CN110106374A - A method of high-purity high temperature alloy is prepared using material is returned - Google Patents
A method of high-purity high temperature alloy is prepared using material is returned Download PDFInfo
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- CN110106374A CN110106374A CN201811576174.7A CN201811576174A CN110106374A CN 110106374 A CN110106374 A CN 110106374A CN 201811576174 A CN201811576174 A CN 201811576174A CN 110106374 A CN110106374 A CN 110106374A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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- C22C1/02—Making non-ferrous alloys by melting
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Abstract
A method of high-purity high temperature alloy is prepared using material is returned, it is characterised in that: successively includes the following steps: to charge;Pretreated high-temperature alloy return material is first added in yttrium oxide crucible, closes vacuum induction melting furnace fire door;Melting: vacuumizing vacuum induction melting furnace, so that vacuum degree starts melting after reaching 0.005 ~ 0.05Pa in furnace, until furnace charge all becomes molten state;When being heated to charge-temperature is 1600 ~ 2000 DEG C, extra argon gas in burner hearth is pumped, metallic yttrium block is added in 0.3 ~ 0.5Pa, and by secondary charging mouth in vacuum degree in maintenance burner hearth, and the additive amount of yttrium block is the 0.01 ~ 0.2% of high-temperature alloy return material weight, refining;After refining, cast molding is carried out.O of the present invention through sublimate melting treated high temperature alloy, N content is reduced to 4ppm hereinafter, purity has reached the level of good high-purity high temperature alloy virgin material, improves the utilization rate of resource.
Description
Technical field
The present invention relates to high temperature alloy preparation fields, and in particular to a kind of to prepare high-purity high temperature alloy using return material
Method.
Background technique
With the development of industrial technology, a large amount of uses of aero-engine and gas turbine, the demand day to high temperature alloy
Benefit increases, and in addition higher requirements are also raised for quality of the development of aircraft industry technology to high temperature alloy.Due to high temperature alloy
Part is usually obtained by casting and forming, and dead head during this can generate certain alloyed scrap at running channel, is in addition cast
The casting flaw generated in the process will cause a large amount of substandard products, and a large amount of vehicle bits can be also generated during casting is mach, these
The alloyed scrap that dead head, waste product casting, running channel generate has accounted for 70% or more of former molten alloy weight.Gas turbine with
And these waste materials generated in the manufacturing process of aero-engine are referred to as return material.It returns in material containing a large amount of strategic conjunction
Gold element, such as: Ni, Cr, Mo, Ti, V, however at present due to the country to the sublimate technology of high-temperature alloy return material not yet at
Ripe, a large amount of high-temperature alloy return material is underused.
Under normal circumstances, compared with virgin material, the type and content of the revert alloy element of high temperature alloy are consistent, mainly
Difference is the difference of impurity element oxygen, nitrogen content, returns to impurity element oxygen in material, nitrogen content increases.Elemental gas oxygen, nitrogen contain
Measure the non-metallic inclusion and show that the mechanical property harm increased to high temperature alloy is more serious, and impurity element and alloying element are formed
The defects of micro- loose, the plasticity and Testing Tensile Strength at Elevated Temperature that will lead to alloy are decreased obviously.It solves to return to the recycling and reusing expected
Problem fundamentally seeks to the sublimate melting for solving the problems, such as to return to material, reduces the oxide and nitride inclusion returned in material
Quantity.Although the removing of nitrogen, oxygen element can be effectively reduced using vacuum induction melting, when vacuum degree is excessively high
The effect of alloy and crucible is also more violent, causes crucible to introduce into alloy and is mingled with.How to improve smelting technology, inhibit fire proofed wood
The physical-chemical reaction of material and alloy melt, so that effectively reducing the elemental gas content in alloy is that scientific research personnel is closed now
The problem of note.
