CN106636702A - Preparation method for low oxygen content and high alloying nickel-based mother alloy and powder - Google Patents
Preparation method for low oxygen content and high alloying nickel-based mother alloy and powder Download PDFInfo
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- CN106636702A CN106636702A CN201611100779.XA CN201611100779A CN106636702A CN 106636702 A CN106636702 A CN 106636702A CN 201611100779 A CN201611100779 A CN 201611100779A CN 106636702 A CN106636702 A CN 106636702A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
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Abstract
The invention discloses a preparation method for a low oxygen content and high alloying nickel-based mother alloy and powder and belongs to the field of powder metallurgy. The technological process of the preparation method includes the steps that firstly, a pure mother alloy ingot is prepared by means of duplex processes of vacuum smelting and electroslag remelting. In the process of vacuum smelting, a calcium oxide crucible is adopted, raw materials are pre-treated, carbon blocks are added in a refining stage for deoxidization, elements prone to the burning loss are supplemented at the end stage of smelting, and the mother alloy ingot in designed components is obtained. In the process of the electroslag smelting, by adjusting the shape, the depth, the viscosity and other parameters of a slag pond, the float-up condition of the nonmetallic inclusion is created, and the mother alloy is further purified. After the mother alloy ingot subjected to electroslag remelting is subjected to scaling, the mother alloy ingot is subjected to high-speed disk grinding breakage under the protective atmosphere, and the ultra-thin mother alloy powder is obtained. The particle size of the K418 mother alloy powder prepared through the method is smaller than 20 microns, the oxygen content is lower than 200 ppm, the sulfur content is lower than 20 ppm, after the alloy podwer is mixed with carbonyl nickel powder, sintering compacting at low temperature can be achieved, and the production cost and the process energy consumption of a high temperature alloy of the powder are greatly reduced.
Description
Technical field
The invention belongs to field of powder metallurgy, there is provided the system of a kind of Ni-based foundry alloy of low oxygen content high-alloying and powder
Preparation Method.
Background technology
Foundry alloy method is the fine master alloy powder that the alloying element in material is prepared into high-alloying, then by foundry alloy
Powder and matrix element powder are mixed in corresponding ratio, sinter the uniform alloy of composition into afterwards.The method is by increasing powder
Last specific surface area and distortion of lattice, improve the chemical composition gradient between powder to improve sintering process in atomic migration driving
Gesture.By appropriate design foundry alloy composition to control sintering process in liquid phase appearance temperature and quantity, further reduce particle
The resistance of rearrangement, raising sintering activity, reduce sintering temperature.This provides new for low cost manufacture Ni-base P/M Superalloy
By way of.
It is the premise for preparing high-performance Ni-base P/M Superalloy to obtain the Ni-based master alloy powder of low oxygen content high-alloying
Condition.The content of active element Cr, Al, Ti and Zr is closed far above common nickel-base high-temperature in high-alloying nickel-base alloy foundry alloy
Gold.In sintering process, impurity oxygen can form more serious oxide folder to master alloy powder particle surface and crystal boundary migration
It is miscellaneous, the comprehensive mechanical property of material is greatly lowered, therefore the oxygen content of master alloy powder has important shadow to properties of product
Ring.The present invention prepares the female conjunction of high-alloying nickel-base alloy using the duplex technique of vacuum induction melting+inert atmosphere electroslag melting
Gold.Vacuum induction melting is capable of the chemical composition of effective control alloy, it is therefore prevented that in high-alloying nickel-base alloy liquation and air
The contact of hydrogen-oxygen nitrogen, but vacuum induction ingot casting is easily polluted by refractory crucible, introduces ceramic inclusions.Electroslag remelting mistake
Cheng Zhong, design is adapted to the slag system of Ni-based foundry alloy remelting, makes the molten alloy droplets of fusing dropwise through the highly active molten slag layer of high temperature,
Floating for field trash provides extraordinary thermodynamics and kineticses condition, is to remove in alloy non-metallic inclusion and efficiently
One of maximally effective refinery practice of desulfurization, can effectively reduce the content of sulphur, remove large scale foreing impuritys, be mingled with interior life
Disperse refinement distribution, reduces the scaling loss of active element Al, Ti etc..Changed by being continuously added to equivalent calcium oxide under inert atmosphere protection
Kind desulfurization condition.During mother alloy ingot is broken, powder is controlled by the broken atmosphere of control and broken intensity
Particle diameter reduce shattering process in oxygenation.Through PHASE DIAGRAM CALCULATION, there is temperature for the alloy in the foundry alloy composition liquid phase of design
System is minimum, and the temperature needed for sintering alloy powder is greatly reduced.
