smelting on the alloy according to the components, so that inclusions or impurity elements can not be decomposed or removed in a targeted manner in the smelting process, and the segregation degree is higher; difficult deformation and easy cracking.
For the reasons, the invention can be widely popularized in the fields of high-temperature alloy preparation and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to the drawings without inventive effort to a person skilled in the art.
FIG. 1 is a schematic diagram of an electron beam induction melting casting apparatus of the present invention.
FIG. 2 is a flow chart of electron beam melting process of the present invention.
FIG. 3 is a graph showing the grain growth of various cooling modes according to the present invention.
In the figure: 1. an electron gun; 2. a mechanical pump; 3. a flapper valve; 4. a diffusion pump; 5. an electron beam; 6. smelting a crucible; 7. a diffusion pump; 8. solidifying the crucible; 9. a cooling water pipe; 10. a cooling water inlet; 11. refining the molten pool.
Detailed Description
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other. The invention will be described in detail below with reference to the drawings in connection with embodiments.
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present invention. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
The relative arrangement of the components and steps, numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless it is specifically stated otherwise. Meanwhile, it should be clear that the dimensions of the respective parts shown in the drawings are not drawn in actual scale for convenience of description. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further discussion thereof is necessary in subsequent figures.
Based on the great advantage of electron beam refining technology in preparing high purity multielement alloy and the characteristic of electron beam layer condensation of its surface heat source, high purity ordered gradient high temperature alloy material may be produced. The invention provides a method for preparing a high-purity ordered gradient superalloy by an electron beam refining casting technology, which realizes the preparation of a high-purity ordered gradient structure of a nickel-cobalt-based superalloy, and the prepared high-purity easily-deformable ingot has few inclusions, low segregation degree and ordered structure, and can further improve the performance of the superalloy.
The electron beam refining casting and induced solidification technology is to bombard the surface of material with high energy electron beam, and is one smelting mode for smelting refractory metal and its alloy, titanium and titanium alloy and smelting purified material. In the invention, during electron beam refining, parameters such as the size of electron beam current, the size of electron beam spot, an electron beam scanning mode and the like are adjusted to ensure that the surface of the high-temperature alloy melt is kept at a higher smelting temperature, and impurities in the high-temperature alloy are decomposed under a high-vacuum and high-superheat environment, so that impurity elements can be effectively removed. And after refining, removing surface impurities through slag absorption, and then pouring the refined high-temperature alloy melt into a water-cooled copper crucible stably. And controlling the gradient and the rate of the solidification front of the ingot by using an electron beam, and obtaining the nickel-cobalt-based superalloy ingot with a gradient ordered structure after the nickel-cobalt-based superalloy in the water-cooled copper crucible is completely solidified.
The invention provides a method for preparing high-purity ordered gradient superalloy by combining electron beam high-purification refining and induced solidification. Inducing inclusion to be concentrated at the edge of the alloy and sucking slag at the end of electron beam refining, melting and pouring the pure melt without inclusion into a water-cooled copper crucible, and performing electron beam induced solidification to obtain the high-purity easy-deformation nickel-cobalt-based superalloy.
The method comprises the following steps:
1. pretreatment of raw materials
1. The raw material is a bar-shaped nickel-cobalt-based superalloy with the diameter of 20-50mm.
2. Cutting the nickel-cobalt-based superalloy bar into small cylinders with phi of 100mm multiplied by 8mm, polishing the surfaces of the small cylinders by a grinder, and removing stains and oxide scales on the surfaces.
3. And cleaning the polished alloy with deionized water and alcohol respectively, cleaning the alloy by using an ultrasonic cleaner, and drying the alloy by using a blower for electron beam melting.
2. High purification refining of electron beam
1. Cleaning the inside of an electron beam melting furnace body, polishing the surfaces of two water-cooled copper crucibles (a No. 1 water-cooled copper crucible and a No. 2 water-cooled copper crucible) to be smooth by using No. 2000 sand paper, removing polished dust by using a powerful dust collector, cleaning a polished surface by using alcohol (anhydrous), and wiping the polished surface by using cotton cloth. The No. 1 water-cooled copper crucible (melting crucible) and the No. 2 water-cooled copper crucible (solidifying crucible) are free from impurity contamination.
2. The polished and finely washed nickel-cobalt-based superalloy raw material (pretreated alloy) is placed in the middle of a No. 1 water-cooled copper crucible, the periphery of the crucible is treated and cleaned by cotton cloth stained with alcohol, and the furnace door is closed after no pollution of the smelting environment is confirmed.
3. The power switch of the cooling water, the air compressor and the electron beam melting equipment is turned on, the melting chamber and the electron gun chamber are vacuumized, and the vacuum degree of the melting chamber is required to be less than 5 multiplied by 10 -2 Pa～8×10 -2 Pa, vacuum degree of electron gun chamber is less than 8×10 -3 Pa～9×10 -3 Pa。
4. After the vacuum degree of the melting chamber and the electron gun chamber reaches the requirement, starting the high voltage of the 1# electron gun (i.e. the electron gun at the left side in fig. 1), slowly increasing the beam current to 200mA after the voltage reaches 20kV and is stable for 1min, and focusing the beam current downwards to 118mA. The smelting power is kept unchanged, and the nickel-cobalt-based superalloy raw material is gradually melted in a spiral line scanning mode. After the nickel-cobalt-based superalloy is completely melted and filled in the crucible, slowly increasing the beam current to 600mA, and after the beam current is stable, carrying out electron beam high-purification refining treatment on the melted alloy.
