CN103045875A - Process method for producing 1 ton of I-690 alloy electroslag remelted ingot in industrialized mode - Google Patents

Process method for producing 1 ton of I-690 alloy electroslag remelted ingot in industrialized mode Download PDF

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CN103045875A
CN103045875A CN2012105743209A CN201210574320A CN103045875A CN 103045875 A CN103045875 A CN 103045875A CN 2012105743209 A CN2012105743209 A CN 2012105743209A CN 201210574320 A CN201210574320 A CN 201210574320A CN 103045875 A CN103045875 A CN 103045875A
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slag
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马颖澈
查向东
高明
张龙
刘奎
张顺南
李依依
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Institute of Metal Research of CAS
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Abstract

The invention belongs to the technical field of electroslag remelting, relates to improvement on a process for producing Inconel 690 alloy electroslag remelted ingot in an industrialized mode, in particular to a process method for producing 1 ton of I-690 alloy electroslag remelting ingot in an industrialized mode. A vacuum induction furnace smelts an electrode bar of phi 240 mm; the size of a crystallizer is phi 340/380*1,500 mm; the remelting process parameters comprise: remelting voltage of 47 to 55 V, current of 7,500 to 8,500 A and slag quantity of 38 to 45 kg; according to the I-690 alloy component requirement, the remelting adopts a new proportioned pentabasic slag system; the components comprise calcium fluoride, calcium oxide, aluminum oxide, magnesium oxide and titanium dioxide; the purity of each component is required to be more than 98.5 percent; the total content of unstable oxide impurities such as manganese oxide, ferrous oxide and silica is less than 0.5 percent; the granularity is less than 50 meshes; before the remelting process, the electrode is roasted at the temperature of 700 DEG C for 8 to 12 hours and the slag is roasted at the temperature of 680 DEG C for 8 to 12 hours for use; and in the remelting process, argon and burning gas are adopted for protection. By the process, the content of the remelted I-690 alloy is reduced to be below 20 ppm, the sulfur content is reduced to be below 5 ppm, oxide inclusion is effectively removed, and high-quality remelted alloy is obtained.

Description

The processing method of 1 ton of I-690 alloy of a kind of suitability for industrialized production electric slag refusion ingot
Technical field
The present invention relates to the esr field, be specially 1 ton of I-690 alloy of a kind of suitability for industrialized production electroslag
The processing method of resmelting ingot.
Background technology
Inconel690 (hereinafter to be referred as I-690) alloy is U.S.'s trade mark, and its main component scope is as follows:
Table 1Inconel690 alloy main component scope
Figure BDA00002655343100011
The I-690 alloy is the nickel base superalloy of using on the nuclear steam generator, and it requires to have excellent stress corrosion dehiscence resistant ability, good metallurgical stability and the good characteristics such as processing characteristics.And the impurity elements such as the O that exists in the alloy, S, be the fatal element that affects its performance, S greatly reduces the processing characteristics of alloy, and O is the main forming element of inclusion in the alloy, thereby the content of answering O, S in the reduce alloy reduces the content of inclusion in the alloy, puies forward heavy alloyed performance.The esr of I-690 alloy, used adopts CaF 2: Al 2O 3: CaO:MgO=71:15:9:5 (mass ratio) quaternary slag system; single argon shield mode is adopted in remelting; effect is not very desirable; be difficult to the alloy oxygen level after the remelting is dropped to below the 20ppm; can not satisfy the demand of actual use; therefore, formulate a kind of technique of suitable remelting I-690 alloy, the electroslag remelting process that can reduce O in the alloy, S content seems particularly necessary.
Summary of the invention
The objective of the invention is the composition characteristic for the I-690 alloy; when remelting, selected a kind of fusing point low; basicity is high; five yuan of slag systems of new proportioning; in the reflow process; in the crystallizer bottom; be that the copper sheet top is placed with the pure iron Dummy plate; above the pure iron Dummy plate, put again and the startup board of resmelting electrode with material; by in crystallizer, passing into argon gas; the duplicate protection measure of exit, top combustion gas; remelting atmosphere is controlled; fact proved; adopt the method can produce O content less than 20ppm; S content has improved the high-temp plastic of alloy less than the high quality I-690 alloy remelting ingot of 5ppm, improves the hot workability of alloy.