The content of the invention
It is an object of the invention to provide a kind of high-alloying high temperature alloy foundry alloy of low oxygen content and the preparation of powder
Technique.Mother alloy ingot is prepared by vacuum induction melting+electroslag remelting process, the oxygen content of mother alloy ingot, sulphur is reduced and is contained
Amount and the amount of inclusions, improve ingot casting disintegrating apparatus, reduce the oxygen content increased in shattering process.
Concrete technology step has:
1st, pretreatment of raw material:Using conjunction in the middle of Ni-50wt.%Cr intermediate alloys, Ni-5wt.%B intermediate alloys, Ni-Mo
Gold, Ni-Nb intermediate alloys, and aluminium block, titanium sponge, sponge zirconium, graphite block, used as raw materials for metallurgy, its purity is all higher than
99.9wt.%.Raw metal is pre-processed in 5vol.% aqueous hydrochloric acid solutions, oxide on surface, pretreatment time is removed
For 25-35min, rinse in alcohol afterwards, and 30-90min is processed at 60 DEG C in baking oven, make raw material drying.
2nd, the vacuum induction melting of mother alloy ingot:Pretreated raw material is carried out according to the composition of high-alloying foundry alloy
Dispensing, obtains mixed material.Mixed material carries out vacuum induction melting.The composition of high-alloying foundry alloy is Ni-9.15Al-
19.23Cr-6.62Mo-3.31Nb-1.15Ti-0.15Zr-0.02B-0.18C (percentage by weight).Foundry alloy is in vacuum induction
Melting is carried out in smelting furnace, lime crucible is adopted in fusion process, and it is after furnace charge is melting down plus high-power, make on bath temperature
1670 DEG C are risen to, the carbon block of 2wt.% is added, 25-35min is incubated, during being somebody's turn to do molten bath is stirred using magnetic stirrer
Mix, oxygen is fully removed, be added followed by the Al and Ti and 0.01wt.%B of 1wt.%, be incubated 10min, lower the temperature afterwards, fill
Enter argon gas, molten steel is poured and builds up mother alloy ingot.
3rd, the electroslag remelting of female alloying ingot:Inert atmosphere electroslag melting is carried out to the ingot casting of vacuum induction melting, slag charge is matched somebody with somebody
Than for 15-20wt.%CaO, 3-5wt.%Ca, 8-10wt.%CeO, 10-15wt.%Al2O3, 3-5wt.%TiO2, surplus
CaF2.Above-mentioned slag charge is heated to after molten condition, in pouring crystallizer into, crystallizer is copper cold-crucible, by step 2 system
The standby foundry alloy consutrode rod for obtaining is slowly drop down in the slag charge for melting, after the energization starting the arc, adjustment remelting voltage to 30-
50V, electric current 3000-5000A, consutrode is delayed fusing by resistance heat, after the molten steel after fusing and slag charge reaction, purification, is being tied
Brilliant device bottom crystal, obtains pure, uniform, any surface finish foundry alloy ESR ingot.
4th, mother alloy ingot is broken:Mother alloy ingot surface scale is removed, cooling system is carried and is protected a kind of
The high-speed disc of shield atmosphere is galled and crushed in crushing device, and the ratio of grinding ring internal diameter and grinding block diameter is 5:1.Mill device is such as
Shown in Fig. 2.Powder after to crushing is screened, and obtains the master alloy powder of average grain diameter≤20 μm.
