CN106884110A - A kind of method that high vacuum electric arc furnaces prepares nickel base superalloy - Google Patents
A kind of method that high vacuum electric arc furnaces prepares nickel base superalloy Download PDFInfo
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- CN106884110A CN106884110A CN201710187602.6A CN201710187602A CN106884110A CN 106884110 A CN106884110 A CN 106884110A CN 201710187602 A CN201710187602 A CN 201710187602A CN 106884110 A CN106884110 A CN 106884110A
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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%
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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
- 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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Abstract
The present invention relates to a kind of method that high vacuum electric arc furnaces prepares nickel base superalloy.The method is mainly included the following steps that:First, the preparation of raw material, the raw material needed for preparation method melting nickel base superalloy Inconel718 has:Nickel plate, ingot iron, High Pure Chromium, High-purity Niobium, rafifinal, high purity titanium, High-Purity Molybdenum.By nickel plate and the surface removal of impurities of ingot iron raw material, after carrying out grinding polishing, it is cleaned by ultrasonic with deionized water and absolute ethyl alcohol, drying.Then composition proportion is carried out according to standard alloy composition;2nd, shove charge, the raw material that will be prepared is positioned in the melting kettle of high vacuum arc-melting furnace, extracts high vacuum, then passes to high-purity argon gas as protection gas;3rd, the melting of alloy, under the protection of argon gas, striking simultaneously carries out melting, is stirred after magnetic after whole melting sources, is opened, and carries out multiple melting, after the completion of melting, extinguishes electric arc, and alloy cast ingot is obtained after cooling.This method is easy to operate, improves preparation efficiency.
Description
Technical field
The invention belongs to nickel base superalloy preparing technical field, and in particular to a kind of high vacuum electric arc furnaces prepares Ni-based height
The method of temperature alloy.
Background technology
The research and development of nickel base superalloy and application start from the thirties in 20th century, and it is in high temperature alloy field in occupation of weighing very much
The status wanted.Britain produces nickel-base alloy Nimonic75 in nineteen forty-one first, and the U.S. and the Soviet Union then also develop Ni-based height
Temperature alloy, China just develops nickel base superalloy in the mid-50.
Nickel base superalloy still has good mechanical property, antioxygenic property, anti-corruption in the extreme environment of high temperature
Corrosion energy, welding performance and workability energy etc., is constantly subjected to the favor of scientific researcher.Current nickel base superalloy by
It is widely used in various devices and environment, for example:Space flight and aviation engine, ocean drilling-production equipment, valve and stone
Preparation of oil-piping etc..Therefore, development of the research nickel base superalloy to fields such as China's Aero-Space is significant.
The research work of nickel base superalloy is concentrated mainly on two aspects:The design and producing technique of alloying component changes
Enter.The tissue of nickel base superalloy and the quality of performance, in addition to being influenceed by the degree of purity of raw materials, largely
Depending on smelting equipment and technological process.At present, conventional nickel base superalloy smelting equipment mainly includes vaccum sensitive stove, electricity
Slag remelting furnace, vacuum arc remelting furnace etc..The smelting technology for generally using is multi-joint technique, and the technique is complex and cumbersome.
Go out master alloy ingot with vacuum induction melting first, then carry out the refining and purification of alloy pig.Follow-up refining process is general
Including electroslag remelting and vacuum arc remelting.
At present, the preparation method of domestic and international nickel base superalloy generally adds electroslag remelting, vacuum induction using vacuum induction
Plus vacuum arc remelting, vacuum induction adds the duplexs such as electroslag remelting plus vacuum arc remelting or three techniques, this production technology
Sufficiently complex, capacity usage ratio is low, low production efficiency.And, production process there is a problem in that:Vacuum induction melting process
Alloy melt can be mingled with material reaction generation oxide in stove;Freezing rate is low during electroslag remelting, and electrode is easily in high-temperature condition
Lower oxidation;Electric arc remelting can not provide high vacuum, therefore can not completely remove the impurity elements such as deoxygenation and nitrogen;Alloy cast ingot surface lacks
Fall into more, scaling loss of low-melting alloy element etc..Therefore, a kind of process is simple is invented, production efficiency is high, product high purity
Nickel base superalloy preparation method seem very necessary.
The content of the invention
Technical problem:The present invention is to overcome above mentioned problem, there is provided a kind of high vacuum electric arc furnaces prepares nickel base superalloy
Method, raw material is matched according to standard analysis, is positioned in high vacuum electric arc furnaces, is stirred using magnetic, melting of revealing the exact details, upset casting
The modes such as ingot, multiple melting, effectively reduce impurity content and alloying component segregation, so as to obtain the nickel-base high-temperature of high-purity
Alloy cast ingot.
