CN110408803A - A kind of sublimate method of smelting for nickel base superalloy master alloy - Google Patents
A kind of sublimate method of smelting for nickel base superalloy master alloy Download PDFInfo
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- CN110408803A CN110408803A CN201910699655.5A CN201910699655A CN110408803A CN 110408803 A CN110408803 A CN 110408803A CN 201910699655 A CN201910699655 A CN 201910699655A CN 110408803 A CN110408803 A CN 110408803A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- 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
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Abstract
The present invention relates to a kind of sublimate method of smelting of alloy more particularly to a kind of sublimate method of smelting for nickel base superalloy master alloy, belong to Metal Melting technical field.The present invention is melted by cloth and alloy, initial refining, alloying and double refining, and the sublimate melting of master alloy is completed in microalloying control, casting.This method can effectively improve the degree of purity of vacuum melting, improve element segregation, the nickel base superalloy prepared using the technology of the present invention, degree of purity height and segregation are low, quality is significantly higher than the prior art and method, improves nickel base superalloy quality, extends application field.Using the different brackets of the technology of the present invention melting and the nickel base superalloy of the trade mark, good result is achieved.Use the type of furnace for 250kg grades and 1.5 tonnes of vaccum sensitive stoves.With before melting and compared with other technologies method, the degree of purity and uniformity of alloy are significantly improved.
Description
Technical field
The present invention relates to a kind of sublimate method of smelting of alloy, more particularly to one kind to be used for nickel base superalloy master alloy
Sublimate method of smelting, belong to Metal Melting technical field.
Background technique
Mechanical property, craftsmanship of the objectionable impurities elements such as oxygen, nitrogen, sulphur to metal material, especially nickel base superalloy
The performances such as energy and high-temperature oxidation resistant corrosion generate extremely severe adverse effect.Therefore, how to reduce in nickel base superalloy
Objectionable impurities elements content be always nickel base superalloy melting technique research and development emphasis direction.In nickel base superalloy,
The oxide and nitride inclusion that oxygen, nitrogen and other alloying elements are formed can become crack initiation original and Quick Extended channel, sternly
The cores mechanical properties such as lasting, creep and fatigue are reduced again.And the sulphur in nickel base superalloy drastically reduces the solderable of alloy
Property, while damaging the high-temperature oxidation resistant of alloy, corrosion resistance etc..Applicant passes through one Chinese invention patent Shen of retrieval discovery
Please a kind of 201810338616.8 nickel base superalloy master alloy sublimate method of smelting, disclose molten using vacuum suspension technology
The method of nickel metallurgy based high-temperature alloy, the alloy melt which is generated by electromagnetic induction suspends, alkalinity CeO-CeF2Slag and
Water jacketed copper crucible combines, and can be only achieved purpose described in the invention.But in vacuum suspension technology fusion process, by electromagnetic force
Limitation, in large-tonnage (250kg or more) equipment, hardly possible forms ideal suspension effect, cannot generate good sublimate effect,
To limit application of the technology in nickel base superalloy industrialization.Therefore, in nickel base superalloy field, though the technology
With technological value, but its social economic value is relatively low.Another 201810810928.4 nickel of Chinese invention patent application
The sublimate method of smelting of base directional solidification cylindrulite, single crystal super alloy master alloy.But the technology has former, auxiliary material higher
Quality requirements not only increase original during the technical application, subsidiary materials cost, and increase control process, improve
Potential economic risk, to limit its application.
Summary of the invention
The purpose of the present invention is being directed to the deficiencies of of the existing technology at high cost, application range is narrow, propose that one kind is used for
The vacuum induction sublimate melting technique of nickel base superalloy master alloy.The technology, which is put forth effort on, develops skill itself, to greatest extent
The removal of impurities that ground plays vacuum induction melting is horizontal, reduces objectionable impurities elements content in nickel base superalloy, improves product quality.
