CN112746177B - Method for refining and purifying high-temperature alloy return material by using electron beams - Google Patents

Method for refining and purifying high-temperature alloy return material by using electron beams Download PDF

Info

Publication number
CN112746177B
CN112746177B CN202011582014.0A CN202011582014A CN112746177B CN 112746177 B CN112746177 B CN 112746177B CN 202011582014 A CN202011582014 A CN 202011582014A CN 112746177 B CN112746177 B CN 112746177B
Authority
CN
China
Prior art keywords
refining
electron beam
alloy
melt
electron
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202011582014.0A
Other languages
Chinese (zh)
Other versions
CN112746177A (en
Inventor
谭毅
游小刚
崔弘阳
李毅
王轶农
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dalian University of Technology
Original Assignee
Dalian University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dalian University of Technology filed Critical Dalian University of Technology
Priority to CN202011582014.0A priority Critical patent/CN112746177B/en
Publication of CN112746177A publication Critical patent/CN112746177A/en
Application granted granted Critical
Publication of CN112746177B publication Critical patent/CN112746177B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/005—Preliminary treatment of scrap
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/001—Dry processes
    • C22B7/003—Dry processes only remelting, e.g. of chips, borings, turnings; apparatus used therefor
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

The invention provides a method for refining and purifying high-temperature alloy return by using electron beams, which comprises the following steps: s1, preprocessing a high-temperature alloy raw material; and S2, refining and purifying the high-temperature alloy return material by using an electron beam to obtain a high-purity FGH4096 high-temperature alloy cast ingot. The invention adopts the electron beam refining means to purify the high-temperature alloy return material, utilizes the environment of high temperature and high vacuum to ensure that the melt fully generates degassing reaction, utilizes local large overheating in the electron beam refining process to realize the dissolution of small-size inclusion in the melt, and removes the large-size inclusion floating to the surface of the melt through the gettering of the condensation rod, thereby comprehensively reducing the content of the impurity and the inclusion in the high-temperature alloy return material and ensuring that the purity of the return material reaches the application level.