Summary of the invention
It is an object of the present invention to provide a kind of using the method for returning to material preparation high-purity high temperature alloy, and this method can reduce
The content of impurity element in alloy, especially reduction impurity element oxygen, nitrogen content, improve the degree of purity of alloy, and by being somebody's turn to do
The mechanical behavior under high temperature for the high-purity high temperature alloy that method obtains is excellent.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: it is a kind of using return material preparation high-purity high temperature close
The method of gold, successively includes the following steps:
Step (1), charging: yttrium oxide crucible and the ingot mould being fully warmed-up are mounted in vacuum induction melting furnace, are cleared up
Crucible and ingot mould, and install aluminium oxide or yttrium filter screen additional on sprue cup;Yttrium oxide crucible and ingot mould cleaning: it uses
Deduster is clean by yttrium oxide crucible and ingot mould inner wall cleaning;Pretreated high temperature alloy is first added in yttrium oxide crucible
Material is returned, vacuum induction melting furnace fire door is closed;
Step (2), melting: vacuumizing the vacuum induction melting furnace so that in furnace vacuum degree reach 0.005 ~
Start melting after 0.05Pa, 10 ~ 15min is heated with 5 ~ 10KW of small-power, argon gas is filled into vaccum sensitive stove, forms protection gas
Atmosphere after increase power continues 5 ~ 10min of heating to 10~15KW later, increases power to 18 ~ 22KW until furnace charge all becomes
Molten state;When being heated to charge-temperature is 1600 ~ 2000 DEG C, extra argon gas in burner hearth is pumped, vacuum degree in burner hearth is maintained to exist
0.3 ~ 0.5Pa, and metallic yttrium block is added by secondary charging mouth, wherein the additive amount of the yttrium block is that the high temperature alloy returns
Expect the 0.01 ~ 0.2% of weight, then start to refine, refining time is 3 ~ 15min;
Step (3) casting: after refining, stops 2 ~ 5min of power transmission, then measures furnace charge temperature to electricity with 10 ~ 15KW of power
When degree is 1400 ~ 1500 DEG C, cast molding is carried out.The O for returning to material, N content are reduced to after sublimate melting processing
4ppm or less.
Since above-mentioned technical proposal is used, the present invention has following advantages and effect compared with prior art:
1, the present invention adds micro metal Y in vacuum induction melting alloy process, using high-temperature alloy return material as system
The raw material of standby high-purity high temperature alloy reasonably make metal resource obtain efficient circulation utilization, are conducive to environmental protection, reduce height
Temperature alloy cost and energy consumption save resource.
2, vacuum induction melting refining process of the present invention is in 10min or so, the case where guaranteeing alloy mass obtained by melting
Under, it is effectively shortened refining time, reduces production cost.
3, the addition of Y of the present invention can significantly reduce the content of O in high-temperature alloy return material.In the low vacuum of 80 ~ 100Pa
Under, 5ppm or less is reduced to from 34ppm using the O content for the high temperature alloy for returning to material preparation.When vacuum degree is lower than 1 Pa, close
Golden O content is reduced to 2 ~ 6ppm.When vacuum degree is 0.035 Pa, O content can be made to be down to 3ppm or less.
4, under condition of high vacuum degree, the Y of addition plays the role of that oxide crucible is inhibited to decompose in fusion process, reduces
Oxygen supply of the crucible to alloy melt;Under rough vacuum, Y has primarily served the effect of deoxidier, and the strong reducing property of Y plays
The effect of depth deoxidation.
5, under rough vacuum, the addition of Y can promote the removing of N.The addition of Y plays deoxidation and then promotes N's
Removing.Under 0.035Pa condition of high vacuum degree, the available optimal sublimate effect of 0.1%Y is added, oxygen, nitrogen content can be dropped
As low as 2 ~ 4ppm.
6, O of the present invention through sublimate melting treated high temperature alloy, N content is reduced to 4ppm hereinafter, purity reaches
The level of good high-purity high temperature alloy virgin material, improves the utilization rate of resource.
7, mechanical behavior under high temperature of the present invention through sublimate melting treated high temperature alloy is excellent, especially significantly improves
The Testing Tensile Strength at Elevated Temperature and high-temperature yield strength of high temperature alloy.
Specific embodiment
The present invention will be further described below with reference to examples:
Embodiment 1: a method of material preparation high-purity high temperature alloy is returned using cast superalloy
The K417 revert that used raw material is 100% carries out the preparation of 417 master alloys.