The present invention specifically provides the processing method of 1 ton of I-690 alloy of a kind of suitability for industrialized production electric slag refusion ingot, adopts vacuum induction furnace to carry out esr, it is characterized in that:
Used slag charge is five yuan of slag systems, and constituent element is Calcium Fluoride (Fluorspan), calcium oxide, aluminum oxide, magnesium oxide and titanium dioxide, and the slag charge proportioning is mass percent: Calcium Fluoride (Fluorspan) 50-55%, calcium oxide 18-22%, aluminum oxide 18-22%, titanium dioxide 1-3%, magnesium oxide surplus;
In reflow process; in the crystallizer bottom; be that Dummy plate is put in the copper sheet top; above Dummy plate, put again and the startup board of resmelting electrode with material; by in crystallizer, passing into the duplicate protection measure of argon gas, exit, crystallizer top combustion gas, remelting atmosphere to be controlled, wherein said Dummy plate is that pure iron is made; startup board is the section of I-690 electrode, and diameter is identical with electrode diameter.
The processing method of 1 ton of I-690 alloy of suitability for industrialized production provided by the invention electric slag refusion ingot is characterized in that: described Dummy plate diameter is than the little 10-15mm of crystallizer lower end diameter of bore, and thickness is 10-12mm; The thickness of startup board is 20-30mm.
The processing method of 1 ton of I-690 alloy of suitability for industrialized production provided by the invention electric slag refusion ingot is characterized in that: described each constituent element purity of five yuan of slag systems〉98.5%, impurity MnO, FeO and SiO 2Total content less than 0.5%, granularity is less than 50 orders.
The processing method of 1 ton of I-690 alloy of suitability for industrialized production provided by the invention electric slag refusion ingot is characterized in that, the concrete technology step is as follows:
1) before the remelting, crystallizer bottom end face and the inner cleaning of crystallizer is clean, and electrode bar is of a size of Φ 240mm, crystallizer specification Φ 340/380 * 1500mm, and electrode bar uses behind 700 ℃ of baking 8-12h;
2) the copper sheet surface finish above the end water tank is clean, remove the upper surface bur;
3) Dummy plate is placed on copper sheet center above the end water tank, get startup board and be placed on the center of Dummy plate, and the solid conduction slag is placed on the startup board, the lifting crystallizer, adjusting the position makes Dummy plate be positioned at the central position of crystallizer, the resmelting electrode rod is fixed on the electrode jaw of electroslag furnace, falls electrode and make its lower side pressure touch Conductive Slag, the argon gas-sealed cover is installed;
4) logical argon gas: pass into argon gas to crystallizer inside, pass into argon gas to the crystallizer bottom first, stop behind 15min ~ 20min, tunger tube is extracted out, continue to pass into argon gas until remelting finishes from crystallizer top;
5) add slag charge: slag charge uses behind 680 ℃ of baking 8-12h, in the disposable adding crystallizer of the slag charge that mixes, after slag charge adds, lights the gas flame circle;
6) change the slag phase: changing time slag phase is 60-70min;
7) melting period: melting period voltage, size of current should guarantee the stable of reflow process and remelting speed, this, voltage was 47-55V in period, electric current 7500A-8500A, remelting speed 4.5-5.5kg/min;
8) the feeding phase: feeding finishes front 25 ~ 30min in remelting and carries out, and reduces power, and the electrode lowering speed that slows down reduces electric current, during the end remelting, stops the electrode that descends, and makes its end melt voluntarily, until electrode has a power failure when exposing the top of the slag and electric arc occuring;
9) remelting finishes, and closes argon gas valve, knock down the flame circle, takes out ESR ingot behind the 1h from crystallizer.