Description

Method for refining and purifying high-temperature alloy return material by using electron beams
Technical Field
The invention relates to a method for refining and purifying high-temperature alloy return by using electron beams.
Background
The high-temperature alloy material is widely applied to the fields of aerospace, petrochemical industry, industrial gas turbines and the like. The annual demand of the high-temperature alloy in China is huge, and the annual demand of only casting the high-temperature alloy is up to 5000 tons. The high-temperature alloy can generate a large amount of return materials in the forms of risers, runners, waste parts and the like in the preparation process, for example, the yield of the wrought alloy prepared by the traditional duplex process is not higher than 60 percent, the weight of the cast single-crystal alloy final part is only about 30 percent of that of the raw materials, and the rest of the cast single-crystal alloy final part exists in the form of the return materials. These returns generally have more inclusions than the virgin ones and higher levels of harmful impurity elements (O, N, S, etc.) and therefore must be subjected to rigorous processing before further use.
The application research work of the return materials in China starts late, the recovery of the return materials is mainly vacuum induction high-temperature refining and casting filtration, the related technical level of the purification and the reutilization of the return materials is far from the large gap compared with that of the foreign developed countries, and the related standards and the specifications of the recovery and the reutilization of the return materials are not established. In the aspect of controlling impurities and inclusions, the purity of the return alloy ingot in China cannot reach the level of a new material, so that the utilization rate of the current high-temperature alloy return material is segregated, and the serious waste of resources is caused.
Disclosure of Invention
According to the proposed recycling of the current return materials, vacuum induction high-temperature refining and casting filtration are mainly used, the related technical level of the purification and recycling of the return materials has a larger gap compared with that of foreign developed countries, and related standards and specifications of the recycling and recycling of the return materials are not established; in the aspect of controlling impurities and inclusions, the purity of the return alloy ingot in China cannot reach the level of a new material, so that the technical problems of utilization rate segregation of the current high-temperature alloy return and serious waste of resources are caused, and the method for refining and purifying the high-temperature alloy return by using the electron beams is provided. The invention mainly adopts the electron beam refining means to purify the high-temperature alloy return material, utilizes the environment of high temperature and high vacuum to ensure that the melt fully generates degassing reaction, utilizes local large overheating in the electron beam refining process to realize the dissolution of small-size inclusion in the melt, and removes the large-size inclusion floating to the surface of the melt through the gettering of the condensation rod, thereby comprehensively reducing the content of impurities and inclusion in the high-temperature alloy return material and ensuring that the purity of the return material reaches the application level.
The technical means adopted by the invention are as follows:
a method for refining and purifying high-temperature alloy return by an electron beam comprises the following steps:
s1, pretreatment of the high-temperature alloy raw material:
s11, the raw material is FGH4096 alloy return;
s12, processing the return material to a proper size, wherein the return material can be placed into a water-cooled copper crucible for refining;
s13, polishing the processed return material, and removing ceramic adhesion, an oxidation layer, processing traces and the like on the surface to ensure that the return material alloy has no external pollutants;
s14, cleaning and drying the polished return material for later use;
s2, refining and purifying the high-temperature alloy return material by using an electron beam:
s21, cleaning the water-cooled copper crucible for electron beam refining: polishing, wiping with alcohol and drying to ensure that the water-cooled copper crucible is clean and pollution-free;
s22, cleaning pollutants on the furnace body and the furnace wall of the electron beam melting furnace, and avoiding the introduction of foreign impurities in the refining process;
s23, placing the pretreated return material in a water-cooled copper crucible, and closing the furnace door of the electron beam melting furnace after the readiness is determined and the furnace body is cleaned;
s24, pre-vacuumizing the electron beam smelting furnace and the electron gun body to reach the target vacuum degree; preheating the electron gun after the target vacuum degree is reached;
s25, after preheating, melting the return material in the water-cooled copper crucible by using an electron gun;
s26, after the alloy returning material is completely melted, refining the alloy melt in a ring scanning mode through electron beams;
