CN106884110B - 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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- CN106884110B CN106884110B CN201710187602.6A CN201710187602A CN106884110B CN 106884110 B CN106884110 B CN 106884110B CN 201710187602 A CN201710187602 A CN 201710187602A CN 106884110 B CN106884110 B CN 106884110B
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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 methods that high vacuum electric arc furnaces prepares nickel base superalloy.This method mainly includes the following steps that：One, the preparation of raw material, the raw material needed for preparation method melting nickel base superalloy Inconel718 have：Nickel plate, ingot iron, High Pure Chromium, High-purity Niobium, rafifinal, high purity titanium, High-Purity Molybdenum.Nickel plate and ingot iron raw material surface are cleaned, carried out after grinding polishing, is cleaned by ultrasonic with deionized water and absolute ethyl alcohol, drying.Then composition proportion is carried out according to standard alloy ingredient；The raw material prepared is positioned in the melting kettle of high vacuum arc-melting furnace by two, shove charge, extracts high vacuum, then passes to high-purity argon gas as protection gas；Three, the melting of alloy, under the protection of argon gas, striking simultaneously carries out melting, after whole melting sources, opens magnetic stirring, and carry out multiple melting, after the completion of melting, extinguishes electric arc, 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 fields, 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 1930s, its in high temperature alloy field in occupation of very heavy
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 develop 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., are constantly subjected to the favor of scientific researcher.At present nickel base superalloy by
It is widely used in various devices and environment, such as：Space flight and aviation engine, ocean drilling-production equipment, valve and stone
The preparation etc. of oil-piping.Therefore, research nickel base superalloy is of great significance to the development in the fields such as China's aerospace.
The research work of nickel base superalloy is concentrated mainly on two aspects：The design and producing technique of alloying component changes
Into.The tissue of nickel base superalloy and the quality of performance, other than being influenced by the degree of purity of raw materials, largely
Depending on smelting equipment and technological process.Currently, common nickel base superalloy smelting equipment includes mainly vaccum sensitive stove, electricity
Slag remelting furnace, vacuum arc remelting furnace etc..The smelting technology of generally use is multi-joint technique, and the process is more complicated and cumbersome for this.
Go out master alloy ingot with vacuum induction melting first, then carries out the refining and purification of alloy pig.Subsequent refining process is general
Including electroslag remelting and vacuum arc remelting.
Currently, the preparation method generally use vacuum induction of nickel base superalloy adds electroslag remelting, vacuum induction both at home and abroad
Add vacuum arc remelting, vacuum induction that electroslag remelting is added to add the duplexs such as vacuum arc remelting or three techniques, this production technology
Sufficiently complex, capacity usage ratio is low, low production efficiency.Moreover, production process there is a problem in that：Vacuum induction melting process
Alloy melt can generate oxide with material reaction in stove and be mingled with；Solidification rate is low when electroslag remelting, and electrode is easily in high-temperature condition
Lower oxidation；Electric arc remelting cannot provide high vacuum, therefore cannot completely remove the impurity elements such as oxygen and nitrogen；Alloy cast ingot surface lacks
Fall into more, the scaling loss etc. of low-melting alloy element.Therefore, a kind of simple for process, production efficiency height is invented, product degree of purity is high
Nickel base superalloy preparation method seem very necessary.
Invention content
Technical problem：The present invention in order to overcome the problems referred above, provides a kind of high vacuum electric arc furnaces and prepares nickel base superalloy
Raw material is matched according to standard analysis, is positioned in high vacuum electric arc furnaces, is stirred using magnetic by method, melting of revealing the exact details, overturning casting
Ingot, the modes such as multiple melting effectively reduce impurity content and alloying component segregation, to obtain the nickel-base high-temperature of high-purity
Alloy cast ingot.
Technical solution：The method that a kind of high vacuum electric arc furnaces of the present invention prepares nickel base superalloy includes 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 progress removing surface to be spent after being ground and being polished
Ionized water cleans, and is cleaned by ultrasonic in absolute ethyl alcohol, dries, 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, proportioned alloy raw material 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
Then crucible bottom carries out the operation for extracting vacuum, waits for that vacuum degree reaches 5 × 10-3When Pa, stop pumping, is 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, startup power supply carries out striking, after preheating 3-5 minutes, by
Melting electric current is gradually increased, after the fusing completely of titanium ingot, melting 3-5 minutes is gradually reduced electric current to minimum, extinguishes electric arc；Then
Electrode bar is gone to melting kettle top by the melting for carrying out alloy, and startup power supply carries out striking, after preheating 3-5 minutes, gradually
Melting electric current is increased, waits for that raw material melts completely substantially, magnetic stirring switch is opened, magnetic stirring is carried out to melt, magnetic is gradually increased and stirs
Electric current is mixed, until can see crucible bottom, after melting 3-5 minutes of reveal the exact details, magnetic stir current is gradually reduced to minimum, closes magnetic
Stirring switch gradually decreases melting electric current to minimum, extinguishes electric arc, 5-10 minutes cooling, overturns ingot casting；It is repeated several times above-mentioned molten
Refining process, after being cooled to room temperature, blow-on takes out alloy cast ingot to get to nickel base superalloy Inconel718 ingot castings.
