CN112048624A - Method for improving component uniformity of nickel-based high-temperature alloy through electron beam circulating overtemperature treatment - Google Patents
Method for improving component uniformity of nickel-based high-temperature alloy through electron beam circulating overtemperature treatment Download PDFInfo
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- CN112048624A CN112048624A CN202010962976.2A CN202010962976A CN112048624A CN 112048624 A CN112048624 A CN 112048624A CN 202010962976 A CN202010962976 A CN 202010962976A CN 112048624 A CN112048624 A CN 112048624A
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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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- 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
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
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- 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
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
Abstract
The invention provides a method for improving the component uniformity of a nickel-based high-temperature alloy by electron beam circulating over-temperature treatment. The method comprises the following steps: s1, preprocessing raw materials; s2, refining by electron beams; and S3, performing electron beam circulating overtemperature treatment on the alloy melt to obtain a refined 718 alloy. The invention adopts the electron beam circulation over-temperature technology to process the melt, breaks through the inheritance of the melt structure, fully utilizes the advantages of high electron beam melting temperature, easy control and the like to improve the uniformity of melt components, and finally realizes the high-homogeneity preparation of the alloy, thereby achieving the purpose of preparing the high-homogeneity nickel-based high-temperature alloy.
Description
Technical Field
The invention relates to a method for improving the component uniformity of a nickel-based high-temperature alloy by electron beam circulating overtemperature treatment.
Background
The nickel-based high-temperature alloy has good high-temperature strength and high-temperature creep property, excellent oxidation corrosion resistance and high-temperature fatigue resistance, and good long-term structure stability, and is increasingly important and widely applied to the industrial fields of aviation, aerospace, energy, chemical industry and the like.
The traditional smelting mode of the nickel-based superalloy at present comprises a double-linkage process of vacuum induction smelting and electric arc remelting, vacuum induction smelting and electric slag remelting and the like, a triple process of vacuum induction smelting and electric arc remelting, vacuum induction smelting and vacuum electric arc remelting and electric slag remelting and the like, and technologies of plasma remelting, powder metallurgy, electron beam rapid prototyping, laser cladding forming and the like. Although the multi-connection process, the powder metallurgy process, the electron beam rapid forming process and the laser cladding process can improve the metallurgical quality of the alloy and reduce the segregation of the cast ingot, the energy consumption is high, and the preparation cost of the alloy is increased.
The electron beam melting process is a melting type for melting materials by bombarding the surface of the materials by utilizing high-energy electron beam flow, has the characteristics of surface heating, high energy density and the like, and avoids the pollution of a water-cooled copper crucible to the alloy due to the use of the water-cooled copper crucible during melting. The technology is widely applied to smelting and purifying high-melting-point refractory metals and alloys thereof, solar-grade polycrystalline silicon, titanium and titanium alloys. During electron beam refining, the surface of the alloy melt is kept at a high smelting temperature by adjusting parameters such as smelting power, electron beam spot size, electron beam scanning path and the like, and impurity elements in the alloy can be effectively removed in a high-temperature high-vacuum environment. The bottom of the melt is in contact with a water-cooled copper crucible, and the segregation of the alloy can be reduced by a higher cooling speed. In the final stage of smelting, the size of the electron beam spot and the smelting power are reduced to enable inclusions in the melt to be enriched on the surface of the alloy, and the surface layer of the cast ingot is removed through polishing after the melt is solidified and cooled to achieve the purpose of removing the inclusions.
The nickel-based high-temperature alloy ingot prepared by the traditional method at present has the problems of large segregation degree, uneven components and the like, so that the rejection rate of the ingot is high, and the production cost is high. The invention provides a method for improving the component uniformity of a nickel-based high-temperature alloy by electron beam circulating over-temperature treatment.