s27, increasing the beam current of the electron beam after refining is finished, and realizing large overheating of the melt;
s28, arc closing is carried out in a slow beam falling mode to a final solidification area of the edge area of the cast ingot;
s29, carrying out rapid gettering treatment on large-size inclusions enriched in the final solidification region;
s210, closing the electron beam melting system, firstly closing the high voltage of an electron gun, increasing the beam current of the electron gun to a certain value to reduce the high voltage from 30kV to 0kV, and then closing the beam current of the electron gun;
s211, fully cooling the cast ingot in the water-cooling copper crucible, and taking out the FGH4096 alloy cast ingot after the furnace body, the gun body and the cast ingot are fully cooled, thereby obtaining the high-purity FGH4096 high-temperature alloy cast ingot.
Further, the specific steps of step S14 are as follows:
and (3) ultrasonically cleaning the polished FGH4096 alloy return material by using deionized water and alcohol respectively, cleaning for three times by using the deionized water and the ultrasonic, placing the alloy into a drying box after cleaning, and drying at 30 ℃ for electron beam refining.
Further, the specific steps of step S24 are as follows:
opening electron beam refining equipment, and pumping the furnace body and the electron gun body of the electron beam smelting furnace to a target vacuum state, wherein the vacuum degree of the furnace body is required to be less than 5 multiplied by 10-2Pa, the vacuum degree of the gun body is required to be less than 5 multiplied by 10-3Pa, starting two electron guns after the target vacuum degree is reached, enabling the beam current size to be 120mA, and preheating for 12 minutes.
Further, the specific steps of step S25 are as follows:
after preheating, adjusting the beam current of the electron gun to 0, starting high voltage, increasing the beam current of the electron beam after the high voltage reaches 30kV and is stabilized, adjusting the radius of a beam spot to 10mm after the beam spot of the electron beam is found in the water-cooled copper crucible for smelting, uniformly moving the beam spot of the electron beam, uniformly heating the return material in the water-cooled copper crucible, and continuously increasing the beam current of the electron beam to 500 mA.
Further, the specific steps of step S26 are as follows:
after the alloy returning material is completely melted, the radius of the beam spot of the electron beam is adjusted to 25mm, the alloy melt is refined in an annular scanning mode for 10min, so that impurities such as O, N in the alloy are fully removed, and meanwhile, large-size impurities gradually float to the surface of the melt.
Further, the specific steps of step S27 are as follows:
after refining is finished, the size of the electron beam is increased to 800mA, the holding time is 10min, and therefore the melt is overheated greatly, small-size inclusions and ordered atomic groups in the melt are fully diffused and dissolved, and the alloy melt is uniform in structure and component distribution.
Further, the specific steps of step S28 are as follows:
and gradually reducing the beam current by adopting a slow beam descending mode, and simultaneously shrinking the radius of a beam spot, so that the beam current is reduced to 0mA within 5min, the radius of the beam spot is reduced to 0mm, and the arc is closed to a final solidification region of the edge region of the cast ingot.
Further, the specific steps of step S29 are as follows:
the method comprises the following steps of (1) carrying out rapid gettering treatment on large-size inclusions enriched in a final solidification region: when the arc-contracting zone is about to solidify, the cold source rod is inserted into the arc-contracting zone through the operating handle and is slowly stirred, so that large-size impurities are gradually enriched on the cold source rod, and the condensation rod is pulled out before the cast ingot is completely solidified.
Compared with the prior art, the invention has the following advantages:
1. the method for refining and purifying the high-temperature alloy return material by the electron beam creatively provides a method for purifying the high-temperature alloy return material by adopting an electron beam refining method aiming at the characteristic of high content of impurities and impurities in the return material, leads the melt to fully generate degassing reaction by utilizing the high-temperature and high-vacuum environment in the electron beam refining process, fully degasses the melt so as to remove volatile impurities such as O, N, S and the like, realizes the dissolution of small-size impurities in the melt by utilizing local large overheating in the electron beam refining process, namely accelerates the dissolution of the small-size impurities in the melt by fully overheating the melt, promotes the floating and aggregation of the large-size impurities in the melting process by utilizing the density difference between the impurities and the melt and the Marangoni effect, further utilizes a condensing rod to absorb and remove the large-size impurities floating to the surface of the melt, therefore, the contents of impurities and inclusions in the high-temperature alloy return material are comprehensively reduced, the purity of the return material reaches the application level, and the method has important significance for reducing the manufacturing cost of the high-temperature alloy in China and promoting the sustainable development of the high-temperature alloy industry in China.