The present invention solves technical problem by the following technical programs: a kind of sublimate for nickel base superalloy master alloy
Method of smelting, comprising the following steps:
Step 1: cloth and alloy melt, raw material is surface-treated, in crucible according in molten alloy ingredient with
The sequence of lower element Ni, Fe, Co, Cr, Mo, C, Nb, Ta, W, Ni successively cloth from bottom to up, as vacuum degree < 8Pa, and Pressure Rise Rate
When≤8Pa/min, start power transmission fusing, after bottom material dissolves, raw material of the addition containing Re, Ru ingredient is to melting down;
Step 2: initial refining controls melt temperature after the raw material of step 1 is melting down, carry out the low-temperature refining stage, essence
It during refining, is stirred, periodic detection vacuum degree and Pressure Rise Rate, as vacuum degree≤2Pa, and Pressure Rise Rate≤2Pa/ twice in succession
When min, one time low-temperature refining is completed, then quickly increases melt temperature, carries out a high temperature refinery, while carrying out electromagnetic agitation,
Stirring frequency is 330-360Hz, after continuing 15-25min, completes initial refining processing;
Step 3: alloying and double refining, after the completion of initial refining, power failure is cooled to raw material and is in fast conjunctiva state,
Easy oxygen/nitridation element ti, Al is added by smelting component, stirs 15-30 minutes, after melting down, melt temperature is increased, into secondary height
Warm refining stage after continuing 15-30 minutes, completes secondary high-temperature refining;Temperature is reduced to add into the secondary low-temperature refining stage
Enter Ce, Mg element, persistently stir 10-20 minutes, as vacuum degree≤5Pa, and twice in succession Pressure Rise Rate≤5Pa/min when, for the first time
Stokehold sampling analysis, when each element content meets the requirements, double refining terminates;
Step 4: microalloying controls, after double refining, Hf, B, Zr element is added, stirring is stirred 10-20 minutes,
Second of stokehold sampling analysis after melting down, when meeting alloying component, microalloying terminates;
Step 5: being poured, after microalloying, melt temperature is reduced to 1450-1470 DEG C, Y, Ce, Mg is added after filling Ar gas
Element, after stirring 5-15 minutes, adjustment temperature completes the sublimate melting of master alloy to 1520-1550 DEG C of casting.
In the step 1 of the above method, raw material are handled, and make its clean surface, are presented metallic luster, and
100 DEG C drying 20 hours.
1520-1570 DEG C of temperature of low-temperature refining stage control in the step 2 carries out electromagnetic agitation, frequency 280-
310Hz, as vacuum degree≤2Pa, and twice in succession Pressure Rise Rate≤2Pa/min when, low-temperature refining is completed;It is rapidly heated supreme
Warm refining stage simultaneously controls 1640-1660 DEG C of temperature, as vacuum degree≤1.3Pa, and Pressure Rise Rate≤1.3Pa/min twice in succession
When, one time high temperature refinery is completed.
Secondary high-temperature refining stage in the step 3 increases temperature to 1570-1620 DEG C, carries out electromagnetic agitation, frequency
For 360-390Hz, after continuing 15-30 minutes, temperature is reduced to 1470-1520 DEG C into the secondary low-temperature refining stage, Ce is added
With Mg element (Ce and Mg total content≤0.1wt.% of addition, and Ce/Mg≤2:8), electromagnetic agitation 10-20 minutes, frequency was
310-340Hz.As vacuum degree≤5Pa, and twice in succession Pressure Rise Rate≤5Pa/min when, double refining complete.
In the step 5, melt temperature is reduced to 1450-1470 DEG C, Y, Ce, Mg is added, wherein the Ce and Mg of addition
Total content≤0.1wt.%, and Mg/Ce≤3:7, after stirring 5-15 minutes, adjustment temperature to 1520-1550 DEG C of completion is poured.