Disclosure of Invention
The technical problems that the nickel-based high-temperature alloy ingot prepared by the conventional method has large segregation degree, uneven components and the like, so that the ingot rejection rate is high and the production cost is high are solved, and the method for improving the component uniformity of the nickel-based high-temperature alloy through electron beam circulating over-temperature treatment is provided. The method mainly utilizes the electron beam circulating over-temperature technology to process the melt, breaks through the inheritance of the melt structure, fully utilizes the advantages of high electron beam melting temperature, easy control and the like to improve the uniformity of melt components, and finally realizes the high-homogeneity preparation of the alloy, thereby achieving the purpose of preparing the high-homogeneity nickel-based high-temperature alloy.
The technical means adopted by the invention are as follows:
a method for improving the component uniformity of a nickel-based superalloy by electron beam circulating overtemperature treatment comprises the following steps:
s1, pretreatment of raw materials:
s11, the raw material is a rod-shaped 718 alloy;
s12, cutting the rodlike 718 alloy into cylinders with the diameter of 100mm multiplied by 8mm, and polishing the cut 718 alloy by using a grinding machine to remove stains and oxide skin on the surface;
s13, cleaning the polished 718 alloy: respectively cleaning with deionized water and alcohol, and cleaning the polished 718 alloy by using an ultrasonic cleaning machine;
s14, after cleaning, drying the 718 alloy by using a blower, and after electron beam melting;
s2, electron beam refining:
s21, cleaning the inside of the furnace body of the electron beam melting furnace: polishing the surface of the water-cooled copper crucible for electron beam refining by using No. 2000 abrasive paper, and wiping the water-cooled copper crucible by using cotton cloth stained with alcohol to ensure that the water-cooled copper crucible is clean and pollution-free;
s22, placing the preprocessed 718 alloy in the middle of a water-cooled copper crucible, cleaning the interior of a furnace body of the electron beam melting furnace, and closing a furnace door after the cleaning is confirmed;
s23, vacuumizing a melting chamber and an electron gun chamber of the electron beam melting furnace to reach a target vacuum degree;
s24, preheating the filament of the electron gun after the vacuum degree meets the requirement; after the electron gun is preheated, carrying out electron beam melting on the 718 alloy in the water-cooled copper crucible;
s3, electron beam circulation overtemperature treatment of the alloy melt:
s31, after the alloy in the water-cooled copper crucible is completely melted, carrying out overtemperature treatment;
s32, repeating the overtemperature treatment operation of the step S31 for 3 times to decompose clusters in the melt and improve the uniformity of the alloy melt;
s33, after the circulating overtemperature treatment is finished, turning off a high-voltage power supply of the electron gun, reducing the beam current to 0mA, and turning off the electron gun;
and S34, after the electron beam melting furnace is cooled for 40min, introducing argon twice to continue cooling the furnace body, and after the furnace body is completely cooled, removing the refined 718 alloy.
Further, the specific steps of step S23 are as follows:
opening cooling water, air compressor, and power switch of electron beam melting equipment, vacuumizing the melting chamber and electron gun chamber of the electron beam melting furnace, wherein the vacuum degree of the melting chamber is required to be less than 5 × 10-2Pa, the vacuum degree of the electron gun chamber is required to be less than 5 x 10- 3Pa。
Further, the specific steps of step S24 are as follows:
starting an electron gun after the vacuum degrees of the smelting chamber and the electron gun chamber reach the requirement, slowly adjusting the beam current to 120mA, and preheating for 12 min;
after the electron gun is preheated, reducing the beam current to 0, starting the high voltage of the electron gun, slowly increasing the beam current to 500mA after the voltage reaches 30kV and is stabilized for 1min, and the radius of the scanning surface is 10 multiplied by 10; the melting power was kept constant and alloy 718 was gradually melted by adjusting the beam spot scanning path.
Further, in step S31, the specific steps of the over-temperature processing are as follows:
s311, after the alloy in the water-cooled copper crucible is completely melted, slowly reducing the beam current to 200mA at the speed of 50 mA/min;
and S312, keeping for 1min after the beam current is reduced to 200mA, continuously increasing the beam current to 500mA, and keeping for 1min under the condition of 500mA beam current.