2. According to the method for purifying the high-temperature alloy return by electron beam refining, the prepared high-temperature alloy return cast ingot is low in impurity content, the content of inclusions in the alloy and the maximum size of the inclusions are lower than those of the high-temperature alloy prepared by the traditional process, and a new method is provided for recycling the high-temperature alloy return.
In conclusion, the technical scheme of the invention can solve the problems that the recovery of the return materials is mainly vacuum induction high-temperature refining and casting filtration, the related technical level of the purification and the reutilization of the return materials has a larger gap compared with the foreign developed countries, and the related standards and specifications of the recovery and the reutilization of the return materials are not established; in the aspect of controlling impurities and inclusions, the purity of the return alloy ingot in China cannot reach the level of a new material, so that the utilization rate of the current high-temperature alloy return material is segregated, and the problem of serious waste of resources is caused.
Based on the reasons, the method can be widely popularized in the fields of purification of high-temperature alloy return materials 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 needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic view of the process of removing inclusions by electron beam super-heated dissolution according to the present invention.
FIG. 2 is a schematic drawing of gettering large-sized inclusions on the surface according to the present invention.
In the figure: 1. an oil diffusion pump; 2. a valve; 3. a mechanical pump; 4. local overheating areas of the melt; 5. small-size inclusions in the melt; 6. an alloy melt; 7. a pulling ingot mechanism; 8. cooling water; 9. an electron gun; 10. an electron beam; 11. large-size impurities floating to the surface of the melt; 12. water-cooling the copper crucible; 13. a roots pump 14 and a cold source impurity absorbing rod; 15. large-sized inclusions aggregated in the final solidification zone.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present 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 invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective portions shown in the drawings are not drawn in an actual proportional relationship for the 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. Any specific values in all examples shown and discussed herein are to be construed as exemplary only and not as limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
As shown in the figure, the invention provides a method for refining and purifying high-temperature alloy return by using an electron beam, which comprises the following steps:
pretreatment of high-temperature alloy raw materials
1. Taking the FGH4096 alloy as an example, the FGH4096 alloy return material is processed to a proper size so as to be put into a water-cooled copper refining crucible.
2. And polishing the processed return material to remove ceramic adhesion, an oxide layer, processing traces and the like on the surface, so that the return material alloy has no external pollutants.
3. And (3) ultrasonically cleaning the polished FGH4096 alloy return material by using deionized water and alcohol respectively, cleaning for three times by using the deionized water and the ultrasonic, placing the alloy into a drying box after cleaning, and drying at 30 ℃ for electron beam refining.
Secondly, refining and purifying the high-temperature alloy return material by using electron beams
1. And cleaning (polishing, alcohol wiping and drying) the water-cooled copper crucible for electron beam refining to ensure that the water-cooled copper crucible is clean and pollution-free.
2. Cleaning the furnace body and the furnace wall of the electron beam melting furnace, and avoiding the introduction of foreign impurities in the refining process.
3. And (3) placing the pretreated FGH4096 alloy return in a water-cooled copper refining crucible, and closing the furnace door of the electron beam smelting furnace after the readiness is determined and the furnace body is cleaned.
4. Opening electron beam refining equipment, and pumping the furnace body and the electron gun body of the electron beam smelting furnace to a target vacuum state, wherein the vacuum degree of the furnace body is required to be less than 5 multiplied by 10-2Pa, the vacuum degree of the gun body is required to be less than 5 multiplied by 10-3Pa, starting two electron guns after the target vacuum degree is reached, enabling the beam current size to be 120mA, and preheating for 12 minutes.