Vacuum induction melting is the key core process of nickel base superalloy master alloy preparation, to objectionable impurities member in alloy
Element control has a major impact, and is the critical process for controlling objectionable impurities content.It is eliminated as much as by vacuum induction melting Ni-based
Objectionable impurities elements in high temperature alloy have meaning of crucial importance for improving nickel base superalloy quality.Method of the invention
Pass through: 1) bottom material fusing time is appropriately extended, improves degasifying effect;2) low-temperature refining early period (low-temperature refining) promotes bottom
Expect depth deoxidation, takes into account removal free state nitrogen;3) high temperature refinery (high temperature refinery) promotes nitride and nonmetallic in bottom material
It is mingled with decomposition, removes nonmetal inclusion and chemical combination states of matter nitrogen;4) plus Ti, Al after high temperature refinery (secondary high-temperature refining), promotion nitrogen
Compound is decomposed, and nitrogen content in Ti, Al is reduced;5) it adds Ce and Mg and carries out secondary low-temperature refining, carry out major ingredient mixing deoxidation, denitrogenation
And first desulfurization;And suitable Ce/Mg ratio reduces response intensity, improves control stability;6) casting before addition Ce and
Mg carries out final deoxidizing, denitrogenation and desulfurization;7) refining process use different scientific judgment basis, be effectively reduced gas in melt,
While significantly improving alloy degree of purity, easy scaling loss element is effectively reduced in the objectionable impurities contents such as non-(class) metal inclusion
The proportion of goods damageds;8) electromagnetic agitating technology of different frequency accelerates elemental gas diffusion in melt, increases melt degassing surface
Product, not only increases degassing and dust removal rate;And the element segregation in melt is significantly improved, significantly improve the uniform of alloy
Property.The beneficial effects of the present invention are: this method can effectively improve the degree of purity of vacuum melting, improve element segregation, using this hair
The nickel base superalloy of bright technology preparation, degree of purity height and segregation are low, and quality is significantly higher than the prior art and method, improves nickel
Based high-temperature alloy quality, extends application field.It is closed using the different brackets of the technology of the present invention melting and the nickel-base high-temperature of the trade mark
Gold achieves good result.Use the type of furnace for 250kg grades and 1.5 tonnes of vaccum sensitive stoves.With before melting and other technologies side
Method is compared, and the degree of purity and uniformity of alloy are significantly improved.
Specific embodiment
Following embodiment one and embodiment two are all made of 250kg grades of vaccum sensitive stoves and carry out sublimate melting;Embodiment
Three, using 1.5 tons of vaccum sensitive stove sublimate meltings.
Embodiment one
Second generation nickel-base high-temperature single crystal alloy Ren é N5 is prepared according to the following steps in the present embodiment:
Step 1, cloth and alloy melting:
Raw material carry out relevant treatment, make its clean surface, metallic luster are presented, and 20 hours dry at 100 DEG C.It presses
Ren é N5 single crystal alloy ingredient, in crucible according to 30%Ni, 100%Co, 100%Cr, 100%Mo, 30%C, 100%Ta,
100%W, 30%Ni raw material sequence successively cloth from bottom to up.
As Pressure Rise Rate < 0.13Pa/min, and when vacuum degree < 1.3Pa, start power transmission fusing.Initial stage, using ladder-like power
In fusion process, residue Ni and C is added in lift mode (frequency 30-50kW/10min, until rated power melt).The bottom of to
After material dissolves, add Re to melting down.Entire fusion process time-consuming about 70-90min.
Step 2, initial refining is handled:
After bottom material is melting down, 1540 ± 10 DEG C of temperature control, the low-temperature refining stage is carried out, during which, electromagnetic agitation frequency is 280-
290Hz, periodic detection vacuum, temperature and Pressure Rise Rate.As vacuum degree≤1.3Pa, and Pressure Rise Rate≤1.3Pa/ twice in succession
When min, low-temperature refining is completed.It is rapidly heated to 1650 ± 10 DEG C, carries out high temperature refinery, during which, electromagnetic agitation frequency is 350-
360Hz after continuing 15-20min, completes initial refining processing.