Nickel plate in the raw material, ingot iron, and the purity of other simple metal raw materials are all higher than 99.9%, pure argon
Purity be more than 99.999%.
In fusion process, coordination electrode stick rotates melting electric arc, electric arc is made fully to sweep to the surface of melt.
During repeating fusion process, alloy cast ingot is transferred to after melting 3-4 time in clean crucible and carries out melting behaviour
Make.
At the end of melting, after electric current minimizes, so that 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 need to being cooled to room temperature, it is filled with air.
Advantageous effect：
(1) cleaning of raw material effectively reduces the introducing of impurity, under high-purity argon gas protection, first melting titanium ingot, into one
Oxygen in step removal stove, purifies furnace air, prevents from being aoxidized during alloy melting.
(2) in loading furnace process, it is fast to be conducive to raw material in crucible bottom in crucible top, low-melting-point metal for refractory metal
The fusing of speed, reduces the scaling loss of low melting point volatile alloy element.
(3) present invention is stirred by using magnetic, and melting is repeated several times, ensure that each alloy raw material fully melts, 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, the content of impurity can be effectively reduced,
Improve the degree of purity of alloy cast ingot.
(5) at the end of melting, so that electric arc is fully scanned alloy cast ingot surface and extinguish again after 2-3 minutes, effectively prevent casting
Ingot Local cooling too fast the defects of causing crackle.
(6) blow-on sampling before, after being cooled to room temperature, be filled with air, it is therefore prevented that the excessively high ingress of air of ingot casting temperature and by oxygen
Change.
(7) present invention uses high vacuum electric arc furnaces, a shove charge that the melting of alloy, simple for process, operation side can be completed
Just, it is suitble to laboratory to prepare small-sized high-purity nickel base superalloy ingot casting.
(8) after identical heat treatment process, nickel-base alloy Inconel718 its mechanical property that the present invention melts out is excellent
In it is conventionally produced go out the alloy.The tensile strength and yield strength of alloy promote 5%-10%, and the plasticity of alloy obtains
It significantly improves.
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 Inconel718 under the identical heat treatment process of Fig. 2.
Specific implementation mode
With reference to specific embodiment, the present invention will be described in detail, but the invention is not limited in specific embodiments.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 progress removing surface to be cleaned with deionized water after being ground and being polished, anhydrous
Ethyl alcohol is cleaned by ultrasonic, then drying is matched according to standard alloy ingredient.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 prepared 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 it carries out
It vacuumizes, waits for that vacuum degree reaches 5 × 10-3When Pa, stop pumping, is filled with argon gas to -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, by
Melting electric current is gradually increased to 250-350mA, after the fusing completely of titanium ingot, melting 3-5 minutes is gradually reduced electric current to minimum, puts out
Go out electric arc.Electrode bar is gone to melting kettle top by the melting for then carrying out alloy, and startup power supply carries out striking, preheats 3-5
After minute, be gradually increased melting electric current to 250-350mA, wait for that raw material melt completely substantially, open magnetic and stir and switchs, to melt into
Row magnetic stirs, and is gradually increased magnetic stir current, until can see crucible bottom, after melting 3-5 minutes of reveal the exact details, is gradually reduced magnetic
Stir current closes magnetic stirring switch to minimum, gradually decreases melting electric current to minimum, extinguishes electric arc, 5-10 minutes cooling, 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 to get to nickel base superalloy
Inconel718 ingot castings.Fig. 1 is the nickel base superalloy Inconel718 micro-organization charts melted out.
(4) the carry out chemical composition detection of alloy obtained by melting, each element percentage composition are 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 elements 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 progress removing surface to be cleaned with deionized water after being ground and being polished, anhydrous
Ethyl alcohol is cleaned by ultrasonic, then drying is matched according to standard alloy ingredient.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 prepared 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 it carries out
It vacuumizes, waits for that vacuum degree reaches 5 × 10-3When Pa, stop pumping, is filled with argon gas to -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, by
Melting electric current is gradually increased to 250-350mA, after the fusing completely of titanium ingot, melting 3-5 minutes is gradually reduced electric current to minimum, puts out
Go out electric arc.Electrode bar is gone to melting kettle top by the melting for then carrying out alloy, and startup power supply carries out striking, preheats 3-5
After minute, be gradually increased melting electric current to 250-350mA, wait for that raw material melt completely substantially, open magnetic and stir and switchs, to melt into
Row magnetic stirs, and is gradually increased magnetic stir current, until can see crucible bottom, after melting 3-5 minutes of reveal the exact details, is gradually reduced magnetic
Stir current closes magnetic stirring switch to minimum, gradually decreases melting electric current to minimum, extinguishes electric arc, 5-10 minutes cooling, 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 to get to nickel base superalloy
Inconel718 ingot castings.