Further, in step S311, the beam current is decreased to ensure that the alloy in the water-cooled copper crucible is still in a molten state.
Further, the diameter of the rod-shaped 718 alloy is 20-50 mm.
Compared with the prior art, the invention has the following advantages:
1. the method for improving the component uniformity of the nickel-based high-temperature alloy through the electron beam circulating over-temperature treatment improves the component uniformity of the nickel-based high-temperature alloy, the prepared cast ingot is low in segregation degree, the secondary dendrite spacing is small, and the performance of the nickel-based high-temperature alloy can be further improved. Meanwhile, the method can reduce the homogenization heat treatment time of the cast ingot and reduce the preparation cost of the alloy.
2. According to the method for improving the component uniformity of the nickel-based high-temperature alloy through the electron beam circulating overtemperature treatment, provided by the invention, the melt is treated by adopting the electron beam circulating overtemperature technology, the inheritance of the melt structure is broken, the uniformity of the components of the melt is improved by fully utilizing the advantages of high electron beam melting temperature, easiness in control and the like, and finally the high-homogeneity preparation of the alloy is realized, so that the aim of preparing the high-homogeneity nickel-based high-temperature alloy is fulfilled.
3. According to the method for improving the component uniformity of the nickel-based superalloy through the electron beam circulating overtemperature treatment, provided by the invention, the electron beam circulating overtemperature treatment is used for carrying out melt treatment on the nickel-based superalloy, so that the advantages of high electron beam heating temperature, easiness in operation and control and the like are integrated, the inheritance of clusters in the nickel-based superalloy is reduced, and the uniformity of the nickel-based superalloy is further improved. The secondary dendrite spacing of the cast ingot is reduced by one half compared with the traditional smelting mode.
In conclusion, the technical scheme of the invention can solve the problems of high ingot rejection rate and high production cost caused by the problems of large segregation degree, uneven components and the like of the nickel-based high-temperature alloy ingot prepared by the traditional method.
Based on the reasons, the invention can be widely popularized in the fields of alloy preparation and the like.
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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 an electron beam circulation over-temperature melt processing apparatus according to the present invention.
In the figure: 1. an electron gun; 2. a diffusion pump; 3. a pneumatic valve; 4. a mechanical pump; 5. an electron beam; 6. water-cooling the copper crucible; 7. a roots pump; 8. a crucible support; 9. a cooling water pipeline I; 10. a cooling water pipeline II; 11. and (4) an alloy molten pool.
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 improving the component uniformity of a nickel-based superalloy by electron beam circulating overtemperature treatment, which comprises the following steps:
firstly, pretreatment of raw materials
1. The raw material uses a rod-shaped 718 alloy with the diameter of 20-50 mm.
2. The 718 alloy bar is cut into small cylinders with the diameter of 100mm multiplied by 8mm, the surfaces of the small cylinders are polished by a grinding machine, and stains and oxide scales on the surfaces are removed. Because the water-cooled copper crucible is smaller, 718 alloy bars need to be cut into small blocks or small cylinders to be placed into the water-cooled copper crucible for smelting, and the small blocks which can be placed into the water-cooled copper crucible in other sizes can also be cut.
3. And cleaning the polished 718 alloy respectively by using deionized water and alcohol, cleaning the alloy by using an ultrasonic cleaning machine, and drying the alloy by using a blower until the alloy is melted by using an electron beam.
Second, electron beam refining
1. The method comprises the following steps of cleaning the inside of a furnace body of an electron beam melting furnace, polishing the surface of the water-cooled copper crucible smoothly by using 2000# abrasive paper, and wiping the water-cooled copper crucible by using cotton cloth stained with alcohol so as to ensure that the water-cooled copper crucible is clean and pollution-free.
2. And (3) placing the 718 alloy which is cut and cleaned completely in the middle of the water-cooled copper crucible, cleaning the interior of the furnace body, and closing the furnace door after the cleaning is confirmed.