Step 3, alloying and double refining:
Power failure is cooled to fast conjunctiva, after adding Ti to stir 2min, Al is added to stir 3-5min to melting down.It is warming up to 1590 ± 10
DEG C, high temperature refinery is carried out, after electromagnetic agitation 15-20 minutes, 1480 ± 10 DEG C is cooled to, Ce and Mg, 310-320Hz electromagnetism is added
Stirring, as vacuum degree≤5Pa, and Pressure Rise Rate≤5Pa/min twice in succession, and when the sampling analysis qualification of stokehold, complete secondary fine
Refining.
Step 4, microalloying controls
After double refining, Hf, B is added, 12-15min is to melting down for stirring.After stokehold sampling analysis is qualified again, microalloy
Changing control terminates.
Step 5, it is poured:
After microalloying, Ar to 10-12kPa is filled, after adding Y, Mg and Ce element to stir 5-6min, adjustment temperature to 1540 ±
10 DEG C of casting.
Embodiment two
Orientation nickel base superalloy DZ125 is prepared according to the following steps in the present embodiment:
Step 1, cloth and alloy melting:
Raw material carry out relevant treatment, make its clean surface, metallic luster are presented, and 20 hours dry at 100 DEG C.It presses
DZ125 directionally solidified alloy ingredient, in crucible according to 30%Ni, 100%Co, 100%Cr, 100%Mo, 35%C, 100%Ta,
100%W, 30%Ni raw material sequence successively cloth from bottom to up.
As Pressure Rise Rate < 0.13pa/min, and when vacuum degree < 2pa, start power transmission fusing.Initial stage, using ladder-like power liter
In fusion process, residue Ni and C is added in height mode (frequency 30-50kW/10min, until rated power melt).It is entire molten
Change process time-consuming about 110-130min.
Step 2, initial refining is handled:
After bottom material is melting down, 1560 ± 10 DEG C of temperature control, the low-temperature refining stage is carried out, during which, electromagnetic agitation frequency is 280-
290Hz, periodic detection vacuum, temperature and Pressure Rise Rate.As vacuum degree≤1.3Pa, and Pressure Rise Rate≤2Pa/min twice in succession
When, low-temperature refining is completed.It is rapidly heated to 1650 ± 10 DEG C, carries out high temperature refinery, during which, electromagnetic agitation frequency is 350-
360Hz after continuing 10-15min, completes initial refining processing.
Step 3, alloying and double refining:
Power failure is cooled to fast conjunctiva, after adding Ti to stir 2min, Al is added to stir 3-5min to melting down.It is warming up to 1600 ± 10
DEG C, high temperature refinery is carried out, after electromagnetic agitation 15-20 minutes, 1490 ± 10 DEG C is cooled to, Ce and Mg, 310-320Hz electromagnetism is added
Stirring, as vacuum degree≤5Pa, Pressure Rise Rate≤5Pa/min twice in succession, and when the sampling analysis qualification of stokehold, complete double refining.
Step 4, microalloying controls
After double refining, add such as Zr, B, stirs 10-12min to melting down.After stokehold sampling analysis is qualified again, microalloy
Changing control terminates.
Step 5, it is poured:
After microalloying, Ar to 10-12kPa is filled, after adding Mg and Ce element stirring 5-8min melting down, adjustment temperature to 1540
± 10 DEG C of casting.
Embodiment three
Isometric nickel base superalloy IN718 is prepared according to the following steps in the present embodiment:
Step 1, cloth and alloy melting:
Raw material carry out relevant treatment, make its clean surface, metallic luster are presented, and 17 hours dry at 100 DEG C.It presses
IN718 alloying component, according to 25%Ni, 100%Fe, 100%Cr, 100%Nb, 100%Mo, 40%C, 40%Ni in crucible
Raw material sequence successively cloth from bottom to up.
As Pressure Rise Rate < 0.13pa/min, and when vacuum degree < 4pa, start power transmission fusing.Initial stage, using ladder-like power liter
In fusion process, residue Ni and C is added in height mode (frequency 30-50kW/10min, until rated power melt).It is entire molten
Change process time-consuming about 120-150min.