Specific sublimate melting step are as follows:
Step (1), charging: yttrium oxide crucible and the ingot mould being fully warmed-up are mounted in vacuum induction melting furnace, are cleared up
Crucible and ingot mould, and install aluminium oxide or yttrium filter screen additional on sprue cup;Yttrium oxide crucible and ingot mould cleaning: it uses
Deduster is clean by yttrium oxide crucible and ingot mould inner wall cleaning;Pretreated high temperature alloy is first added in yttrium oxide crucible
Material is returned, vacuum induction melting furnace fire door is closed;
In the step (1), the pretreated method to the high-temperature alloy return material is carried out to high-temperature alloy return material
After blast or grinding process, recycles industrial ultrasonic cleaning agent or acetone under conditions of frequency is 30 ~ 50KHz, surpass
Sound cleans 5 ~ 10min, is put in baking oven after cleaning and dries 20min under the conditions of 90 DEG C, obtained pretreated high temperature alloy and return
Feed back.
Step (2), melting: vacuumizing the vacuum induction melting furnace, so that vacuum degree reaches 0.035Pa in furnace
After start melting, 13min is heated with 5 ~ 10 KW of small-power, fills argon gas into vaccum sensitive stove, forms protective atmosphere, later
Increase power to continue after heating 10min to 10~15 KW, increases power to 18 ~ 25KW until furnace charge all becomes molten state;
It when being heated to charge-temperature is 1700 DEG C, pumps in burner hearth more than argon gas, maintains in burner hearth vacuum degree in 0.3 ~ 0.5Pa, and
Metallic yttrium block is added by secondary charging mouth, wherein the additive amount of the yttrium is the 0.01% of the high-temperature alloy return material weight,
Start to refine, refining time 10min;
Step (3) casting: after refining, stops power transmission 3min, then measures charge-temperature to electricity with 10 ~ 15KW of power
When being 1500 DEG C, cast molding is carried out.
Oxygen-containing, nitrogen quantity analysis test is carried out to the K417 alloy of 1 cast molding of embodiment.It returns and expects the sublimate
O that processing method contains in alloy before and after the processing, N content, using noble gas pulsed infrared thermal conductivity method (IGI, LECO TC-436,
ASTME1119-2011 is referring to QB-QT-34-1997) measurement.Test result shows described in K417 high-temperature alloy return material process
The processing of sublimate method of smelting after, N, O content in gained alloy respectively by 43ppm, 34ppm be reduced to 2ppm and
The sublimate significant effect of 3ppm, K417 high temperature alloy improves.
900 DEG C of high temperature tensile properties of 1 K417 alloy of table
High temperature tensile properties | Comparative example 1 | Embodiment 1 |
Tensile strength | 704.2 | 725.1 |
Yield strength | 527.6 | 546.9 |
The contraction percentage of area | 3.13 | 6.05 |
Elongation percentage | 15.0 | 20.6 |
From table 1 it follows that preparing high-purity high temperature alloy using return material compared with common induction melting gained alloy
Method processing returns to material gained alloy elongation percentage and the contraction percentage of area be increased to 6.05% He from 3.13% and 12.0% respectively
20.6%.Add 0.1%Y after, the tensile strength and yield strength of K417 high temperature alloy be respectively increased stood 40.7MPa (from
704.2MPa is increased to 745.9MPa) and 39.0 MPa (being increased to 566.6MPa from 527.6MPa).This shows using the place
The method for managing high-temperature alloy return material, can significantly improve the Testing Tensile Strength at Elevated Temperature and high-temperature yield strength of K417 high temperature alloy.
Embodiment 2: a method of material preparation high-purity high temperature alloy is returned using single crystal super alloy
The method that material carries out sublimate melting is returned using N5 single crystal super alloy of the yttrium oxide crucible to 25Kg.