The processing method of 1 ton of I-690 alloy of suitability for industrialized production provided by the invention electric slag refusion ingot is characterized in that: crystallizer bottom argon gas flow velocity is 80-120L/min, and top argon gas flow velocity is 40-50L/min.
The present invention has following advantage:
1, crystallizer bottom has used pure iron Dummy plate and startup board that the copper sheet above the end water tank is protected, both guaranteed striking during the copper sheet surface not damaged, can stop again copper to enter into resmelting ingot as impurity element.
2, utilize argon gas proportion greater than the characteristics of air specific weight; pass into argon gas to the crystallizer bottom; air that can it is inner (particularly oxygen) is discharged; reduced the oxygen partial pressure of slag bath top; protect with burning coal gas in the crystallizer exit simultaneously; can further cut off the source of oxygen, guarantee " pure " of remelting atmosphere.
3, the used slag charge of remelting is five yuan of slag systems of high alkalinity, temperature of fusion lower (1260-1280 ℃), and than low about 130 ℃ of I-690 alloy melting point, this is conducive to the foundation of slag bath and stablizing of Electroslag Process; Highly purified (>98.5%) slag system constituent element and total content<0.5% unstable oxide impurity has reduced the probability that oxygen transmits to metal pool by slag bath.
4, total change slag time is 60-70min, than traditional time lengthening nearly 20min, guaranteed that the fusing of slag charge is complete, simultaneously, adopt relatively low remelting voltage (47-55V) and the electric current of 7500A-8500A, make reflow process very stable.
Embodiment
Embodiment 1
The processing method of 1 ton of I-690 alloy of a kind of suitability for industrialized production electric slag refusion ingot, resmelting electrode is vacuum induction furnace smelting, concrete operation step is as follows:
1) before the remelting, crystallizer bottom end face and the inner cleaning of crystallizer is clean, electrode bar is of a size of Φ 240mm, must not there be serious crackle, pipe, joint flash in its surface, scab and the defective such as slag inclusion, non-scale or iron rust, the grease that the surface adheres to, refractory materials fragment etc. have been removed clean; Crystallizer specification Φ 340/380 * 1500mm, electrode bar uses behind 700 ℃ of baking 10h;
2) with finishing wheel that the surface finish of copper sheet above the end water tank is clean first, the bur above removing;
3) Dummy plate is placed on copper sheet center above the end water tank, get startup board and be placed on the center of Dummy plate, and the solid conduction slag is placed on the startup board, the lifting crystallizer, adjust the position and make Dummy plate be positioned at the central position of crystallizer, from retort furnace, take out consumable electrode, be fixed on the electrode jaw of electroslag furnace, fall electrode and make its lower side pressure touch Conductive Slag, the argon gas-sealed cover is installed;
Wherein, the Dummy plate of employing is that pure iron is made, and diameter is than the little 10mm of crystallizer lower end diameter of bore, and thickness is 10mm; Startup board is the section of I-690 electrode, and diameter is identical with electrode diameter, thickness 25mm; Dry, smooth, bright and clean, non-scale are wanted in Dummy plate and startup board surface, are convenient to the two close contact, and conduction is good;
4) logical argon gas: tunger tube is goed deep into the crystallizer bottom begin to pass into argon gas, passing into the argon gas flow velocity is 100L/min, stop behind the 15min passing into to the bottom, the tunger tube that will stretch to the bottom is extracted out, be placed on crystallizer place suitable for reading, continue to pass into argon gas, the argon gas stream speed that passes into of this moment is adjusted into 50L/min, until remelting finishes;
5) add slag charge: the slag charge proportioning of employing is (mass percent): Calcium Fluoride (Fluorspan) 50%, calcium oxide 22%, aluminum oxide 19%, titanium oxide 2%, clout are MgO.Each constituent element purity>98.5% of slag system, unstable oxide oxidation of impurities manganese (MnO), iron protoxide (FeO), silicon-dioxide (SiO 2) total content is less than 0.5%, granularity is less than 50 orders.Slag charge uses behind 680 ℃ of baking 10h, in the disposable adding crystallizer of the slag charge that mixes, after slag charge adds, lights the gas flame circle;
6) change the slag phase: changing time slag phase is 65min;
7) melting period: melting period voltage 50V, electric current 8000A; The remelting rate-controlling is at 4.8kg/min;
8) the feeding phase: feeding 30min before remelting finishes carries out, and reduces gradually power, and the electrode lowering speed that slows down reduces electric current, during the end remelting, stops the electrode that descends, and makes its end melt voluntarily, until electrode has a power failure when exposing the top of the slag and electric arc occuring;
9) remelting finishes, and closes argon gas valve, coal gas, and the knock down the flame circle takes out ESR ingot from crystallizer behind the 1h.I-690 alloy composition analytical data sees Table 2 after the remelting.
Embodiment 2
Be with the difference of embodiment 1:
1) the slag charge proportioning that adopts is (mass percent): Calcium Fluoride (Fluorspan) 52%, calcium oxide 22%, aluminum oxide 20%, titanium dioxide 3%, clout are MgO.Each constituent element purity>98.5% of slag system, unstable oxide oxidation of impurities manganese (MnO), iron protoxide (FeO), silicon-dioxide (SiO 2) total content is less than 0.5%, granularity is less than 50 orders.Slag charge uses behind 680 ℃ of baking 10h, in the disposable adding crystallizer of the slag charge that mixes, after slag charge adds, lights the gas flame circle;
2) Dummy plate that adopts is that pure iron is made, and diameter is than the little 15mm of crystallizer lower end diameter of bore, and thickness is 12mm; Startup board is the section of I-690 electrode, and diameter is identical with electrode diameter, thickness 30mm;
3) crystallizer bottom argon gas flow velocity is 80L/min, and top argon gas flow velocity is 40/min.
I-690 alloy composition analytical data sees Table 2 after the remelting.
Embodiment 3
Be with the difference of embodiment 1:
1) the slag charge proportioning that adopts is (mass percent): Calcium Fluoride (Fluorspan) 55%, calcium oxide 18%, aluminum oxide 20%, titanium dioxide 3%, clout are MgO.Each constituent element purity>98.5% of slag system, unstable oxide oxidation of impurities manganese (MnO), iron protoxide (FeO), silicon-dioxide (SiO 2) total content is less than 0.5%, granularity is less than 50 orders.Slag charge uses behind 680 ℃ of baking 10h, in the disposable adding crystallizer of the slag charge that mixes, after slag charge adds, lights the gas flame circle;
2) startup board is the section of I-690 electrode, and diameter is identical with electrode diameter, thickness 30mm;
3) crystallizer bottom argon gas flow velocity is 90L/min, and top argon gas flow velocity is 50L/min.
I-690 alloy composition analytical data sees Table 2 after the remelting.
Comparative Examples 1
Be with the difference of embodiment 1: the remelting slag system proportioning (mass ratio) that adopts is CaF 2: Al 2O 3: CaO:MgO=71:15:9:5.I-690 alloy composition analytical data sees Table 2 after the remelting.
Comparative Examples 2
Be with the difference of Comparative Examples 1: do not adopt protective atmosphere.I-690 alloy composition analytical data sees Table 3 after the remelting.
Under table 2 protective atmosphere, indivedual Trace Elements (wt%) of the I-690 alloy of different slag system remeltings
Element O S N Al Ti
Resmelting electrode 0.0006 0.0005 0.0051 0.21 0.20
Comparative Examples 1 0.0033 0.0005 0.0057 0.16 0.25
Embodiment 1 0.0014 <0.0005 0.0058 0.20 0.15
Embodiment 2 0.0015 0.0005 0.0050 0.19 0.15
Embodiment 3 0.0014 <0.0005 0.0057 0.21 0.16
Table 3 has-unprotect atmosphere under the indivedual Trace Elements of Inconel690 alloy (wt%) of remelting
Figure BDA00002655343100081
By table 2 data as can be known, behind the employing protective atmosphere, use the I-690 ALLOY O content of slag system remelting of the present invention to hang down about 20ppm than the alloy that uses traditional slag system remelting.By table 3 data as can be known, the remelting slag system is identical, adopts I-690 ALLOY O content after the protective atmosphere remelting than not adopting the alloy oxygen level after the protective atmosphere remelting to hang down about 10ppm.As seen, under protective atmosphere, can effectively fall low-alloyed oxygenation after having used new remelting slag system, greatly improve the purity of alloy.