Step 2, initial refining is handled:
After bottom material is melting down, 1550 ± 10 DEG C of temperature control, the low-temperature refining stage is carried out, during which, electromagnetic agitation frequency is 280-
290Hz, periodic detection vacuum, temperature and Pressure Rise Rate.As vacuum degree≤2Pa, and twice in succession Pressure Rise Rate≤2Pa/min when,
Low-temperature refining is completed.It is rapidly heated to 1620 ± 10 DEG C, carries out high temperature refinery, during which, electromagnetic agitation frequency is 350-360Hz,
After continuing 20-25min, initial refining processing is completed.
Step 3, alloying and double refining:
Power failure is cooled to fast conjunctiva, after adding Ti to stir 3min, Al is added to stir 2-4min to melting down.It is warming up to 1590 ± 10
DEG C, high temperature refinery is carried out, after electromagnetic agitation 10-15 minutes, 1480 ± 10 DEG C is cooled to, Ce and Mg, 310-320Hz electromagnetism is added
Stirring, as vacuum degree≤5Pa, and Pressure Rise Rate≤5Pa/min twice in succession, and when the sampling analysis qualification of stokehold, complete secondary fine
Refining.
Step 4, microalloying controls
After double refining, add such as Zr, B, stirs 10-12min to melting down.After stokehold sampling analysis is qualified again, microalloy
Changing control terminates.
Step 5, it is poured:
After microalloying, Ar to 9-10kPa is filled, after adding Mg and Ce element stirring 6-8min melting down, adjustment temperature to 1470
± 10 DEG C of casting.
Detection is using impurity content in the nickel base superalloy of the technology of the present invention preparation, as a result as listed in table 1:
Table 1
The result shows that significantly reduced using objectionable impurities content in the nickel base superalloy of the technology of the present invention melting preparation,
And O content 4-10ppm, N content 10-15ppm, S content in the nickel-base high-temperature single crystal alloy for using the prior art and method to produce
≤ 5ppm, trace element total amount about 180ppm.It can be seen that compared with nickel base superalloy prepared by the prior art and method, the present invention
High temperature alloy melting technique significantly improves the degree of purity of nickel base superalloy.It present invention can be suitably applied to 250kg and 1.5 ton of industry
Grade vaccum sensitive stove.Fusion process of the present invention is short, and low energy consumption, tonnage is high, homogenizes strong, and impurity content is low in alloy melt, and
Fusion process is stable, easily controllable, is suitable for industrial applications.The present invention relates to process for vacuum induction smelting itself, and to original
Material and auxiliary material do not have excessively high requirement, and not only application cost is low but also process is stably and controllable, to improve the technology
The scope of application has fully demonstrated technological value with higher of the invention and economic value.
In addition to above-mentioned implementation, the present invention can also have other embodiments.It is all to be formed using equivalent substitution or equivalent transformation
Technical solution, fall within the scope of protection required by the present invention.
Claims (10)
1. a kind of sublimate method of smelting for nickel base superalloy master alloy, comprising the following steps:
Step 1: cloth and alloy melt, raw material is surface-treated, according to member following in molten alloy ingredient in crucible
The sequence of plain Ni, Fe, Co, Cr, Mo, C, Nb, Ta, W, Ni successively cloth from bottom to up, as vacuum degree < 8Pa, and Pressure Rise Rate≤
When 8Pa/min, start power transmission fusing, after bottom material dissolves, raw material of the addition containing Re, Ru ingredient is to melting down;
Step 2: initial refining controls melt temperature after the raw material of step 1 is melting down, the low-temperature refining stage is carried out, was refined
Cheng Zhong is stirred, periodic detection vacuum degree and Pressure Rise Rate, as vacuum degree≤2Pa, and Pressure Rise Rate≤2Pa/min twice in succession
When, one time low-temperature refining is completed, then quickly increases melt temperature, carries out a high temperature refinery, while carrying out electromagnetic agitation, is stirred
Frequency is 330-360Hz, after continuing 15-25min, completes initial refining processing;
Step 3: alloying and double refining, after the completion of initial refining, power failure is cooled to raw material and be in fast conjunctiva state, by melting
It is smelt point easy oxygen of an addition/nitridation element ti, Al, is stirred 15-30 minutes, after melting down, increases melt temperature, into secondary high-temperature essence
The refining stage after continuing 10-20 minutes, completes secondary high-temperature refining;It reduces temperature and works as vacuum into the secondary low-temperature refining stage
Degree≤5Pa, and twice in succession Pressure Rise Rate≤5Pa/min when, Ce, Mg element is added, lasting to stir, stokehold sampling analysis for the first time,
When each element content meets the requirements, double refining terminates;
Step 4: microalloying controls, after double refining, Hf, B, Zr element is added, stirring stirring 10-20 minutes is melting down
Second of stokehold sampling analysis afterwards, when meeting alloying component, microalloying terminates;
Step 5: being poured, after microalloying, melt temperature is reduced, Y, Ce, Mg element is added after filling Ar gas, after stirring, adjustment temperature
It is poured after degree, completes the sublimate melting of master alloy.