5. After refining and purifying for 10min, driving the impurities to concentrate towards the edge of the crucible in an electron beam spiral line scanning mode, collecting the impurities to a slag taking area, removing impurities on the surface of the melt through a slag sucking system, and pouring (after refining is finished, obtaining the high-purity melt to be poured).
3. Alloy casting
1. After the impurities on the surface of the alloy are completely removed, starting a crucible dumping device, and uniformly scanning an electron beam on the surface of a melt of the No. 1 water-cooled crucible.
2. And (3) pouring the high-purity melt in the No. 1 water-cooled crucible into the No. 2 water-cooled copper crucible at the speed of 150g/min, starting a No. 2 electron gun (namely an electron gun on the right side in the figure 1), performing induced solidification on the melt in the No. 2 water-cooled copper crucible, adjusting the beam current of the No. 2 electron gun, and reducing the beam current from 600mA to 0mA within 5min to achieve the aim that the ingot casting structure is a columnar crystal-equiaxed crystal-columnar crystal multi-size structure. The cooling mode is to alternately reduce the beam current to control the temperature gradient of the solid-liquid section. So that the alloy is converted from columnar crystal orientation to equiaxial crystal. Fig. 2 is a process diagram of uniform reduced beam cooling and alternating reduced beam cooling. Experiments and calculations show that (fig. 3, a crystal grain growth diagram of different electron beam cooling modes), the alternate cooling can keep the crystal grain growth mode (from bottom to top) in a mixed crystal area, so that a solid-liquid interface is transformed from columnar crystal to equiaxed crystal.
3. And after pouring, the No. 1 water-cooled crucible is restored to the original position, and the solidified alloy containing a large amount of impurities in the deep arc-collecting region is still remained in the No. 1 water-cooled copper crucible, so that the high-purity melt and the impurities are effectively separated. The high voltage of the two electron guns is turned off, and the two electron guns are turned off after the beam current is reduced to 0 mA.
4. And after the electron beam melting furnace is cooled for 60min, argon is introduced into the furnace body for continuously cooling the furnace body twice, and the furnace body is completely cooled and then the high-purity ordered gradient superalloy cast ingot is taken out.
FIG. 1 is a schematic diagram of an electron beam induction melting casting apparatus according to the present invention, which is used to prepare high purity ordered gradient superalloys using the apparatus shown in FIG. 1. Two electron guns 1 are respectively fixed at two side angles at the top of the electron beam melting furnace, a No. 1 water-cooled copper crucible (melting crucible 6) and a No. 2 water-cooled copper crucible (solidifying crucible 8) are placed at the bottom of the electron beam melting furnace through crucible supports, cooling water pipelines 9 are connected with the two electron guns, and cooling water inlets 10 are formed in the side edges of the electron beam melting furnace. The nickel-cobalt-based superalloy is placed in a No. 1 water-cooled copper crucible 6 and is smelted and refined in the scanning range of an electron beam 5, and a refined molten pool 11 is formed by the refined nickel-cobalt-based superalloy. The refined high-purity melt in the No. 1 water-cooled copper crucible 6 is poured into the No. 2 water-cooled copper crucible 8 through a crucible pouring device. The diffusion pump 4 is adjacent to the mechanical pump 2, and the communication relationship between the two is controlled by the baffle valve 3; the diffusion pump 7 is adjacent to the mechanical pump 2, and the two are connected together.
The method is combined with casting on the basis of refining the nickel-cobalt-based superalloy by using an electron beam, so that the high-temperature alloy and impurities are effectively separated, the production period of a high-purity easily-deformable cast ingot is shortened, and the purity of the cast ingot and a hot working window are further improved. The preparation yield of the alloy is improved to more than 85% from the traditional 60%.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. The method for preparing the high-purity ordered gradient superalloy by using the electron beam refining casting technology is characterized by comprising the following steps of:
s1, pretreatment of raw materials:
s11, using a rod-shaped nickel-cobalt-based superalloy as a raw material;
s12, cutting, polishing, cleaning and drying the nickel-cobalt-based superalloy bar for later use;
s2, high purification and refining by electron beams:
s21, cleaning the inside of a furnace body of the electron beam smelting furnace, and polishing and cleaning two water-cooled copper crucibles;
s22, placing the pretreated nickel-cobalt-based superalloy raw material in the middle of a No. 1 water-cooled copper crucible, treating and cleaning the periphery of the crucible by using cotton cloth stained with alcohol, and closing a furnace door after confirming that the smelting environment is pollution-free;
s23, turning on a power switch of the cooling water, the air compressor and the electron beam melting equipment, and vacuumizing a melting chamber and an electron gun chamber to reach a target vacuum degree;
s24, after the vacuum degree of the smelting chamber and the electron gun chamber meets the requirement, starting a No. 1 electron gun to melt the nickel-cobalt-based superalloy;
s25, after the nickel-cobalt-based superalloy is completely melted, carrying out electron beam high-purification refining treatment;
s26, refining and purifying for 10min, removing impurities on the surface of the melt by utilizing an electron beam, and obtaining a high-purity melt to be poured after refining;
s3, alloy casting:
s31, after all inclusions on the alloy surface in the step S26 are removed, starting a crucible dumping device, pouring high-purity melt in a No. 1 water-cooled crucible into a No. 2 water-cooled copper crucible, and starting a No. 2 electron gun to apply electron beams to the melt in the No. 2 water-cooled copper crucible to obtain an ingot casting structure;
s32, after pouring, recovering the No. 1 water-cooled crucible to the original position; closing the high voltage of the two electron guns, reducing the beam current to 0mA, and closing the two electron guns;
s33, after the electron beam melting furnace is cooled for 60min, argon is introduced twice to continuously cool the furnace body, and after the furnace body is completely cooled, the high-purity ordered gradient superalloy cast ingot is taken out.