Specific sublimate melting step are as follows:
Step (1), charging: yttrium oxide crucible and the ingot mould being fully warmed-up are mounted in vacuum induction melting furnace, are cleared up
Crucible and ingot mould, and install aluminium oxide or yttrium filter screen additional on sprue cup;Yttrium oxide crucible and ingot mould cleaning: it uses
Deduster is clean by yttrium oxide crucible and ingot mould inner wall cleaning;Pretreated high temperature alloy is first added in yttrium oxide crucible
After returning to material, vacuum induction melting furnace fire door is closed;
In the step (1), the pretreated method to the high-temperature alloy return material is carried out to high-temperature alloy return material
After blast or grinding process, recycles industrial ultrasonic cleaning agent or acetone under conditions of frequency is 30 ~ 50KHz, surpass
Sound cleans 5 ~ 10min, is put in baking oven after cleaning and dries 20min under the conditions of 90 DEG C, obtained pretreated high temperature alloy and return
Feed back.
Step (2), melting: vacuumizing the vacuum induction melting furnace, so that vacuum degree reaches 0.035Pa in furnace
After start melting, 13min is heated with 5 ~ 10 KW of small-power, fills argon gas into vaccum sensitive stove, forms protective atmosphere, later
Increase power to continue after heating 10min to 10~15 KW, increases power to 18 ~ 22KW until furnace charge all becomes melting
State;It when being heated to charge-temperature is 1600 DEG C, pumps in burner hearth more than argon gas, maintains in burner hearth vacuum degree in 0.3 ~ 0.5Pa,
And metallic yttrium block is added by secondary charging mouth, wherein the additive amount of the yttrium is the high-temperature alloy return material weight
0.03%, start to refine, refining time 10min;
Step (3) casting: after refining, stops 2 ~ 5min of power transmission, then measures furnace charge temperature to electricity with 10 ~ 15KW of power
When degree is 1500 DEG C, cast molding is carried out.
Oxygen-containing, nitrogen quantity analysis test is carried out to the N5 single crystal super alloy of 2 cast molding of embodiment.Return to material sublimate
The O that contains in alloy before and after the processing, N content, using noble gas pulsed infrared thermal conductivity method (IGI, LECO TC-436, ASTME1119-
2011 referring to QB-QT-34-1997) measurement.Compared with test result shows the N5 high temperature alloy obtained by the common method of smelting, N5
High-temperature alloy return material is after the sublimate method of smelting processing, and N, O content in gained alloy are respectively by pure
35ppm, 30ppm before change processing are reduced to sublimate treated 3ppm and 4ppm, and the sublimate effect of N5 high temperature alloy obtains
To significantly improving.
870 DEG C of high temperature tensile properties of 2 N5 alloy of table
High temperature tensile properties | Comparative example 2 | Embodiment 2 |
Tensile strength | 927 | 1017 |
Yield strength | 821 | 842 |
The contraction percentage of area | 34 | 33 |
Elongation percentage | 16 | 20 |
From Table 2, it can be seen that preparing the resulting alloy contraction percentage of area base of high-purity high temperature alloy method using return material
This does not change (34% to 33%), and elongation percentage is increased to 20% from 16%.Sublimate processing after, the tensile strength of N5 high temperature alloy and bend
It takes intensity and 90MPa (being increased to 1017MPa from 927MPa) and 21 MPa (being increased to 842MPa from 821MPa) has been respectively increased.
This shows the available high-purity of method of the processing high-temperature alloy return material and the excellent N5 high temperature of mechanical behavior under high temperature closes
Gold.
Embodiment 3: a method of high-purity cast superalloy is prepared using material is returned
The method that material carries out sublimate melting is returned using K417 alloy riser of the yttrium oxide crucible to 25Kg.
Specific sublimate melting step are as follows:
Step (1), charging: yttrium oxide crucible and the ingot mould being fully warmed-up are mounted in vacuum induction melting furnace, are cleared up
Crucible and ingot mould, and install aluminium oxide or yttrium filter screen additional on sprue cup;Yttrium oxide crucible and ingot mould cleaning: it uses
Deduster is clean by yttrium oxide crucible and ingot mould inner wall cleaning;Pretreated high temperature alloy is first added in yttrium oxide crucible
After returning to material, vacuum induction melting furnace fire door is closed;
In the step (1), the pretreated method to the high-temperature alloy return material is carried out to high-temperature alloy return material
After blast or grinding process, recycles industrial ultrasonic cleaning agent or acetone under conditions of frequency is 30 ~ 50KHz, surpass
Sound cleans 5 ~ 10min, is put in baking oven after cleaning and dries 20min under the conditions of 90 DEG C, obtained pretreated high temperature alloy and return
Feed back.