5. After preheating, adjusting the beam current of the electron gun to 0, starting high voltage, increasing the beam current of the electron beam after the high voltage reaches 30kV and is stabilized, adjusting the radius of a beam spot to 10mm after the beam spot of the electron beam is found in the water-cooled copper crucible for smelting, uniformly moving the beam spot of the electron beam, uniformly heating the return material in the water-cooled copper crucible, and continuously increasing the beam current of the electron beam to 500 mA.
6. After the alloy returning material is completely melted, the radius of the beam spot of the electron beam is adjusted to 25mm, the alloy melt is refined in an annular scanning mode for 10min, so that impurities such as O, N in the alloy are fully removed, and meanwhile, large-size impurities gradually float to the surface of the melt.
7. After refining is finished, the size of the electron beam is increased to 800mA, the holding time is 10min, and therefore the melt is overheated greatly, small-size inclusions and ordered atomic groups in the melt are fully diffused and dissolved, and the alloy melt is uniform in structure and component distribution (figure 1).
8. And gradually reducing the beam current by adopting a slow beam descending mode, and simultaneously shrinking the radius of a beam spot, so that the beam current is reduced to 0mA within 5min, the radius of the beam spot is reduced to 0mm, and the arc is closed to a final solidification region of the edge region of the cast ingot.
9. Carrying out rapid impurity-absorbing treatment on large-size impurities enriched in the final solidification zone, specifically: when the arc-closing region is about to be solidified, the cold source rod is inserted into the arc-closing region through the operating handle and is slowly stirred, so that large-size impurities are gradually enriched on the cold source rod, and the condensation rod is pulled out before the cast ingot is completely solidified (figure 2).
10. And (3) closing the electron beam melting system, firstly closing the high voltage of the electron gun, increasing the beam current of the electron gun to a certain value to reduce the high voltage from 30kV to 0kV, and then closing the beam current of the electron gun.
11. And fully cooling the cast ingot in the water-cooled copper crucible, and taking out the FGH4096 alloy cast ingot after the furnace body, the gun body and the cast ingot are fully cooled, thereby obtaining the high-purity FGH4096 high-temperature alloy cast ingot.
FIG. 1 is a schematic view showing the process of removing inclusions by electron beam hot melting, and FIG. 2 is a schematic view showing the gettering of large-sized inclusions on the surface. The present invention adopts the equipment shown in figure 1 and figure 2 to purify the high-temperature alloy return material. The electron gun 9 is fixed at two side corners of the top of the electron beam melting furnace, the water-cooled copper crucible 12 is placed at the bottom of the electron beam melting furnace, cooling water 8 is introduced, the ingot pulling mechanism 7 is arranged below the water-cooled copper crucible 12, and the up-and-down motion of the water-cooled copper crucible 12 can be controlled through the ingot pulling mechanism 7. The FGH4096 alloy returns are placed in a water cooled copper crucible 12 and within the scanning range of the electron beam 10. The oil diffusion pump 1 is adjacent to the mechanical pump 3, and the communication relationship between the oil diffusion pump 1 and the mechanical pump is controlled by a valve 2; the roots pump 13 is adjacent to the furnace body mechanical pump 3, and the two are connected together. The alloy melt 6 is a molten metal material in a water-cooled copper crucible 12 and forms a local superheat zone 4 of the melt after melting. In the electron beam refining process, low-density inclusions in the molten metal continuously float upwards to form large-size inclusions 11 floating to the surface of the melt, and the inclusions are sucked away through a cold source impurity sucking rod 14; the melt is overheated greatly, so that small-size inclusions 5 in the melt are fully diffused and dissolved; and drawing the large-size inclusion 11 floating to the surface of the melt to the edge of the upper surface of the melt by controlling arc closing and solidification to form the large-size inclusion 15 gathered in a final solidification region.
According to the method, gas impurities such as O, N, S and the like in the high-temperature alloy return material are fully removed through a high-temperature high-vacuum environment in an electron beam refining process, the melt is fully overheated to dissolve small-size inclusions in the melt, the floating and aggregation of the large-size inclusions in the melting process are promoted by using the density difference between the inclusions and the melt and the Marangoni effect, and then the large-size inclusions are removed by using the adsorption effect of a condensation rod, so that the contents of the impurities and the inclusions in the high-temperature alloy return material ingot are fully reduced. The high-temperature alloy return material cast ingot prepared by the method has low impurity content, and the content of inclusions and the maximum size of the inclusions in the alloy are lower than those of the high-temperature alloy prepared by the traditional process, so that a new method is provided for recycling the high-temperature alloy return material.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (8)

