CN105695777B - The method that electron beam directional solidification technique refines nickel base superalloy - Google Patents
The method that electron beam directional solidification technique refines nickel base superalloy Download PDFInfo
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- CN105695777B CN105695777B CN201610139446.1A CN201610139446A CN105695777B CN 105695777 B CN105695777 B CN 105695777B CN 201610139446 A CN201610139446 A CN 201610139446A CN 105695777 B CN105695777 B CN 105695777B
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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
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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
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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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
- C22C1/12—Making non-ferrous alloys by processing in a semi-solid state, e.g. holding the alloy in the solid-liquid phase
Abstract
The invention discloses a kind of method that electron beam directional solidification technique refines nickel base superalloy, with following steps：S1, nickel base superalloy pretreatment；S2, electron beam melting purification and drawing ingot.The present invention improves the degree of purity of 718 high temperature alloys, and wherein S and P content are respectively lower than 0.002wt.% and 0.01wt.%；Improve the performance of 718 high temperature alloys so that 718 high temperature alloys have excellent antioxygenic property and resistance to electrochemical corrosion energy, the parabola oxidation kinetics constant at 1000 DEG C is 12.62g2/m4.h, the 718 high temperature alloy (47.62g prepared far below traditional approach2/m4.h), after Overheating Treatment, it is separated out, and γ ` phase sizes are tiny (about 10nm), and dispersion-strengthened effect is notable so that 718 high temperature alloys have higher Vickers hardness number.
Description
Technical field
The present invention relates to refining nickel base superalloy field, specifically a kind of electron beam directional solidification technique Refining Nickel
The method of based high-temperature alloy.
Background technology
In order to ensure that high temperature alloy has excellent quality level, it is necessary to strictly control chemical composition, improved from source
The degree of purity of high temperature alloy, and these depend primarily on smelting technology.The traditional preparation method of high temperature alloy has vacuum induction to melt
Refining power-up arc remelting, vacuum induction melting add the duplex technique such as electroslag remelting, and vacuum induction adds vacuum arc plus electroslag remelting, true
Sky sensing plus electroslag melting add the technique of vacuum arc remelting etc. three, powder metallurgy, electron beam rapid shaping technique, electron beam from
By molding fabrication techniques, laser cladding forming technology etc..Though duplex and multi-joint technique can effectively improve the metallurgical quality of alloy,
Energy consumption is larger, and the reaction of crucible and melt material can pollute molten bath during induction melting.Powder metallurgy and electron beam are fast
Though fast forming technique etc. can solve the problems, such as component segregation, the preparation of high temperature alloy powder body material adds cost, dusty material
Because larger specific surface area is easy to introduce defect in the alloy.
Electron beam melting purification is to make melt material and melting material using the surface of the beam bombardment material of high-energy-density
Technical process, the technology is widely used in the purification of solar-grade polysilicon, prepared by the refining of refractory metal and its alloy
In high-purity special steel and ultra clean steel, titanium and its alloy and other metal materials.Made by adjusting power and speed of melting
Molten bath is maintained at higher temperature, and degassing reaction fully occurs for melt in the environment of high temperature high vacuum, the smelting such as is conducive to being mingled with
The removal of the impurity such as golden defect and sulphur, phosphorus.In addition, crucible can be prevented effectively from using water jacketed copper crucible during electronic torch melting
Reacted with melt alloy, and then improve the degree of purity of alloy.The directional solidification technique of electron beam is high in electron beam melting purification
On the basis of temperature alloy, the preparation of large scale ingot casting is realized, can be prepared by changing the shape and size of water jacketed copper crucible
Go out various sizes of high temperature alloy ingot casting, the need for meeting actual production, the characteristics of electron beam directional solidification technique possesses and
Advantage becomes one of effective ways of the preparation high-purity high temperature alloy of large scale.Therefore, it is a kind of to use electron beam directional solidification
The method of technology refining nickel base superalloy is urgently researched and developed.
The content of the invention
According to technical problem set forth above, and provide a kind of electron beam directional solidification technique refining nickel base superalloy
Method.
The present invention has refined nickel base superalloy ingot casting using the method for electron beam melting purification, improves nickel base superalloy
Degree of purity, so as to improve the performance of high temperature alloy.Using friction feeding and ingot pulling mechanism, high temperature alloy is realized
Directional solidification.Large-sized high temperature alloy ingot casting can be obtained by this method, due to stable thermograde, crystal grain life
Length direction is parallel to ingot direction is drawn, and alloy structure and component distributing are more uniformly distributed.