(4) the carry out chemical composition detection of alloy obtained by melting, each element percentage composition are：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 elements 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 progress removing surface to be cleaned with deionized water after being ground and being polished, anhydrous
Ethyl alcohol is cleaned by ultrasonic, then drying is matched according to standard alloy ingredient.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 prepared 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 it carries out
It vacuumizes, waits for that vacuum degree reaches 5 × 10-3When Pa, stop pumping, is filled with argon gas to -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, by
Melting electric current is gradually increased to 250-350mA, after the fusing completely of titanium ingot, melting 3-5 minutes is gradually reduced electric current to minimum, puts out
Go out electric arc.Electrode bar is gone to melting kettle top by the melting for then carrying out alloy, and startup power supply carries out striking, preheats 3-5
After minute, be gradually increased melting electric current to 250-350mA, wait for that raw material melt completely substantially, open magnetic and stir and switchs, to melt into
Row magnetic stirs, and is gradually increased magnetic stir current, until can see crucible bottom, after melting 3-5 minutes of reveal the exact details, is gradually reduced magnetic
Stir current closes magnetic stirring switch to minimum, gradually decreases melting electric current to minimum, extinguishes electric arc, 5-10 minutes cooling, 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 to get to nickel base superalloy
Inconel718 ingot castings.
(4) the carry out chemical composition detection of alloy obtained by melting, each element percentage composition are：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 elements 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, which is characterized in that this approach includes 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 to use deionization after being ground and being polished
Water cleans, and is cleaned by ultrasonic in absolute ethyl alcohol, dries, then according to the standard alloy of nickel base superalloy Inconel718
Ingredient is matched；
2) shove charge：Pure titanium ingot is positioned in center of arc furnace crucible, proportioned alloy raw material 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
Then portion carries out the operation for extracting vacuum, waits for that vacuum degree reaches 5 × 10-3When Pa, stops pumping, be filled with pure argon to vacuum degree
For -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, gradually adds
Big melting electric current, after the fusing completely of titanium ingot, melting 3-5 minutes is gradually reduced electric current to minimum, extinguishes electric arc；Then it carries out
Electrode bar is gone to melting kettle top by the melting of alloy, and startup power supply carries out striking, after preheating 3-5 minutes, is gradually increased
Melting electric current waits for that raw material melts completely substantially, opens magnetic stirring switch, magnetic stirring is carried out to melt, is gradually increased magnetic stirring electricity
Stream after melting 3-5 minute of reveal the exact details, is gradually reduced magnetic stir current to minimum, closes magnetic and stir until can see crucible bottom
Switch gradually decreases melting electric current to minimum, extinguishes electric arc, 5-10 minutes cooling, overturns ingot casting；Above-mentioned melting is repeated several times
Journey, after being cooled to room temperature, blow-on takes out alloy cast ingot to get to 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
Nickel plate in raw material, ingot iron, and the purity of other simple metal raw materials are 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
In the process, coordination electrode stick rotates melting electric arc, electric arc is made fully to sweep 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：It repeats
In fusion process, alloy cast ingot is transferred in clean crucible after melting 3-4 times and carries out smelting operation.
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 minimizes, so that 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 need to being cooled to room temperature, it is filled with air.
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| CN108546834B (en) * | 2018-04-16 | 2020-02-07 | 北京科技大学 | Purification smelting method for nickel-based high-temperature alloy master alloy |
| 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 |
| CN111041255B (en) * | 2019-12-09 | 2021-04-30 | 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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| CN105483411A (en) * | 2015-12-11 | 2016-04-13 | 西北工业大学 | Nickel-based quinary intermediate alloy containing high-melting point components and preparation method thereof |
| CN105543564A (en) * | 2015-12-11 | 2016-05-04 | 西北工业大学 | Nickel-based ternary intermediate alloy containing high-melting-point components and preparation method of nickel-based ternary intermediate alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105483411A (en) * | 2015-12-11 | 2016-04-13 | 西北工业大学 | Nickel-based quinary intermediate alloy containing high-melting point components and preparation method thereof |
| CN105543564A (en) * | 2015-12-11 | 2016-05-04 | 西北工业大学 | Nickel-based ternary intermediate alloy containing high-melting-point components and preparation method of nickel-based ternary intermediate alloy |
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