1. A method for refining and purifying high-temperature alloy return by using electron beams is characterized in that the high-temperature alloy return is purified by using an electron beam refining means, a melt is fully subjected to a degassing reaction by using a high-temperature high-vacuum environment, small-size impurities in the melt are dissolved by using local large overheating in the electron beam refining process, and the large-size impurities floating to the surface of the melt are removed by absorbing impurities through a condensation rod, so that the contents of impurities and impurities in the high-temperature alloy return are comprehensively reduced, and the purity of the return reaches an application level;
the method comprises the following steps:
s1, pretreatment of the high-temperature alloy raw material:
s11, the raw material is FGH4096 alloy return;
s12, processing the return material to a proper size, wherein the return material can be placed into a water-cooled copper crucible for refining;
s13, polishing the processed return material to remove ceramic adhesion, an oxidation layer and processing traces on the surface, so that the return material alloy has no external pollutants;
s14, cleaning and drying the polished return material for later use;
s2, refining and purifying the high-temperature alloy return material by using an electron beam:
s21, cleaning the water-cooled copper crucible for electron beam refining: polishing, wiping with alcohol and drying to ensure that the water-cooled copper crucible is clean and pollution-free;
s22, cleaning pollutants on the furnace body and the furnace wall of the electron beam melting furnace, and avoiding the introduction of foreign impurities in the refining process;
s23, placing the pretreated return material in a water-cooled copper crucible, and closing the furnace door of the electron beam melting furnace after the readiness is determined and the furnace body is cleaned;
s24, pre-vacuumizing the electron beam smelting furnace and the electron gun body to reach the target vacuum degree; preheating the electron gun after the target vacuum degree is reached;
s25, after preheating, melting the return material in the water-cooled copper crucible by using an electron gun;
s26, after the alloy returning material is completely melted, refining the alloy melt in a ring scanning mode through electron beams;
s27, increasing the beam current of the electron beam after refining is finished, and realizing large overheating of the melt;
s28, arc closing is carried out in a slow beam falling mode to a final solidification area of the edge area of the cast ingot;
s29, carrying out rapid gettering treatment on large-size inclusions enriched in the final solidification region;
s210, closing the electron beam melting system, firstly closing the high voltage of an electron gun, increasing the beam current of the electron gun to a certain value to reduce the high voltage from 30kV to 0kV, and then closing the beam current of the electron gun;
s211, fully cooling the cast ingot in the water-cooling copper crucible, and taking out the FGH4096 alloy cast ingot after the furnace body, the gun body and the cast ingot are fully cooled to obtain the high-purity FGH4096 high-temperature alloy cast ingot.
2. The method for refining and purifying superalloy returns according to claim 1, wherein the step S14 is embodied as follows:
and (3) ultrasonically cleaning the polished FGH4096 alloy return material by using deionized water and alcohol respectively, cleaning for three times by using the deionized water and the ultrasonic, placing the alloy into a drying box after cleaning, and drying at 30 ℃ for electron beam refining.
3. The method for refining and purifying superalloy returns according to claim 1, wherein the step S24 is embodied as follows:
opening electron beam refining equipment, and pumping the furnace body and the electron gun body of the electron beam smelting furnace to a target vacuum state, wherein the vacuum degree of the furnace body is required to be less than 5 multiplied by 10-2Pa, the vacuum degree of the gun body is required to be less than 5 multiplied by 10-3Pa, starting two electron guns after the target vacuum degree is reached, enabling the beam current size to be 120mA, and preheating for 12 minutes.
4. The method for refining and purifying superalloy returns according to claim 1 or 2, wherein the step S25 is embodied as follows:
after preheating, adjusting the beam current of the electron gun to 0, starting high voltage, increasing the beam current of the electron beam after the high voltage reaches 30kV and is stabilized, adjusting the radius of a beam spot to 10mm after the beam spot of the electron beam is found in the water-cooled copper crucible for smelting, uniformly moving the beam spot of the electron beam, uniformly heating the return material in the water-cooled copper crucible, and continuously increasing the beam current of the electron beam to 500 mA.
5. The method for refining and purifying superalloy returns according to claim 1, wherein the step S26 is embodied as follows:
after the alloy return material is completely melted, the radius of the beam spot of the electron beam is adjusted to 25mm, the alloy melt is refined in an annular scanning mode for 10min, so that O, N impurities in the alloy are fully removed, and meanwhile, large-size impurities gradually float to the surface of the melt.
6. The method for refining and purifying superalloy returns according to claim 1, wherein the step S27 is embodied as follows:
after refining is finished, the size of the electron beam is increased to 800mA, the holding time is 10min, and therefore the melt is overheated greatly, small-size inclusions and ordered atomic groups in the melt are fully diffused and dissolved, and the alloy melt is uniform in structure and component distribution.
7. The method for refining and purifying superalloy returns according to claim 1, wherein the step S28 is embodied as follows:
and gradually reducing the beam current by adopting a slow beam descending mode, and simultaneously shrinking the radius of a beam spot, so that the beam current is reduced to 0mA within 5min, the radius of the beam spot is reduced to 0mm, and the arc is closed to a final solidification region of the edge region of the cast ingot.
8. The method for refining and purifying superalloy returns according to claim 1, wherein the step S29 is embodied as follows:
the method comprises the following steps of (1) carrying out rapid gettering treatment on large-size inclusions enriched in a final solidification region: when the arc-contracting zone is about to solidify, the cold source rod is inserted into the arc-contracting zone through the operating handle and is slowly stirred, so that large-size impurities are gradually enriched on the cold source rod, and the condensation rod is pulled out before the cast ingot is completely solidified.
CN202011582014.0A 2020-12-28 2020-12-28 Method for refining and purifying high-temperature alloy return material by using electron beams Active CN112746177B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011582014.0A CN112746177B (en) 2020-12-28 2020-12-28 Method for refining and purifying high-temperature alloy return material by using electron beams