The technological means that the present invention is used is as follows：
A kind of method that electron beam directional solidification technique refines nickel base superalloy, with following steps：
S1, nickel base superalloy pretreatment：
S11, using 718 high temperature alloy pole materials it is used as raw material；
S12,718 high temperature alloy pole materials are cut into coupon, and coupon one end is processed into internal thread；
S13, the oxide layer for removing coupon surface；
S14, coupon is cleaned, it is stand-by after drying；
S2, electron beam melting purification and drawing ingot：
S21, the water jacketed copper crucible in cleaning electron beam furnace and vertical ingot pulling mechanism drawing ingot end, water jacketed copper crucible
Bottom is the drawing ingot end of vertical ingot pulling mechanism；
S22, pretreated coupon is connected by straight feeding mechanism on the left of internal thread and electron beam furnace, passed through
Adjust straight feeding mechanism so that the other end of coupon is located above water jacketed copper crucible；
S23, the body of heater to electron beam furnace are cleared up；
S24, startup electron beam furnace, the vacuum of body of heater is evacuated to less than 5 × 10-2Pa, the vacuum of electron gun gun body
Degree is evacuated to less than 5 × 10-3Pa, afterwards, start be located at body of heater in left side electron gun and right side electron gun, make left side electron gun and
The line of right side electron gun is 120mA, is preheated 12 minutes；
S25, the line of left side electron gun and right side electron gun is adjusted to 0, starts high pressure, after slowly increasing after high-voltage-stable
Plus left side electron gun line is to 500mA, sweep radius is adjusted to 5 × 5mm, and regulation scanning pattern fusing coupon treats that coupon starts to melt
Start straight feeding mechanism after change, regulation stall is to shelves at a slow speed, and it is 20mm/min to make its feeding speed；
After S26,10min, right side electron gun line is slowly increased to 500mA, and it is 15 × 15mm, regulation to keep beam spot size
718 high temperature alloys that scanning pattern refining is fallen into water jacketed copper crucible；
After S27,10min, start vertical ingot pulling mechanism, regulation stall to shelves at a slow speed draws ingot speed degree for 10mm/min, downwards
Draw after ingot 1min, close vertical ingot pulling mechanism；
After S28,10min, vertical ingot pulling mechanism is restarted, regulation stall to shelves at a slow speed draws ingot speed degree for 10mm/min, downwards
Draw after ingot 1min, close vertical ingot pulling mechanism；
S29, repeat step S28, until straight feeding mechanism kinematic untill after range, by left side electron gun line
Adjust to 0,10min, right side electron gun line is adjusted to 0, close the high pressure of left side electron gun and right side electron gun, and simultaneously
Increase line to 60mA until high-voltage value is closing left side electron gun and right side electron gun after 0；Treat that electron beam furnace cools down 2h
718 alloy cast ingots of electron beam melting purification are taken out afterwards.
A diameter of 20-50mm of the coupon, a length of 1m.
The internal thread is the internal thread of M10 × 0.75, and the depth of thread is 30mm.
Grinding process is carried out to the coupon with emery wheel in the step S13, to remove the oxide layer on the coupon surface.
The coupon is cleaned by deionized water and alcohol respectively in the step S14, blown with hair-dryer cold wind
Do the coupon.
The water jacketed copper crucible and vertical ingot pulling mechanism cleared up in the step S21 with 1500# sand paper in electron beam furnace
Drawing ingot end, to surface both light after wiped using cotton with alcohol, untill contamination-free on cotton.
The present invention compared with prior art, improves the degree of purity of 718 high temperature alloys, and wherein S and P content are respectively lower than
0.002wt.% and 0.01wt.%；Improve the performance of 718 high temperature alloys so that 718 high temperature alloys have excellent resist
Oxidation susceptibility and resistance to electrochemical corrosion energy, as shown in Fig. 2 the parabola oxidation kinetics constant at 1000 DEG C is
12.62g2/m4.h, the 718 high temperature alloy (47.62g prepared far below traditional approach2/m4.h), after Overheating Treatment, it is separated out
γ ` phase sizes are tiny (about 10nm), and dispersion-strengthened effect is notable so that 718 high temperature alloys have higher Vickers hardness number.
The present invention can be widely popularized in fields such as refining nickel base superalloys for the foregoing reasons.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the knot of electron beam directional solidification technique refining nickel base superalloy device in embodiment of the invention
Structure schematic diagram.
Fig. 2 is a kind of 718 conjunctions of the method preparation of electron beam directional solidification technique refining nickel base superalloy of the present invention
The oxidizing dynamics curve for 718 alloys that gold is prepared with conventional method.