The present invention makes in advance foundry alloy alloy with high activity element (such as Cr, Ti, Al, Nb, Zr, B and C), then with mother
The form of alloy, rather than the form of individual element is added in material, by alloying element is oxidizable etc., condition is not limited, energy
The oxidation of active element is enough prevented effectively from, oxygen content is advantageously reduced.The pretreatment of raw material can be reduced effectively the purchasing of raw materials and
The oxidation produced during storage and impurity, it is ensured that the high-purity of raw material during smelting.Using in Ni-50Cr intermediate alloys, Ni-5B
Between alloy, Ni-Mo intermediate alloys, Ni-Nb intermediate alloys as raw materials for metallurgy, can further reduce the temperature needed for alloying,
So as to reduce scaling loss with oxidation, it is ensured that the recovery rate of alloying element.Meanwhile, using lime crucible during vacuum induction melting
Oxygen content in good stability, desulfating and deoxidation reduction fusion process, and it is further by the addition of melting later stage carbon block
Deoxidation, and the easy scaling loss element of supplement before coming out of the stove, it is ensured that the alloy content of foundry alloy is in the range of requiring.It is molten to vacuum induction
The ingot casting that refining is obtained carries out the electroslag remelting of inert gas shielding, further reduces oxygen, sulfur content in ingot casting, and reduction is mingled with
Thing, makes ingot casting sublimate.Mother alloy ingot plasticity is low, is easily broken, readily available fine alloy powder.The high speed of designed, designed
Mill device can effectively prevent the Powder Oxidation in shattering process, be easy to obtain the master alloy powder of low oxygen content, final to obtain
Master alloy powder of the oxygen content less than 200ppm, sulfur content less than 20ppm, its average grain diameter is below 20 μm.Closed using the mother
Bronze end prepares K418 alloys, and sintering process can be made to carry out under conditions of the appearance of a small amount of liquid phase, contributes to solving product burning
Knot problem on deformation, it is possible to increase the dimensional accuracy of sample, moreover it is possible to significantly reduce material powder cost and process energy consumption.
In technical process, the change of foundry alloy impurity content is as shown in table 1.
The impurity content of foundry alloy under the Ni-based foundry alloy of the low oxygen content high-alloying of table 1 and each processing step of powder
Description of the drawings
Fig. 1 is process chart
Fig. 2 is that high-speed disc galls crushing device schematic diagram.
Specific embodiment
Embodiment 1:
By in Ni-50wt.%Cr intermediate alloys, Ni-5wt.%B intermediate alloys, Ni-Mo of the purity more than 99.9wt.%
Between alloy, Ni-Nb intermediate alloys, and aluminium block, titanium sponge, sponge zirconium pre-processed in 5vol.% aqueous hydrochloric acid solutions,
Oxide on surface is removed, pretreatment time is 30min, and alcohol processes in an oven drying 60min after cleaning at 60 DEG C;Pre- place
Raw material after reason carries out dispensing according to target component, and target component is Ni-9.15wt.%Al-19.23wt.%Cr-
6.62wt.%Mo-3.31wt.%Nb-1.15wt.%Ti-0.15wt.%Zr-0.02wt.%B-0. 18wt.%C.By raw material
Melting is carried out in vacuum induction melting furnace, ceramic crucible is adopted in fusion process, and it is after furnace charge is melting down plus high-power, make to melt
Pond temperature rises to 1670 DEG C, adds the carbon block of 2wt.%, is incubated 30min, using magnetic stirrer to molten bath during being somebody's turn to do
It is stirred, oxygen is fully removed, be added followed by the Al and Ti and 0.01wt.%B of 1wt.%, be incubated 10min, drops afterwards
Temperature, be filled with argon gas, molten steel is poured and builds up foundry alloy consutrode rod.The electroslag that consutrode rod carries out inert atmosphere protection is melted
Refining, slag charge proportioning is 18wt.%CaO, 4wt.%Ca, 9wt.%CeO, 12wt.%Al2O3, 4wt.%TiO2, surplus CaF2.Will
Above-mentioned slag charge is heated to after molten condition, in pouring crystallizer into.Consutrode rod is slowly drop down in the slag charge for melting, and is powered
After arc, adjustment remelting voltage to 50V, electric current 3000A, consutrode is by the slow fusing of resistance heat, and the molten steel after fusing is anti-with slag charge
After should, purifying, in crystalliser feet crystallization, pure, uniform, any surface finish foundry alloy ESR ingot is obtained.Afterwards by ESR ingot
Epidermis is removed, and is crushed in crushing device is galled with the high-speed disc of protective atmosphere with cooling system.Powder after will be broken
Screened, finally given master alloy powder.