Technical scheme:The method that a kind of high vacuum electric arc furnaces of the invention prepares nickel base superalloy comprises the following steps:
1) preparation of raw material:Raw material needed for preparation method melting nickel base superalloy Inconel718 has nickel plate, work
The pure iron of industry, chromium, niobium, aluminium, titanium, molybdenum, nickel plate and ingot iron need to carry out removing surface, after being ground and being polished, spend
Ionized water is cleaned, and is cleaned by ultrasonic in absolute ethyl alcohol, is dried, then according to the standard of nickel base superalloy Inconel718
Alloying component is matched;
2) shove charge:Pure titanium ingot is positioned in center of arc furnace crucible, the alloy raw material for having matched is put into other melting earthenwares
In crucible;The placement rule of raw material is that dystectic raw metal is positioned over crucible top, and the raw metal of low melting point is positioned over earthenware
Crucible bottom, then carries out extracting the operation of vacuum, treats that vacuum reaches 5 × 10-3During Pa, stop pumping, be filled with pure argon to true
Reciprocal of duty cycle is -0.05MPa;
3) melting of alloy:The melting of pure titanium ingot is carried out first, and startup power supply carries out striking, after preheating 3-5 minutes, by
Melting electric current is gradually increased, after after the fusing completely of titanium ingot, melting 3-5 minutes, electric current to minimum is gradually reduced, extinguishes electric arc;Then
The melting of alloy is carried out, electrode bar is gone into melting kettle top, startup power supply carries out striking, after preheating 3-5 minutes, gradually
Melting electric current is increased, treats that raw material melts completely substantially, open magnetic stirring switch, magnetic stirring is carried out to melt, be gradually increased magnetic and stir
Electric current is mixed, crucible bottom can be extremely seen, after reveal the exact details melting 3-5 minutes, magnetic stir current to minimum is gradually reduced, magnetic is closed
Stirring switch, gradually decreases melting electric current to minimum, extinguishes electric arc, cools down 5-10 minutes, overturns ingot casting;It is repeated several times above-mentioned molten
Refining process, after being cooled to room temperature, alloy cast ingot is taken out in blow-on, that is, obtain nickel base superalloy Inconel718 ingot castings.
Nickel plate in the raw material, ingot iron, and the purity of other simple metal raw materials is all higher than 99.9%, pure argon
Purity be more than 99.999%.
In fusion process, coordination electrode rod rotates melting electric arc, electric arc is fully swept to the surface of melt.
Repeat during fusion process, being transferred to alloy cast ingot after melting 3-4 times carries out melting behaviour in clean crucible
Make.
At the end of melting, after electric current is minimized, electric arc is fully scanned alloy cast ingot surface 2-3 minutes, then extinguish
Electric arc.
Before alloy cast ingot is taken out in blow-on, after room temperature need to being cooled to, air is filled with.
Beneficial effect:
(1) cleaning of raw material, effectively reduces the introducing of impurity, and under high-purity argon gas protection, first melting titanium ingot enters one
Oxygen in step removal stove, purifies furnace air, prevents from being oxidized during alloy melting.
(2) in loading furnace process, on crucible top, low-melting-point metal is conducive to raw material fast to refractory metal in crucible bottom
The fusing of speed, reduces the scaling loss of low melting point volatile alloy element.
(3) present invention is stirred by using magnetic, melting is repeated several times, it is ensured that each alloy raw material fully melts, so as to have
Effect reduces the segregation of refractory metal element (such as niobium).
(4) alloy cast ingot is transferred in clean crucible during melt back, can effectively reduces the content of impurity,
Improve the degree of purity of alloy cast ingot.
(5) at the end of melting, electric arc is extinguished again after fully scanning alloy cast ingot surface 2-3 minutes, effectively prevent casting
Ingot Local cooling is too fast to cause the defects such as crackle.
(6) blow-on sampling before, after being cooled to room temperature, be filled with air, it is therefore prevented that the too high ingress of air of ingot casting temperature and by oxygen
Change.
(7) present invention uses high vacuum electric arc furnaces, and a shove charge can complete the melting of alloy, process is simple, operation side
Just, it is adapted to laboratory and prepares small-sized high-purity nickel base superalloy ingot casting.