Step (2), melting: vacuumizing the vacuum induction melting furnace, so that vacuum degree reaches 0.035Pa in furnace
After start melting, 13min is heated with 5 ~ 10 KW of small-power, fills argon gas into vaccum sensitive stove, forms protective atmosphere, it
After increase power continues 5 ~ 10min of heating to 10~15 KW afterwards, increase power to 18 ~ 22KW until furnace charge all becomes
Molten state;When being heated to charge-temperature is 1700 DEG C, pump in burner hearth more than argon gas, maintain in burner hearth vacuum degree 0.3 ~
0.5Pa, and metallic yttrium block is added by secondary charging mouth, wherein the additive amount of the yttrium is the high-temperature alloy return material weight
0.2%, start to refine, refining time 10min;
Step (3) casting: after refining, stops 2 ~ 5min of power transmission, then measures furnace charge temperature to electricity with 10 ~ 15KW of power
When degree is 1500 DEG C, cast molding is carried out.
Oxygen-containing, nitrogen quantity analysis test is carried out to the K417 alloy of 3 cast molding of embodiment.Before returning to material sublimate processing
O, N content contained in alloy afterwards, using noble gas pulsed infrared thermal conductivity method (IGI, LECO TC-436, ASTME1119-2011
Referring to QB-QT-34-1997) measurement.Before test result shows that N, O content of high-temperature alloy return material are handled by sublimate respectively
43ppm, 34ppm be reduced to sublimate treated 4ppm and 4ppm, significantly improve the sublimate effect of high temperature alloy.
900 DEG C of high temperature tensile properties of 3 K417 alloy of table
High temperature tensile properties | Comparative example 1 | Embodiment 3 |
Tensile strength | 704.2 | 736.8 |
Yield strength | 527.6 | 552.6 |
The contraction percentage of area | 3.13 | 3.57 |
Elongation percentage | 15.0 | 13.2 |
From table 3 it is observed that expecting after preparing high-purity high temperature alloy method processing that K417 alloy is disconnected using return by described
Face shrinking percentage is increased to 3.57% from 3.13%, the tensile strength and yield strength under high temperature be respectively increased 25MPa (from
704.2MPa to 736.8MPa) and 25MPa (from 527.6MPa to 552.6MPa).It is high-purity that this shows prepared by the utilization return material
High temperature alloy method can handle K417 alloy riser and return to material, and obtain the excellent K417 high temperature alloy of mechanical behavior under high temperature.
Embodiment 4: a method of high-purity wrought superalloy is prepared using material is returned
The method that sublimate melting is carried out to GH4169 revert using yttrium oxide crucible.
Specific sublimate melting step are as follows:
Step (1), charging: yttrium oxide crucible and the ingot mould being fully warmed-up are mounted in vacuum induction melting furnace, are cleared up
Crucible and ingot mould, and install aluminium oxide or yttrium filter screen additional on sprue cup;Yttrium oxide crucible and ingot mould cleaning: it uses
Deduster is clean by yttrium oxide crucible and ingot mould inner wall cleaning;Pretreated high temperature alloy is first added in yttrium oxide crucible
Material is returned, vacuum induction melting furnace fire door is closed;
In the step (1), the pretreated method to the high-temperature alloy return material is carried out to high-temperature alloy return material
After blast or grinding process, recycles industrial ultrasonic cleaning agent or acetone under conditions of frequency is 30 ~ 50KHz, surpass
Sound cleans 5 ~ 10min, is put in baking oven after cleaning and dries 20min under the conditions of 90 DEG C, obtained pretreated high temperature alloy and return
Feed back.
Step (2), melting: vacuumizing the vacuum induction melting furnace, so that vacuum degree reaches 0.035Pa in furnace
After start melting, 13min is heated with 5 ~ 10 KW of small-power, fills argon gas into vaccum sensitive stove, forms protective atmosphere, later
Increase power to continue after heating 10min to 10~15 KW, increases power to 18 ~ 22KW until furnace charge all becomes molten state;
It when being heated to charge-temperature is 1600 DEG C, pumps in burner hearth more than argon gas, maintains in burner hearth vacuum degree in 0.3 ~ 0.5Pa, and
Metallic yttrium block is added by secondary charging mouth, wherein the additive amount of the yttrium is the 0.05% of the high-temperature alloy return material weight,
Start to refine, refining time 10min;
Step (3) casting: after refining, stops power transmission 3min, then with 10 ~ 15KW of power to electricity, measuring charge-temperature is
At 1500 DEG C, cast molding is carried out.
Oxygen-containing, nitrogen quantity analysis test is carried out to the GH4169 alloy of 4 cast molding of embodiment.Return to material sublimate processing
The O that contains in the alloy of front and back, N content, using noble gas pulsed infrared thermal conductivity method (IGI, LECO TC-436, ASTME1119-2011
Referring to QB-QT-34-1997) measurement.Before test result shows that the N of high-temperature alloy return material, O content are handled by sublimate respectively
30ppm, 31ppm be reduced to sublimate treated 2ppm and 3ppm, significantly improve the sublimate effect of high temperature alloy.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of utilize the method for returning to material preparation high-purity high temperature alloy, it is characterised in that: successively include the following steps:
Step (1), charging: yttrium oxide crucible and the ingot mould being fully warmed-up are mounted in vacuum induction melting furnace, are cleared up
Crucible and ingot mould, and install aluminium oxide or yttrium filter screen additional on sprue cup;It is first added in yttrium oxide crucible in advance
High-temperature alloy return material that treated closes vacuum induction melting furnace fire door;
Step (2), melting: vacuumizing the vacuum induction melting furnace so that in furnace vacuum degree reach 0.005 ~
Start melting after 0.05Pa, 10 ~ 15min is heated with 5 ~ 10KW of small-power, argon gas is filled into vaccum sensitive stove, forms protection gas
Atmosphere after increase power continues 5 ~ 10min of heating to 10~15KW later, increases power to 18 ~ 22KW until furnace charge all becomes
Molten state;When being heated to charge-temperature is 1600 ~ 2000 DEG C, extra argon gas in burner hearth is pumped, vacuum degree in burner hearth is maintained to exist
0.3 ~ 0.5Pa, and metallic yttrium block is added by secondary charging mouth, wherein the additive amount of the yttrium block is that the high temperature alloy returns
Expect the 0.01 ~ 0.2% of weight, then start to refine, refining time is 3 ~ 15min;
Step (3) casting: after refining, stops 2 ~ 5min of power transmission, then measures charge-temperature to electricity with 10 ~ 15KW of power
When being 1400 DEG C ~ 1500 DEG C, cast molding is carried out.
2. according to claim 1 utilize the method for returning to material preparation high-purity high temperature alloy, it is characterised in that: the height
It is material head, running channel, riser, faulty part or chip waste material that temperature alloy, which returns to material, concretely wrought superalloy return material,
Cast superalloy returns to material or single crystal super alloy returns to material.
3. according to claim 1 utilize the method for returning to material preparation high-purity high temperature alloy, it is characterised in that: described
In step (1), the yttrium block is technical grade yttrium block.
4. according to claim 1 utilize the method for returning to material preparation high-purity high temperature alloy, it is characterised in that: described
In step (1), the pretreated method to high-temperature alloy return material is to carry out blast or burnishing part to high-temperature alloy return material
After reason, recycles industrial ultrasonic cleaning agent or acetone under conditions of frequency is 30 ~ 50KHz, is cleaned by ultrasonic 5 ~ 10min,
It is put in after cleaning in baking oven and dries 10 ~ 30min under the conditions of 80 ~ 120 DEG C, obtain pretreated high-temperature alloy return material.
5. according to claim 1 utilize the method for returning to material preparation high-purity high temperature alloy, it is characterised in that: the yttrium
The addition of block is the back addition crucible in refining, is added by secondary charging mouth.
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