Embodiment
As shown in figure 1, a kind of method that electron beam directional solidification technique refines nickel base superalloy, with following steps：
S1, nickel base superalloy pretreatment：
S11, using 718 high temperature alloy pole materials it is used as raw material；
S12,718 high temperature alloy pole materials are cut into a diameter of 20-50mm, a length of 1m coupon 1, and by coupon 1 one
End processes the internal thread of M10 × 0.75, and the depth of thread is 30mm；
S13, with emery wheel grinding process is carried out to the coupon 1, to remove the oxide layer on the coupon surface.
S14, by deionized water and alcohol the coupon 1 is cleaned respectively, the examination is dried up with hair-dryer cold wind
It is stand-by after rod.
S2, electron beam melting purification and drawing ingot：
S21, the water jacketed copper crucible 2 cleared up with 1500# sand paper in electron beam furnace and vertical ingot pulling mechanism 3 drawing ingot end
4, to surface both light after wiped using cotton with alcohol, untill contamination-free on cotton, water jacketed copper crucible 2
Bottom is the drawing ingot end 4 of vertical ingot pulling mechanism 3；
S22, pretreated coupon 1 is connected by internal thread with the left side straight feeding mechanism 6 of electron beam furnace 5,
By adjusting straight feeding mechanism 6 so that the other end of coupon 1 is located at the top of water jacketed copper crucible 2；
S23, the body of heater to electron beam furnace 5 are cleared up；
S24, startup electron beam furnace 5, the vacuum of body of heater is evacuated to less than 5 × 10-2Pa, the vacuum of electron gun gun body
Degree is evacuated to less than 5 × 10-3Pa, afterwards, starts the left side electron gun 7 and right side electron gun 8 being located in body of heater, makes left side electron gun
7 and the line of right side electron gun 8 be 120mA, preheat 12 minutes；
S25, the line of left side electron gun 7 and right side electron gun 8 is adjusted to 0, starts high pressure, after slow after high-voltage-stable
The increase left side line of electron gun 7 is to 500mA, and sweep radius is adjusted to 5 × 5mm, and regulation scanning pattern fusing coupon 1 treats that coupon 1 is opened
Begin to start straight feeding mechanism 6 after fusing, regulation stall is to shelves at a slow speed, and it is 20mm/min to make its feeding speed；
After S26,10min, the right side line of electron gun 8 is slowly increased to 500mA, and it is 15 × 15mm to keep beam spot size, is adjusted
718 high temperature alloys that section scanning pattern refining is fallen into water jacketed copper crucible 2；
After S27,10min, start vertical ingot pulling mechanism 3, regulation stall to shelves at a slow speed draws ingot speed degree for 10mm/min, to
Pull down after ingot 1min, close vertical ingot pulling mechanism 3；
After S28,10min, vertical ingot pulling mechanism 3 is restarted, regulation stall to shelves at a slow speed draws ingot speed degree for 10mm/min, to
Pull down after ingot 1min, close vertical ingot pulling mechanism 3；
S29, repeat step S28, untill straight feeding mechanism 6 is moved to after range, by the beam of left side electron gun 7
Stream is adjusted to 0,10min, and the line of right side electron gun 8 is adjusted into 0, closes the high pressure of left side electron gun 7 and right side electron gun 8,
And increase line closes left side electron gun 7 and right side electron gun 8 to 60mA after high-voltage value is 0 simultaneously；Treat electronic torch melting
718 alloy cast ingots of electron beam melting purification are taken out after the cooling of stove 5 2h.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (6)
1. a kind of method that electron beam directional solidification technique refines nickel base superalloy, it is characterised in that with following steps：
S1, nickel base superalloy pretreatment：
S11, using 718 high temperature alloy pole materials it is used as raw material；
S12,718 high temperature alloy pole materials are cut into coupon, and coupon one end is processed into internal thread；
S13, the oxide layer for removing coupon surface；
S14, coupon is cleaned, it is stand-by after drying；
S2, electron beam melting purification and drawing ingot：
S21, the water jacketed copper crucible in cleaning electron beam furnace and vertical ingot pulling mechanism drawing ingot end, the bottom of water jacketed copper crucible
For the drawing ingot end of vertical ingot pulling mechanism；
S22, pretreated coupon be connected by straight feeding mechanism on the left of internal thread and electron beam furnace, pass through and adjust
Straight feeding mechanism so that the other end of coupon is located above water jacketed copper crucible；
S23, the body of heater to electron beam furnace are cleared up；