(8) by after identical Technology for Heating Processing, its mechanical property of the present invention is melted out nickel-base alloy Inconel718 is excellent
In it is conventionally produced go out the alloy.Tensile strength and yield strength the lifting 5%-10% of alloy, the plasticity of alloy are obtained
Significantly improve.
Brief description of the drawings
The nickel base superalloy Inconel718 micro-organization charts that Fig. 1 is melted out.
The tensile strength and yield strength of the Inconel718 under the identical Technologies for Heating Processing of Fig. 2.
Specific embodiment
The present invention is described in detail with reference to specific embodiment, but the invention is not limited in specific embodiment.Implement
Example one
(1) preparation of raw material:The raw material of use has a nickel plate, ingot iron, High Pure Chromium, High-purity Niobium, rafifinal, high purity titanium,
High-Purity Molybdenum.Nickel plate and ingot iron need to carry out removing surface, after being ground and being polished, are cleaned with deionized water, anhydrous
Ethanol is cleaned by ultrasonic, drying, is then matched according to standard alloy composition.Its composition proportion is:Nickel 26.911g;Chromium
9.805g;Niobium 2.654g;Molybdenum 1.462g;Titanium 0.452g;Aluminium 0.204g;Iron 8.512g.
(2) shove charge:Titanium ingot is positioned in center of arc furnace crucible, the alloy raw material for preparing is put into other melting kettles
Interior, it is that dystectic metal is positioned over crucible top to place rule, and the metal of low melting point is positioned over crucible bottom.Then carry out
Vacuumize, treat that vacuum reaches 5 × 10-3During Pa, stop pumping, be filled with argon gas to -0.05MPa.
(3) melting of alloy:The melting of pure titanium ingot is carried out first, and startup power supply carries out striking, after preheating 3-5 minutes, by
Melting electric current to 250-350mA is gradually increased, after after the fusing completely of titanium ingot, melting 3-5 minutes, electric current to minimum is gradually reduced, put out
Go out electric arc.Then the melting of alloy is carried out, electrode bar is gone into melting kettle top, startup power supply carries out striking, preheats 3-5
After minute, melting electric current being gradually increased to 250-350mA, treating that raw material melts completely substantially, open magnetic stirring switch, melt is entered
Row magnetic is stirred, and is gradually increased magnetic stir current, can extremely see crucible bottom, after reveal the exact details melting 3-5 minutes, is gradually reduced magnetic
Stir current closes magnetic stirring switch to minimum, gradually decreases melting electric current to minimum, extinguishes electric arc, cools down 5-10 minutes, turns over
Turn ingot casting.Above-mentioned fusion process is repeated several times.After being cooled to room temperature, alloy cast ingot is taken out, that is, obtain nickel base superalloy
Inconel718 ingot castings.Fig. 1 is the nickel base superalloy Inconel718 micro-organization charts for melting out.
(4) melting gained alloy carries out chemical composition detection, and each element percentage composition is nickel 53.20;Chromium 18.20g;Niobium
5.78;Molybdenum 2.83;Titanium 0.849;Aluminium 0.406;Iron 18.51;Carbon 0.027;The each element content such as sulphur 0.0068 meets into minute mark
It is accurate.
Embodiment two
(1) preparation of raw material:The raw material of use has a nickel plate, ingot iron, High Pure Chromium, High-purity Niobium, rafifinal, high purity titanium,
High-Purity Molybdenum.Nickel plate and ingot iron need to carry out removing surface, after being ground and being polished, are cleaned with deionized water, anhydrous
Ethanol is cleaned by ultrasonic, drying, is then matched according to standard alloy composition.Its composition proportion is:Nickel 27.061g;Chromium
9.846g;Niobium 2.695g;Molybdenum 1.495g;Titanium 0.550g;Aluminium 0.196g;Iron 8.797g.
(2) shove charge:Titanium ingot is positioned in center of arc furnace crucible, the alloy raw material for preparing is put into other melting kettles
Interior, it is that dystectic metal is positioned over crucible top to place rule, and the metal of low melting point is positioned over crucible bottom.Then carry out
Vacuumize, treat that vacuum reaches 5 × 10-3During Pa, stop pumping, be filled with argon gas to -0.05MPa.