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011582014.0A CN112746177B (en) 2020-12-28 2020-12-28 Method for refining and purifying high-temperature alloy return material by using electron beams

Publications (2)

Publication Number Publication Date
CN112746177A CN112746177A (en) 2021-05-04
CN112746177B true CN112746177B (en) 2022-02-18

Family

ID=75646395

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011582014.0A Active CN112746177B (en) 2020-12-28 2020-12-28 Method for refining and purifying high-temperature alloy return material by using electron beams

Country Status (1)

Country Link
CN (1) CN112746177B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112095019B (en) * 2020-08-11 2021-07-30 大连理工大学 Method for removing inclusions in high-temperature alloy through electron beam overheating dissolution
CN113976918B (en) * 2021-07-29 2023-04-04 江苏奇纳新材料科技有限公司 Remelting process for metal powder return material in additive manufacturing
CN116790924B (en) * 2023-08-25 2023-11-17 北京理工大学 Method for preparing refractory high-entropy alloy by remelting return materials through electron beam melting

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107267788A (en) * 2017-07-12 2017-10-20 大连理工大学 A kind of electron beam melting purification is combined the method for preparing high-purity nickel base superalloy with low-temperature receiver gettering
CN112095019A (en) * 2020-08-11 2020-12-18 大连理工大学 Method for removing inclusions in high-temperature alloy through electron beam overheating dissolution

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107267788A (en) * 2017-07-12 2017-10-20 大连理工大学 A kind of electron beam melting purification is combined the method for preparing high-purity nickel base superalloy with low-temperature receiver gettering
CN112095019A (en) * 2020-08-11 2020-12-18 大连理工大学 Method for removing inclusions in high-temperature alloy through electron beam overheating dissolution

Also Published As

Publication number Publication date
CN112746177A (en) 2021-05-04

Similar Documents

Publication Publication Date Title
CN112746177B (en) Method for refining and purifying high-temperature alloy return material by using electron beams
CN112095019B (en) Method for removing inclusions in high-temperature alloy through electron beam overheating dissolution
CN110423918B (en) Method for preparing high-purity nickel-based high-temperature alloy by electron beam induced refining casting technology
JP4523274B2 (en) High purity metallic silicon and its smelting method
CN105695777B (en) The method that electron beam directional solidification technique refines nickel base superalloy
CN107164639B (en) A kind of electron beam covers the method that formula solidification technology prepares high temperature alloy
CN112095030B (en) Method for preparing high-purity nickel-based high-temperature alloy by integrating vacuum induction melting and electron beam refining
CN107267788B (en) A kind of electron beam melting purification is combined the method for preparing high-purity nickel base superalloy with low-temperature receiver gettering
CN111961897B (en) Method for preparing high-purity nickel-based high-temperature alloy by vacuum induction melting-casting-electron beam refining process
CN112080662A (en) Method for preparing high-homogeneity nickel-based high-temperature alloy by electromagnetic stirring coupling electron beam layered solidification casting technology
CN107385244B (en) A kind of electron beam covers the method that induced coagulation technology High Purity prepares nickel base superalloy
CN102659110A (en) Method for directionally solidifying and purifying polycrystalline silicon by adopting ferro-silicon alloy
CN111549237B (en) Method for separating iron element impurities from pulse current in secondary aluminum melt
CN112760508A (en) Method for continuously refining high-temperature alloy return material by using electron beams
CN101603129B (en) Method for removing iron impurity from aluminium alloy
CN112746183B (en) Method for synchronously removing high-density impurities and low-density impurities in high-temperature alloy
CN112210673B (en) Method for removing inclusions in high-temperature alloy through electron beam surface pyrolysis
CN112813282B (en) Method for removing high-density inclusions in high-temperature alloy
CN112048624B (en) Method for improving component uniformity of nickel-based high-temperature alloy through electron beam circulating overtemperature treatment
CN112063864A (en) Method for preparing high-purity nickel-based high-temperature alloy by magnetic field enhanced electron beam refining pouring technology
CN110484742B (en) Method for preparing Fe-W intermediate alloy by electron beam melting and high purification
CN112746181B (en) Method for refining and refining carbide in high-temperature alloy by electron beam
CN112813281B (en) Method for removing low-density inclusions in high-temperature alloy by combining melt overheating and foamed ceramic filtering
US11981978B2 (en) Method for preparing high-purity nickel-based superalloy by electron beam induced refining and casting technology
CN112746188B (en) Method for preparing high-homogeneity nickel-based high-temperature alloy by external electric field and fluid cooling auxiliary coupling electron beam layer-solidifying pouring technology

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant