CN103045875B - 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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CN103045875B
CN103045875B CN201210574320.9A CN201210574320A CN103045875B CN 103045875 B CN103045875 B CN 103045875B CN 201210574320 A CN201210574320 A CN 201210574320A CN 103045875 B CN103045875 B CN 103045875B
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slag
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remelting
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alloy
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CN103045875A (en
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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 electric slag refusion ingot of a kind of suitability for industrialized production
Technical field
The present invention relates to esr field, be specially 1 ton of I-690 alloy electroslag of a kind of suitability for industrialized production
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
I-690 alloy is the nickel base superalloy of using on nuclear steam generator, and it requires to have excellent stress corrosion dehiscence resistant ability, the features such as good metallurgical stability and good processing characteristics.And the impurity element such as O, S existing in alloy, 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 alloy, thereby the content that should as far as possible reduce O in alloy, S reduces the content of inclusion in 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; remelting adopts single argon shield mode; effect is not very desirable; be difficult to the alloy oxygen level after remelting to drop to below 20ppm; can not meet the demand of actual use; therefore, formulate a kind of technique of applicable remelting I-690 alloy, the electroslag remelting process that can reduce O in alloy, S content seems particularly necessary.
Summary of the invention
The object of the invention is the composition characteristic for I-690 alloy, in the time of remelting, select a kind of fusing point low, basicity is high, five yuan of slag systems of new proportioning, in reflow process, in crystallizer bottom, be that copper sheet top is placed with pure iron Dummy plate, above pure iron Dummy plate, put again and the startup board of resmelting electrode with material, by pass into argon gas in crystallizer, the duplicate protection measure of exit, top combustion gas, remelting atmosphere is controlled, fact proved, adopt the method can produce O content and be less than 20ppm, S content is less than the high quality I-690 alloy remelting ingot of 5ppm, improve the high-temp plastic of alloy, improve the hot workability of alloy.
The present invention specifically provides the processing method of 1 ton of I-690 alloy electric slag refusion ingot of a kind of suitability for industrialized production, adopts vacuum induction furnace to carry out esr, it is characterized in that:
Slag charge used is five yuan of slag systems, and constituent element is Calcium Fluoride (Fluorspan), calcium oxide, aluminum oxide, magnesium oxide and titanium dioxide, and 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 crystallizer bottom; be that Dummy plate is put in copper sheet top; above Dummy plate, put again and the startup board of resmelting electrode with material; by pass into the duplicate protection measure of argon gas, exit, crystallizer top combustion gas in crystallizer, 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 electric slag refusion ingot of suitability for industrialized production provided by the invention, 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 electric slag refusion ingot of suitability for industrialized production provided by the invention, is characterized in that: the described five yuan of each constituent element purity of slag system >98.5%, impurity MnO, FeO and SiO 2total content be less than 0.5%, granularity is less than 50 orders.
The processing method of 1 ton of I-690 alloy electric slag refusion ingot of suitability for industrialized production provided by the invention, is characterized in that, concrete technology step is as follows:
1), before remelting, by clean to crystallizer bottom end face and the inner cleaning of crystallizer, electrode bar is of a size of Φ 240mm, crystallizer specification Φ 340/380 × 1500mm, and electrode bar uses after 700 DEG C of baking 8-12h;
2), by clean the copper sheet surface finish above end water tank, remove upper surface bur;
3) Dummy plate is placed on to the copper sheet center above end water tank, get startup board and be placed on the center of Dummy plate, and solid conduction slag is placed in startup board, lifting crystallizer, adjusting position makes Dummy plate be positioned at the central position of crystallizer, resmelting electrode rod is fixed on the electrode jaw of electroslag furnace, falls electrode and make its lower side pressure touch Conductive Slag, argon gas-sealed cover is installed;
4) logical argon gas: pass into argon gas to crystallizer inside, first pass into argon gas to crystallizer bottom, stop after 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 after 680 DEG C of baking 8-12h, adds in crystallizer disposable the slag charge mixing, and after slag charge adds, lights 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 ensure 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 25 ~ 30min before remelting finishes carries out, and reduces power, and the electrode lowering speed that slows down, reduces electric current, finishes when remelting, to stop the electrode that declines, and makes its end melt voluntarily, until electrode has a power failure when exposing the top of the slag and electric arc occurring;
9) remelting finishes, and closes argon gas valve, knock down the flame circle, takes out ESR ingot after 1h from crystallizer.
The processing method of 1 ton of I-690 alloy electric slag refusion ingot of suitability for industrialized production provided by the invention, is characterized in that: crystallizer bottom argon gas flow velocity is 80-120L/min, and top argon gas flow velocity is 40-50L/min.
Tool of the present invention has the following advantages:
1, crystallizer bottom, has been used pure iron Dummy plate and startup board to be protected the copper sheet above end water tank, both ensured striking during copper sheet surface not damaged, can stop again copper to enter into resmelting ingot as impurity element.
2, utilize argon gas proportion to be greater than the feature of air specific weight; pass into argon gas to crystallizer bottom; its inner air (particularly oxygen) can be discharged; reduce the oxygen partial pressure of slag bath top; protect with burning coal gas in crystallizer exit simultaneously; can further cut off the source of oxygen, ensure " pure " of remelting atmosphere.
3, five yuan of slag systems that remelting slag charge used is high alkalinity, temperature of fusion lower (1260-1280 DEG C), than the low 130 DEG C of left and right 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, 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, ensured that the fusing of slag charge is complete, meanwhile, adopt relatively low remelting voltage (47-55V) and the electric current of 7500A-8500A, make reflow process very stable.
Embodiment
Embodiment 1
A processing method for 1 ton of I-690 alloy electric slag refusion ingot of suitability for industrialized production, resmelting electrode is vacuum induction furnace smelting, concrete operation step is as follows:
1) before remelting, by clean to crystallizer bottom end face and the inner cleaning of crystallizer, electrode bar is of a size of Φ 240mm, must not there be serious crackle, pipe, joint flash in its surface, scab and the defect such as slag inclusion, non-scale or iron rust, grease, refractory materials fragment etc. that surface adheres to have been removed totally; Crystallizer specification Φ 340/380 × 1500mm, electrode bar uses after 700 DEG C of baking 10h;
2) first with finishing wheel by clean the surface finish of copper sheet above end water tank, remove bur above;
3) Dummy plate is placed on to the copper sheet center above end water tank, get startup board and be placed on the center of Dummy plate, and solid conduction slag is placed in startup board, lifting crystallizer, adjust 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, 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; Dummy plate and startup board surface will be dried, smooth, bright and clean, non-scale, are convenient to the two close contact, and conduction is good;
4) logical argon gas: tunger tube is goed deep into crystallizer bottom and start to pass into argon gas, passing into argon gas flow velocity is 100L/min, after 15min, stop passing into bottom, the tunger tube that stretches to 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 is now 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.The each constituent element purity of slag system > 98.5%, 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 after 680 DEG C of baking 10h, adds in crystallizer disposable the slag charge mixing, and after slag charge adds, lights gas flame circle;
6) change the slag phase: changing time slag phase is 65min;
7) melting period: melting period voltage 50V, electric current 8000A; 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, finishes when remelting, to stop the electrode that declines, and makes its end melt voluntarily, until electrode has a power failure when exposing the top of the slag and electric arc occurring;
9) remelting finishes, and closes argon gas valve, coal gas, and knock down the flame circle takes out ESR ingot from crystallizer after 1h.After remelting, I-690 alloy composition analytical data is in table 2.
Embodiment 2
Be with the difference of embodiment 1:
1) the slag charge proportioning adopting is (mass percent): Calcium Fluoride (Fluorspan) 52%, calcium oxide 22%, aluminum oxide 20%, titanium dioxide 3%, clout are MgO.The each constituent element purity of slag system > 98.5%, 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 after 680 DEG C of baking 10h, adds in crystallizer disposable the slag charge mixing, and after slag charge adds, lights gas flame circle;
2) Dummy plate adopting 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.
After remelting, I-690 alloy composition analytical data is in table 2.
Embodiment 3
Be with the difference of embodiment 1:
1) the slag charge proportioning adopting is (mass percent): Calcium Fluoride (Fluorspan) 55%, calcium oxide 18%, aluminum oxide 20%, titanium dioxide 3%, clout are MgO.The each constituent element purity of slag system > 98.5%, 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 after 680 DEG C of baking 10h, adds in crystallizer disposable the slag charge mixing, and after slag charge adds, lights 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.
After remelting, I-690 alloy composition analytical data is in table 2.
Comparative example 1
Be with the difference of embodiment 1: the remelting slag system proportioning (mass ratio) adopting is CaF 2: Al 2o 3: CaO:MgO=71:15:9:5.After remelting, I-690 alloy composition analytical data is in table 2.
Comparative example 2
Be with the difference of comparative example 1: do not adopt protective atmosphere.After remelting, I-690 alloy composition analytical data is in table 3.
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 example 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
The indivedual Trace Elements of Inconel690 alloy (wt%) of remelting under have-unprotect of table 3 atmosphere
From table 2 data, adopt after protective atmosphere, use the I-690 ALLOY O content of slag system remelting of the present invention than the low 20ppm of the alloy that uses traditional slag system remelting left and right.From table 3 data, remelting slag system is identical, and the I-690 ALLOY O content after the remelting of employing protective atmosphere is than the low 10ppm of the alloy oxygen level left and right not adopting after protective atmosphere remelting.Visible, under protective atmosphere, low-alloyed oxygenation can effectively be fallen after having used new remelting slag system, greatly improve the purity of alloy.
Above-described embodiment is only explanation technical conceive of the present invention and feature, and its object is to allow person skilled in the art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences that spirit is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.

Claims (4)

1. a processing method for 1 ton of I-690 alloy electric slag refusion ingot of suitability for industrialized production, adopts vacuum induction furnace to carry out esr, it is characterized in that:
Slag charge used is five yuan of slag systems, and constituent element is Calcium Fluoride (Fluorspan), calcium oxide, aluminum oxide, magnesium oxide and titanium dioxide, and 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 crystallizer bottom, be that Dummy plate is put in copper sheet top, above Dummy plate, put again and the startup board of resmelting electrode with material, by pass into the duplicate protection measure of argon gas, exit, crystallizer top combustion gas in crystallizer, 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; Crystallizer bottom argon gas flow velocity is 80-120L/min, and top argon gas flow velocity is 40-50L/min.
2. according to the processing method of 1 ton of I-690 alloy electric slag refusion ingot of suitability for industrialized production described in claim 1, 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 electric slag refusion ingot of suitability for industrialized production described in claim 1, it is characterized in that: the described five yuan of each constituent element purity of slag system >98.5%, impurity MnO, FeO and SiO 2total content be less than 0.5%, granularity is less than 50 orders.
4. according to the processing method of 1 ton of I-690 alloy electric slag refusion ingot of suitability for industrialized production described in claim 1~3, it is characterized in that, concrete technology step is as follows:
1), before remelting, by clean to crystallizer bottom end face and the inner cleaning of crystallizer, electrode bar is of a size of Φ 240mm, crystallizer specification Φ 340/380 × 1500mm, and electrode bar uses after 700 DEG C of baking 8-12h;
2), by clean the copper sheet surface finish above end water tank, remove upper surface bur;
3) Dummy plate is placed on to the copper sheet center above end water tank, get startup board and be placed on the center of Dummy plate, and solid conduction slag is placed in startup board, lifting crystallizer, adjusting position makes Dummy plate be positioned at the central position of crystallizer, resmelting electrode rod is fixed on the electrode jaw of electroslag furnace, falls electrode and make its lower side pressure touch Conductive Slag, argon gas-sealed cover is installed;
4) logical argon gas: pass into argon gas to crystallizer inside, first pass into argon gas to crystallizer bottom, stop after 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 after 680 DEG C of baking 8-12h, adds in crystallizer disposable the slag charge mixing, and after slag charge adds, lights 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 25~30min before remelting finishes carries out, and reduces power, and the electrode lowering speed that slows down, reduces electric current, finishes when remelting, to stop the electrode that declines, and makes its end melt voluntarily, until electrode has a power failure when exposing the top of the slag and electric arc occurring;
9) remelting finishes, and closes argon gas valve, knock down the flame circle, takes out ESR ingot after 1h from crystallizer.
CN201210574320.9A 2012-12-26 2012-12-26 Process method for producing 1 ton of I-690 alloy electroslag remelted ingot in industrialized mode Active CN103045875B (en)

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