(3) melting of alloy:The melting of pure titanium ingot is carried out first, and startup power supply carries out striking, after preheating 3-5 minutes, by
Melting electric current to 250-350mA is gradually increased, after after the fusing completely of titanium ingot, melting 3-5 minutes, electric current to minimum is gradually reduced, put out
Go out electric arc.Then the melting of alloy is carried out, electrode bar is gone into melting kettle top, startup power supply carries out striking, preheats 3-5
After minute, melting electric current being gradually increased to 250-350mA, treating that raw material melts completely substantially, open magnetic stirring switch, melt is entered
Row magnetic is stirred, and is gradually increased magnetic stir current, can extremely see crucible bottom, after reveal the exact details melting 3-5 minutes, is gradually reduced magnetic
Stir current closes magnetic stirring switch to minimum, gradually decreases melting electric current to minimum, extinguishes electric arc, cools down 5-10 minutes, turns over
Turn ingot casting.Above-mentioned fusion process is repeated several times.After being cooled to room temperature, alloy cast ingot is taken out, that is, obtain nickel base superalloy
Inconel718 ingot castings.
(4) melting gained alloy carries out chemical composition detection, and each element percentage composition is:Nickel 50.4;Chromium 20.32g;Niobium
5.50;Molybdenum 2.82;Titanium 0.843;Aluminium 0.382;Iron 18.88;Carbon 0.025;The each element content such as sulphur 0.0042 meets into minute mark
It is accurate.
Embodiment three
(1) preparation of raw material:The raw material of use has a nickel plate, ingot iron, High Pure Chromium, High-purity Niobium, rafifinal, high purity titanium,
High-Purity Molybdenum.Nickel plate and ingot iron need to carry out removing surface, after being ground and being polished, are cleaned with deionized water, anhydrous
Ethanol is cleaned by ultrasonic, drying, is then matched according to standard alloy composition.Its composition proportion is:Nickel 26.940g;Chromium
9.522g;Niobium 2.719g;Molybdenum 1.529g;Titanium 0.501g;Aluminium 0.195g;Iron 8.639g.
(2) shove charge:Titanium ingot is positioned in center of arc furnace crucible, the alloy raw material for preparing is put into other melting kettles
Interior, it is that dystectic metal is positioned over crucible top to place rule, and the metal of low melting point is positioned over crucible bottom.Then carry out
Vacuumize, treat that vacuum reaches 5 × 10-3During Pa, stop pumping, be filled with argon gas to -0.05MPa.
(3) melting of alloy:The melting of pure titanium ingot is carried out first, and startup power supply carries out striking, after preheating 3-5 minutes, by
Melting electric current to 250-350mA is gradually increased, after after the fusing completely of titanium ingot, melting 3-5 minutes, electric current to minimum is gradually reduced, put out
Go out electric arc.Then the melting of alloy is carried out, electrode bar is gone into melting kettle top, startup power supply carries out striking, preheats 3-5
After minute, melting electric current being gradually increased to 250-350mA, treating that raw material melts completely substantially, open magnetic stirring switch, melt is entered
Row magnetic is stirred, and is gradually increased magnetic stir current, can extremely see crucible bottom, after reveal the exact details melting 3-5 minutes, is gradually reduced magnetic
Stir current closes magnetic stirring switch to minimum, gradually decreases melting electric current to minimum, extinguishes electric arc, cools down 5-10 minutes, turns over
Turn ingot casting.Above-mentioned fusion process is repeated several times.After being cooled to room temperature, alloy cast ingot is taken out, that is, obtain nickel base superalloy
Inconel718 ingot castings.
(4) melting gained alloy carries out chemical composition detection, and each element percentage composition is:Nickel 52.9;Chromium 18.19;Niobium
5.77;Molybdenum 2.84;Titanium 0.855;Aluminium 0.407;Iron 18.64;Carbon 0.0261;The each element content such as sulphur 0.0066 meets into minute mark
It is accurate.
Claims (6)
1. a kind of method that high vacuum electric arc furnaces prepares nickel base superalloy, it is characterised in that the method is comprised the following steps:
1) preparation of raw material:Raw material needed for preparation method melting nickel base superalloy Inconel718 has nickel plate, technical pure
Iron, chromium, niobium, aluminium, titanium, molybdenum, nickel plate and ingot iron need to carry out removing surface, after being ground and being polished, uses deionization
Water is cleaned, and is cleaned by ultrasonic in absolute ethyl alcohol, is dried, then according to the standard alloy of nickel base superalloy Inconel718
Composition is matched;
2) shove charge:Pure titanium ingot is positioned in center of arc furnace crucible, the alloy raw material for having matched is put into other melting kettles;
The placement rule of raw material is that dystectic raw metal is positioned over crucible top, and the raw metal of low melting point is positioned over crucible bottom
Portion, then carries out extracting the operation of vacuum, treats that vacuum reaches 5 × 10-3During Pa, stop pumping, be filled with pure argon to vacuum
For -0.05MPa;
3) melting of alloy:The melting of pure titanium ingot is carried out first, startup power supply carries out striking, after preheating 3-5 minutes, gradually add
Big melting electric current, after after the fusing completely of titanium ingot, melting 3-5 minutes, is gradually reduced electric current to minimum, extinguishes electric arc;Then carry out
The melting of alloy, melting kettle top is gone to by electrode bar, and startup power supply carries out striking, after preheating 3-5 minutes, is gradually increased
Melting electric current, treats that raw material melts completely substantially, opens magnetic stirring switch, and magnetic stirring is carried out to melt, is gradually increased magnetic stirring electricity
Stream, can extremely see crucible bottom, after reveal the exact details melting 3-5 minutes, be gradually reduced magnetic stir current to minimum, close magnetic stirring
Switch, gradually decreases melting electric current to minimum, extinguishes electric arc, cools down 5-10 minutes, overturns ingot casting;Above-mentioned melting is repeated several times
Journey, after being cooled to room temperature, alloy cast ingot is taken out in blow-on, that is, obtain nickel base superalloy Inconel718 ingot castings.
2. a kind of method that high vacuum electric arc furnaces prepares nickel base superalloy according to claim 1, it is characterised in that:It is described
The purity of the nickel plate in raw material, ingot iron, and other simple metal raw materials is all higher than 99.9%, and the purity of pure argon is more than
99.999%.
3. a kind of method that high vacuum electric arc furnaces prepares nickel base superalloy according to claim 1, it is characterised in that:Melting
During, coordination electrode rod rotates melting electric arc, electric arc is fully swept to the surface of melt.
4. a kind of method that high vacuum electric arc furnaces prepares nickel base superalloy according to claim 1, it is characterised in that:Repeat
In fusion process, being transferred to alloy cast ingot after melting 3-4 times carries out smelting operation in clean crucible.
5. a kind of method that high vacuum electric arc furnaces prepares nickel base superalloy according to claim 1, it is characterised in that:Melting
At the end of, after electric current is minimized, electric arc is fully scanned alloy cast ingot surface 2-3 minutes, then extinguish electric arc.
6. a kind of method that high vacuum electric arc furnaces prepares nickel base superalloy according to claim 1, it is characterised in that:Blow-on
Before taking out alloy cast ingot, after room temperature need to being cooled to, air is filled with.
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Cited By (5)
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CN108546834A (en) * | 2018-04-16 | 2018-09-18 | 北京科技大学 | A kind of nickel base superalloy master alloy sublimate method of smelting |
CN108788101A (en) * | 2018-07-20 | 2018-11-13 | 广东省焊接技术研究所(广东省中乌研究院) | A kind of sheet nickel base superalloy and preparation method thereof |
CN111041255A (en) * | 2019-12-09 | 2020-04-21 | 江苏隆达超合金航材有限公司 | Vacuum induction smelting feeding method for reducing inclusion content of high-temperature master alloy |
CN111074102A (en) * | 2020-02-16 | 2020-04-28 | 广东石油化工学院 | Method for desulfurizing nickel-based high-temperature alloy |
CN114183448A (en) * | 2021-12-14 | 2022-03-15 | 苏州昭伍亿精密五金有限公司 | High-strength corrosion-resistant bolt and production process thereof |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108546834A (en) * | 2018-04-16 | 2018-09-18 | 北京科技大学 | A kind of nickel base superalloy master alloy sublimate method of smelting |
CN108788101A (en) * | 2018-07-20 | 2018-11-13 | 广东省焊接技术研究所(广东省中乌研究院) | A kind of sheet nickel base superalloy and preparation method thereof |
CN108788101B (en) * | 2018-07-20 | 2020-03-24 | 广东省焊接技术研究所(广东省中乌研究院) | Preparation method of sheet nickel-based superalloy |
CN111041255A (en) * | 2019-12-09 | 2020-04-21 | 江苏隆达超合金航材有限公司 | Vacuum induction smelting feeding method for reducing inclusion content of high-temperature master alloy |
CN111074102A (en) * | 2020-02-16 | 2020-04-28 | 广东石油化工学院 | Method for desulfurizing nickel-based high-temperature alloy |
CN114183448A (en) * | 2021-12-14 | 2022-03-15 | 苏州昭伍亿精密五金有限公司 | High-strength corrosion-resistant bolt and production process thereof |
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