2. The method for preparing high-purity ordered gradient superalloy by electron beam refining casting technology according to claim 1, wherein in step S11, the diameter of the rod-shaped nickel-cobalt-based superalloy is 20-50mm;
the specific steps of the step S12 are as follows:
s121, cutting the nickel-cobalt-based superalloy bar into small cylinders with phi of 100mm multiplied by 8mm, and polishing the surfaces of the small cylinders by a grinder to remove stains and oxide skin on the surfaces;
s122, cleaning the polished nickel-cobalt-based superalloy with deionized water and alcohol respectively, cleaning the polished nickel-cobalt-based superalloy with an ultrasonic cleaner, drying the cleaned nickel-cobalt-based superalloy with a blower, and smelting the nickel-cobalt-based superalloy with an electron beam.
3. The method for preparing the high-purity ordered gradient superalloy by using the electron beam refining casting technology according to claim 1, wherein in the step S21, the surfaces of the two water-cooled copper crucibles are polished smooth by using No. 2000 sand paper, the polished dust is removed by using a powerful dust collector, the polished surface is cleaned by using alcohol, and the polished surface is wiped clean by using cotton cloth, so that the two water-cooled copper crucibles are free from impurity contamination.
4. The method for preparing high-purity ordered gradient superalloy by electron beam refining casting according to claim 1, wherein in step S23, the target vacuum is: the vacuum degree of the smelting chamber is required to be less than 5 multiplied by 10 -2 Pa～8×10 - 2 Pa, vacuum degree of electron gun chamber is less than 8×10 -3 Pa～9×10 -3 Pa。
5. The method for preparing high-purity ordered gradient superalloy by electron beam refining casting technology according to claim 1, wherein the specific steps of step S24 are as follows:
after the vacuum degree of the smelting chamber and the electron gun chamber reaches the requirement, starting the high voltage of the 1# electron gun, slowly increasing the beam current to 200mA after the voltage reaches 20kV and is stable for 1min, and focusing 118mA downwards; the smelting power is kept unchanged, and the nickel-cobalt-based superalloy raw material is gradually melted in a spiral line scanning mode.
6. The method for preparing the high-purity ordered gradient superalloy by using the electron beam refining casting technology according to claim 1, wherein the specific steps of step S25 are as follows:
after the nickel-cobalt-based superalloy is completely melted and filled in the crucible, slowly increasing the beam current to 600mA, and after the beam current is stable, carrying out electron beam high-purification refining treatment on the melted alloy.
7. The method for preparing high-purity ordered gradient superalloy by electron beam refining casting technology according to claim 1, wherein in step S26, after refining and purifying for 10min, the inclusions are driven to concentrate toward the crucible edge by electron beam helical line scanning, and collected into a slag extraction area, and the inclusions on the surface of the melt are removed by a slag absorption system.
8. The method for preparing the high-purity ordered gradient superalloy by using the electron beam refining casting technology according to claim 1, wherein the specific steps of the step S31 are as follows:
after all impurities on the alloy surface are removed in the step S26, starting a crucible dumping device, pouring the high-purity melt in the No. 1 water-cooling crucible into the No. 2 water-cooling copper crucible at the speed of 150g/min, starting a No. 2 electron gun, performing induced solidification on the melt in the No. 2 water-cooling copper crucible, adjusting the beam current of the No. 2 electron gun, and reducing the beam current from 600mA to 0mA within 5min to obtain an ingot casting structure with a columnar crystal-equiaxed crystal-columnar crystal multi-size structure.
9. The method for preparing high purity ordered gradient superalloy by electron beam refining casting technology according to claim 1 or 8, wherein the electron beam uniformly scans the melt surface in a # 1 water cooled crucible during casting.
10. The method for preparing high-purity ordered gradient superalloy by electron beam refining casting according to claim 1, wherein in step S32, the solidified alloy containing a large amount of impurities in the deep arc zone remains in the 1# water cooled copper crucible after pouring, thereby realizing effective separation of high-purity melt and impurities.
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