Above-described embodiment only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the personage who is familiar with technique can understand content of the present invention and according to this enforcement, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.

Claims (5)

1. the processing method of 1 ton of I-690 alloy of suitability for industrialized production electric slag refusion ingot adopts vacuum induction furnace to carry out esr, it is characterized in that:
Used slag charge is five yuan of slag systems, and constituent element is Calcium Fluoride (Fluorspan), calcium oxide, aluminum oxide, magnesium oxide and titanium dioxide, and the slag charge proportioning is mass percent: Calcium Fluoride (Fluorspan) 50-55%, calcium oxide 18-22%, aluminum oxide 18-22%, titanium dioxide 1-3%, magnesium oxide surplus;
In reflow process; in the crystallizer bottom; be that Dummy plate is put in the copper sheet top; above Dummy plate, put again and the startup board of resmelting electrode with material; by in crystallizer, passing into the duplicate protection measure of argon gas, exit, crystallizer top combustion gas, remelting atmosphere to be controlled, wherein said Dummy plate is that pure iron is made; startup board is the section of I-690 electrode, and diameter is identical with electrode diameter.
2. according to the processing method of 1 ton of I-690 alloy of the described suitability for industrialized production of claim 1 electric slag refusion ingot, it is characterized in that: described Dummy plate diameter is than the little 10-15mm of crystallizer lower end diameter of bore, and thickness is 10-12mm; The thickness of startup board is 20-30mm.
3. according to the processing method of 1 ton of I-690 alloy of the described suitability for industrialized production of claim 1 electric slag refusion ingot, it is characterized in that: described each constituent element purity of five yuan of slag systems 98.5%, impurity MnO, FeO and SiO 2Total content less than 0.5%, granularity is less than 50 orders.
4. according to the processing method of 1 ton of I-690 alloy of the described suitability for industrialized production of claim 1 ~ 3 electric slag refusion ingot, it is characterized in that, the concrete technology step is as follows:
1) before the remelting, crystallizer bottom end face and the inner cleaning of crystallizer is clean, and electrode bar is of a size of Φ 240mm, crystallizer specification Φ 340/380 * 1500mm, and electrode bar uses behind 700 ℃ of baking 8-12h;
2) the copper sheet surface finish above the end water tank is clean, remove the upper surface bur;
3) Dummy plate is placed on copper sheet center above the end water tank, get startup board and be placed on the center of Dummy plate, and the solid conduction slag is placed on the startup board, the lifting crystallizer, adjusting the position makes Dummy plate be positioned at the central position of crystallizer, the resmelting electrode rod is fixed on the electrode jaw of electroslag furnace, falls electrode and make its lower side pressure touch Conductive Slag, the argon gas-sealed cover is installed;
4) logical argon gas: pass into argon gas to crystallizer inside, pass into argon gas to the crystallizer bottom first, stop behind 15min ~ 20min, tunger tube is extracted out, continue to pass into argon gas until remelting finishes from crystallizer top;
5) add slag charge: slag charge uses behind 680 ℃ of baking 8-12h, in the disposable adding crystallizer of the slag charge that mixes, after slag charge adds, lights the gas flame circle;
6) change the slag phase: changing time slag phase is 60-70min;
7) melting period: melting period voltage be 47-55V, electric current 7500A-8500A, remelting speed 4.5-5.5kg/min;
8) the feeding phase: feeding finishes front 25 ~ 30min in remelting and carries out, and reduces power, and the electrode lowering speed that slows down reduces electric current, during the end remelting, stops the electrode that descends, and makes its end melt voluntarily, until electrode has a power failure when exposing the top of the slag and electric arc occuring;
9) remelting finishes, and closes argon gas valve, knock down the flame circle, takes out ESR ingot behind the 1h from crystallizer.