3. Turning on cooling water, air compressor, and power switch of electron beam melting equipment, vacuumizing the melting chamber and electron gun chamber, wherein the vacuum degree of the melting chamber is required to be less than 5 × 10-2Pa, the vacuum degree of the electron gun chamber is required to be less than 5 x 10-3Pa. And starting an electron gun after the vacuum degrees of the smelting chamber and the electron gun chamber reach the requirement, slowly adjusting the beam current to 120mA, and preheating for 12 min.
4. After the electron gun is preheated, the beam current is reduced to 0, the high voltage of the electron gun is started, the beam current is slowly increased to 500mA after the voltage reaches 30kV and is stabilized for 1min, and the radius of the scanning surface is 10 multiplied by 10. The melting power was kept constant and alloy 718 was gradually melted by adjusting the beam spot scanning path.
Thirdly, electron beam circulation overtemperature treatment of alloy melt
1. After the alloy in the water-cooled copper crucible is completely melted, the beam current is slowly reduced to 200mA at the speed of 50mA/min, and the alloy in the water-cooled copper crucible is ensured to be still in a molten state in the process of reducing the beam current.
2. Keeping the beam current for 1min after reducing to 200mA, then continuing to increase the beam current to 500mA, and keeping the beam current for 1min under the condition of 500 mA.
3. The above-mentioned overtemperature treatment operation is repeated for 3 times, so that the clusters in the melt are decomposed, and the uniformity of the alloy melt is improved.
4. And after the circulating overtemperature treatment is finished, the high-voltage power supply of the electron gun is closed, and the electron gun is closed after the beam current is reduced to 0 mA.
5. And after the electron beam melting furnace is cooled for 40min, argon is introduced twice to continue cooling the furnace body, and after the furnace body is completely cooled, the refined 718 alloy is removed.
FIG. 1 is a schematic diagram of an electron beam circulation overtemperature melt processing device, which is used for carrying out electron beam circulation overtemperature processing so as to improve the component uniformity of the nickel-based superalloy. Electron gun 1 is equipped with in electron beam melting furnace's smelting room shell top both sides, and water-cooling copper crucible 6 places in smelting the room shell through crucible support 8, and cooling water piping I9 is connected in one side of electron beam melting furnace, and cooling water piping II 10 is connected with water-cooling copper crucible 6's bottom, and during raw and other materials added water-cooling copper crucible 6 to be in the 5 scanning range of electron beam of electron gun 1, form alloy molten bath 11 after the raw and other materials melts. 3 diffusion pumps 2, 3 mechanical pumps 4 and a roots pump 7 are arranged outside the electron beam melting furnace, wherein one end of one diffusion pump 2 is connected with the electron beam melting furnace, and the other end of the diffusion pump is communicated with the mechanical pump 4 through a pneumatic valve 3 on the left side of the upper part of the electron beam melting furnace; one end of a diffusion pump 2 is connected with the electron beam melting furnace, and the other end of the diffusion pump is communicated with a mechanical pump 4 through a pneumatic valve 3; on the right side of the middle part of the electron beam melting furnace, one end of a diffusion pump 2 is connected with the electron beam melting furnace, the other end is connected with one end of a roots pump 7, one end of the roots pump 7 is also connected with the electron beam melting furnace, and the other end is connected with a mechanical pump 4.
The method of the invention uses the electron beam to carry out melt processing on the nickel-based superalloy by circulating overtemperature, integrates the advantages of high electron beam heating temperature, easy operation and control and the like, reduces the inheritance of clusters in the nickel-based superalloy, and further improves the uniformity of the nickel-based superalloy. The secondary dendrite spacing of the cast ingot is reduced by one half compared with the traditional smelting mode.