S24, startup electron beam furnace, the vacuum of body of heater is evacuated to less than 5 × 10-2Pa, the vacuum of electron gun gun body is taken out
To less than 5 × 10-3Pa, afterwards, starts the left side electron gun and right side electron gun being located in body of heater, makes left side electron gun and right side
The line of electron gun is 120mA, is preheated 12 minutes；
S25, the line of left side electron gun and right side electron gun is adjusted to 0, starts high pressure, after being slowly increased a left side after high-voltage-stable
Side electron gun line is to 500mA, and sweep radius is adjusted to 5 × 5mm, regulation scanning pattern fusing coupon, after coupon starts fusing
Start straight feeding mechanism, regulation stall is to shelves at a slow speed, and it is 20mm/min to make its feeding speed；
After S26,10min, right side electron gun line is slowly increased to 500mA, and it is 15 × 15mm, regulation scanning to keep beam spot size
718 high temperature alloys that path refining is fallen into water jacketed copper crucible；
After S27,10min, start vertical ingot pulling mechanism, regulation stall to shelves at a slow speed draws ingot speed degree for 10mm/min, pulls down ingot
After 1min, vertical ingot pulling mechanism is closed；
After S28,10min, vertical ingot pulling mechanism is restarted, regulation stall to shelves at a slow speed draws ingot speed degree for 10mm/min, pulls down ingot
After 1min, vertical ingot pulling mechanism is closed；
S29, repeat step S28, until straight feeding mechanism kinematic untill after range, left side electron gun line is adjusted
To 0,10min, right side electron gun line is adjusted to 0, the high pressure of left side electron gun and right side electron gun is closed, and increased simultaneously
Line is to 60mA until high-voltage value is closing left side electron gun and right side electron gun after 0；Taken after after electron beam furnace cooling 2h
Go out 718 alloy cast ingots of electron beam melting purification.
2. according to the method described in claim 1, it is characterised in that：A diameter of 20-50mm of the coupon, a length of 1m.
3. according to the method described in claim 1, it is characterised in that：The internal thread is the internal thread of M10 × 0.75, the depth of thread
For 30mm.
4. according to the method described in claim 1, it is characterised in that：The coupon is beaten with emery wheel in the step S13
Mill processing, to remove the oxide layer on the coupon surface.
5. according to the method described in claim 1, it is characterised in that：Pass through deionized water and alcohol respectively in the step S14
The coupon is cleaned, the coupon is dried up with hair-dryer cold wind.
6. according to the method described in claim 1, it is characterised in that：Melted in the step S21 with 1500# sand paper cleaning electron beam
The drawing ingot end of water jacketed copper crucible and vertical ingot pulling mechanism in furnace, to surface both light after wiped using cotton with alcohol
Wipe, untill contamination-free on cotton.
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| CN107164639B (en) * | 2017-06-27 | 2019-01-15 | 大连理工大学 | A kind of electron beam covers the method that formula solidification technology prepares high temperature alloy |
| CN107385244B (en) * | 2017-07-13 | 2019-01-15 | 大连理工大学 | A kind of electron beam covers the method that induced coagulation technology High Purity prepares nickel base superalloy |
| CN107574322B (en) * | 2017-08-29 | 2019-05-21 | 大连理工大学 | A kind of method that electron-beam smelting technology High Purity prepares nickel base superalloy |
| CN110423918B (en) * | 2019-08-01 | 2020-09-29 | 大连理工大学 | Method for preparing high-purity nickel-based high-temperature alloy by electron beam induced refining casting technology |
| CN112210673B (en) * | 2020-08-11 | 2022-06-10 | 大连理工大学 | Method for removing inclusions in high-temperature alloy through electron beam surface pyrolysis |
| CN112048624B (en) * | 2020-09-14 | 2021-08-03 | 大连理工大学 | Method for improving component uniformity of nickel-based high-temperature alloy through electron beam circulating overtemperature treatment |
| CN114134353A (en) * | 2021-11-25 | 2022-03-04 | 宁波江丰电子材料股份有限公司 | Aluminum-scandium alloy and preparation method and application thereof |
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| AU1474692A (en) * | 1991-06-05 | 1992-12-10 | General Electric Company | Method and apparatus for casting an electron beam melted metallic material in ingot form |
| CN104131165B (en) * | 2014-07-03 | 2017-04-12 | 大连理工大学 | Electron beam melting apparatus and method for preparing niobium-based superhigh temperature alloy by using electron beam melting apparatus |
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