2. being used for the sublimate method of smelting of nickel base superalloy master alloy according to claim 1, it is characterised in that: described
In step 1, raw material are handled, and make its clean surface, metallic luster are presented, and 20 hours dry at 100 DEG C.
3. being used for the sublimate method of smelting of nickel base superalloy master alloy according to claim 1, it is characterised in that: described
1520-1570 DEG C of temperature of low-temperature refining stage control in step 2 carries out electromagnetic agitation, frequency 280-310Hz;Quickly rise
Temperature is to high temperature refining stage and controls 1620-1670 DEG C of temperature, after continuing 15-25 minutes, completion high temperature refinery.
4. being used for the sublimate method of smelting of nickel base superalloy master alloy according to claim 3, it is characterised in that: take seriously
Reciprocal of duty cycle≤2Pa, and twice in succession Pressure Rise Rate≤2Pa/min when, low-temperature refining is completed.As vacuum degree≤1.3Pa, and it is continuous
Twice when Pressure Rise Rate≤1.3Pa/min, one time high temperature refinery is completed.
5. being used for the sublimate method of smelting of nickel base superalloy master alloy according to claim 1, it is characterised in that: described
In step 3, raw material is in fast conjunctiva state, and vacuum degree≤2Pa, and twice in succession Pressure Rise Rate≤2Pa/min when, be added easy
Oxygen/nitridation element ti, Al.
6. being used for the sublimate method of smelting of nickel base superalloy master alloy according to claim 1, it is characterised in that: described
Secondary high-temperature refining stage raising temperature in step 3 is to 1570-1620 DEG C, progress electromagnetic agitation, frequency 360-390Hz,
After continuing 15-30 minutes, temperature is reduced to 1470-1520 DEG C into the secondary low-temperature refining stage, Ce and Mg element, electromagnetism is added
Stirring 10-20 minutes, frequency 310-340Hz.
7. being used for the sublimate method of smelting of nickel base superalloy master alloy according to claim 1, it is characterised in that: described
In step 4, after the completion of double refining, Hf, B, Zr element, stirring stirring 10-20 minutes is added to 1490-1520 DEG C in temperature control.
8. being used for the sublimate method of smelting of nickel base superalloy master alloy according to claim 6, it is characterised in that: be added
Ce and Mg total content≤0.1wt.%, and Ce/Mg≤2:8.
9. being used for the sublimate method of smelting of nickel base superalloy master alloy according to claim 6, it is characterised in that: take seriously
Reciprocal of duty cycle≤5Pa, and twice in succession Pressure Rise Rate≤5Pa/min when, double refining complete.
10. being used for the sublimate method of smelting of nickel base superalloy master alloy according to claim 1, it is characterised in that: institute
It states in step 5, reduces melt temperature to 1450-1470 DEG C, Y, Ce, Mg is added after filling Ar gas, wherein Ce and Mg total content≤
0.1wt.%, and Mg/Ce≤3:7 are stirred 5-15 minutes, are adjusted temperature to 1520-1550 DEG C, are completed casting.
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