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 (6)
1. A method for improving the component uniformity of a nickel-based superalloy by electron beam circulating overtemperature treatment is characterized by comprising the following steps:
s1, pretreatment of raw materials:
s11, the raw material is a rod-shaped 718 alloy;
s12, cutting the rodlike 718 alloy into cylinders with the diameter of 100mm multiplied by 8mm, and polishing the cut 718 alloy by using a grinding machine to remove stains and oxide skin on the surface;
s13, cleaning the polished 718 alloy: respectively cleaning with deionized water and alcohol, and cleaning the polished 718 alloy by using an ultrasonic cleaning machine;
s14, after cleaning, drying the 718 alloy by using a blower, and after electron beam melting;
s2, electron beam refining:
s21, cleaning the inside of the furnace body of the electron beam melting furnace: polishing the surface of the water-cooled copper crucible for electron beam refining by using No. 2000 abrasive paper, and wiping the water-cooled copper crucible by using cotton cloth stained with alcohol to ensure that the water-cooled copper crucible is clean and pollution-free;
s22, placing the preprocessed 718 alloy in the middle of a water-cooled copper crucible, cleaning the interior of a furnace body of the electron beam melting furnace, and closing a furnace door after the cleaning is confirmed;
s23, vacuumizing a melting chamber and an electron gun chamber of the electron beam melting furnace to reach a target vacuum degree;
s24, preheating the filament of the electron gun after the vacuum degree meets the requirement; after the electron gun is preheated, carrying out electron beam melting on the 718 alloy in the water-cooled copper crucible;
s3, electron beam circulation overtemperature treatment of the alloy melt:
s31, after the alloy in the water-cooled copper crucible is completely melted, carrying out overtemperature treatment;
s32, repeating the overtemperature treatment operation of the step S31 for 3 times to decompose clusters in the melt and improve the uniformity of the alloy melt;
s33, after the circulating overtemperature treatment is finished, turning off a high-voltage power supply of the electron gun, reducing the beam current to 0mA, and turning off the electron gun;
and S34, after the electron beam melting furnace is cooled for 40min, introducing argon twice to continue cooling the furnace body, and after the furnace body is completely cooled, removing the refined 718 alloy.
2. The method for improving the uniformity of the components of the nickel-base superalloy by the electron beam cyclic overtemperature treatment according to claim 1, wherein the step S23 is as follows:
opening cooling water, air compressor, and power switch of electron beam melting equipment, vacuumizing the melting chamber and electron gun chamber of the electron beam melting furnace, wherein the vacuum degree of the melting chamber is required to be less than 5 × 10-2Pa, the vacuum degree of the electron gun chamber is required to be less than 5 x 10-3Pa。
3. The method for improving the uniformity of the components of the nickel-base superalloy by the electron beam cyclic overtemperature treatment according to claim 1, wherein the step S24 is as follows:
starting an electron gun after the vacuum degrees of the smelting chamber and the electron gun chamber reach the requirement, slowly adjusting the beam current to 120mA, and preheating for 12 min;
after the electron gun is preheated, reducing the beam current to 0, starting the high voltage of the electron gun, slowly increasing the beam current to 500mA after the voltage reaches 30kV and is stabilized for 1min, and the radius of the scanning surface is 10 multiplied by 10; the melting power was kept constant and alloy 718 was gradually melted by adjusting the beam spot scanning path.
4. The method for improving the uniformity of the components of the nickel-base superalloy by electron beam cyclic overtemperature treatment according to claim 1, wherein the overtemperature treatment in the step S31 comprises the following specific steps:
s311, after the alloy in the water-cooled copper crucible is completely melted, slowly reducing the beam current to 200mA at the speed of 50 mA/min;
and S312, keeping for 1min after the beam current is reduced to 200mA, continuously increasing the beam current to 500mA, and keeping for 1min under the condition of 500mA beam current.
5. The method for improving the uniformity of the components of the Ni-based superalloy through the electron beam cycling overtemperature treatment as claimed in claim 4, wherein in step S311, the beam current is reduced while the alloy in the water-cooled copper crucible is still in a molten state.
6. The method of claim 1, wherein the rod 718 alloy has a diameter of 20-50 mm.
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| CN112746181A (en) * | 2020-12-28 | 2021-05-04 | 大连理工大学 | Method for refining and refining carbide in high-temperature alloy by electron beam |
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