5. according to the processing method of 1 ton of I-690 alloy of the described suitability for industrialized production of claim 4 electric slag refusion ingot, it is characterized in that: crystallizer bottom argon gas flow velocity is 80-120L/min, and top argon gas flow velocity is 40-50L/min.
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CN104674144A (en) * 2015-02-28 2015-06-03 钢铁研究总院 Heat treatment method of large-size, high-strength and fine-grain nickel-based superalloy forge piece for nuclear reactor
CN105861847A (en) * 2016-04-19 2016-08-17 四川六合锻造股份有限公司 Quinary electroslag remelting system and production method applying quinary electroslag remelting system to 3379B blade steel material
CN106756077A (en) * 2016-10-20 2017-05-31 深圳市万泽中南研究院有限公司 A kind of high temperature alloy electroslag remelting slag system and its application method
CN108660320A (en) * 2018-06-20 2018-10-16 张家港广大特材股份有限公司 A kind of low-aluminium high titanium-type high temperature alloy electroslag remelting process
CN108728662A (en) * 2018-06-14 2018-11-02 湖州久立永兴特种合金材料有限公司 A kind of N06625 nickel-base alloys electro-slag re-melting method and the slag system used
CN110846515A (en) * 2019-11-21 2020-02-28 重庆材料研究院有限公司 Preparation method of nickel-based alloy 690 with ultralow gas content
CN111069574A (en) * 2019-12-21 2020-04-28 江苏骏茂新材料科技有限公司 Preparation method of wide-width fine-grain nickel-based alloy plate
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CN114540633A (en) * 2020-11-26 2022-05-27 中国科学院金属研究所 Control method for carbon hydrogen content of 1 ton iron-nickel-based high-temperature alloy electroslag remelting ingot produced industrially
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CN104674144A (en) * 2015-02-28 2015-06-03 钢铁研究总院 Heat treatment method of large-size, high-strength and fine-grain nickel-based superalloy forge piece for nuclear reactor
CN105861847A (en) * 2016-04-19 2016-08-17 四川六合锻造股份有限公司 Quinary electroslag remelting system and production method applying quinary electroslag remelting system to 3379B blade steel material
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CN108728662B (en) * 2018-06-14 2020-02-18 湖州久立永兴特种合金材料有限公司 Electroslag remelting method for N06625 nickel-based alloy and slag system used by electroslag remelting method
CN108728662A (en) * 2018-06-14 2018-11-02 湖州久立永兴特种合金材料有限公司 A kind of N06625 nickel-base alloys electro-slag re-melting method and the slag system used
CN108660320A (en) * 2018-06-20 2018-10-16 张家港广大特材股份有限公司 A kind of low-aluminium high titanium-type high temperature alloy electroslag remelting process
CN110846515A (en) * 2019-11-21 2020-02-28 重庆材料研究院有限公司 Preparation method of nickel-based alloy 690 with ultralow gas content
CN111069574A (en) * 2019-12-21 2020-04-28 江苏骏茂新材料科技有限公司 Preparation method of wide-width fine-grain nickel-based alloy plate
CN114540633A (en) * 2020-11-26 2022-05-27 中国科学院金属研究所 Control method for carbon hydrogen content of 1 ton iron-nickel-based high-temperature alloy electroslag remelting ingot produced industrially
CN114540633B (en) * 2020-11-26 2024-04-12 中国科学院金属研究所 Control method for carbon and hydrogen content of electroslag remelting ingot for industrial production of 1 ton iron-nickel-based superalloy
CN113637860A (en) * 2021-08-13 2021-11-12 江苏隆达超合金航材有限公司 Preparation process of GH690 alloy
CN115198126A (en) * 2022-07-12 2022-10-18 中国科学院金属研究所 Method for controlling carbon content of head of 1-ton nickel-based wrought superalloy electroslag remelting ingot in industrial production

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