Embodiment 2:
By in Ni-50wt.%Cr intermediate alloys, Ni-5wt.%B intermediate alloys, Ni-Mo of the purity more than 99.9wt.%
Between alloy, Ni-Nb intermediate alloys, and aluminium block, titanium sponge, sponge zirconium are pre-processed in 5wt.% aqueous hydrochloric acid solutions, gone
Except oxide on surface, pretreatment time is 30min, and alcohol processes in an oven drying 60min after cleaning at 60 DEG C;Pretreatment
Raw material afterwards carries out dispensing according to target component, and target component is Ni-9.15wt.%Al-19.23wt.%Cr-6.62wt.%
Mo-3.31wt.%Nb-1.15wt.%Ti-0.15wt.%Zr-0.02wt.%B-0.18wt.%C.By raw material in vacuum induction
Melting is carried out in smelting furnace, ceramic crucible is adopted in fusion process, and it is after furnace charge is melting down plus high-power, bath temperature is increased
To 1670 DEG C, the carbon block of 2wt.% is added, be incubated 30min, during being somebody's turn to do molten bath is stirred using magnetic stirrer, made
Oxygen is fully removed, and is added followed by the Al and Ti and 0.01wt.%B of 1wt.%, is incubated 10min, is lowered the temperature afterwards, is filled with argon
Gas, molten steel is poured and builds up foundry alloy consutrode rod.Consutrode rod is carried out into the electroslag melting of inert atmosphere protection, slag charge is matched somebody with somebody
Than for 16wt.%CaO, 3wt.%Ca, 10wt.%CeO, 12wt.%Al2O3, 5wt.%TiO2, surplus CaF2.By above-mentioned slag charge
After being heated to molten condition, in pouring crystallizer into.Consutrode rod is slowly drop down in the slag charge for melting, and after the energization starting the arc, is adjusted
, to 30V, electric current 5000A, consutrode is by the slow fusing of resistance heat, the molten steel after fusing and slag charge reaction, purification for the molten voltage of bulk wight
Afterwards, crystallize in crystalliser feet, obtain pure, uniform, any surface finish foundry alloy ESR ingot.ESR ingot epidermis is gone afterwards
Remove, crushed in crushing device is galled with the high-speed disc of protective atmosphere with cooling system.Powder after will be broken is sieved
Choosing, finally gives master alloy powder.
Embodiment 3:
By in Ni-50wt.%Cr intermediate alloys, Ni-5wt.%B intermediate alloys, Ni-Mo of the purity more than 99.9wt.%
Between alloy, Ni-Nb intermediate alloys, and aluminium block, titanium sponge, sponge zirconium are pre-processed in 5wt.% aqueous hydrochloric acid solutions, gone
Except oxide on surface, pretreatment time is 30min, and alcohol processes in an oven drying 60min after cleaning at 60 DEG C;Pretreatment
Raw material afterwards carries out dispensing according to target component, and target component is Ni-9.15wt.%Al-19.23wt.%Cr-6.62wt.%
Mo-3.31wt.%Nb-1.15wt.%Ti-0.15wt.%Zr-0.02wt.%B-0.18wt.%C.By raw material in vacuum induction
Melting is carried out in smelting furnace, ceramic crucible is adopted in fusion process, and it is after furnace charge is melting down plus high-power, bath temperature is increased
To 1670 DEG C, the carbon block of 2wt.% is added, be incubated 30min, during being somebody's turn to do molten bath is stirred using magnetic stirrer, made
Oxygen is fully removed, and is added followed by the Al and Ti and 0.01wt.%B of 1wt.%, is incubated 10min, is lowered the temperature afterwards, is filled with argon
Gas, molten steel is poured and builds up foundry alloy consutrode rod.Consutrode rod is carried out into the electroslag melting of inert atmosphere protection, slag charge is matched somebody with somebody
Than for 15wt.%CaO, 5wt.%Ca, 8wt.%CeO, 11wt.%Al2O3, 4wt.%TiO2, surplus CaF2.By above-mentioned slag charge
After being heated to molten condition, in pouring crystallizer into.Consutrode rod is slowly drop down in the slag charge for melting, and after the energization starting the arc, is adjusted
, to 45V, electric current 3500A, consutrode is by the slow fusing of resistance heat, the molten steel after fusing and slag charge reaction, purification for the molten voltage of bulk wight
Afterwards, crystallize in crystalliser feet, obtain pure, uniform, any surface finish foundry alloy ESR ingot.ESR ingot epidermis is gone afterwards
Remove, crushed in crushing device is galled with the high-speed disc of protective atmosphere with cooling system.Powder after will be broken is sieved
Choosing, finally gives master alloy powder.
Claims (5)
1. the preparation method of a kind of Ni-based foundry alloy of low oxygen content high-alloying and powder, it is characterised in that:
Step one, with Ni-50wt.%Cr intermediate alloys, Ni-5wt.%B intermediate alloys, Ni-Mo intermediate alloys, Ni-Nb in the middle of
Alloy, and aluminium block, titanium sponge, sponge zirconium, graphite block, used as raw material, the purity of various raw materials is all higher than 99.9%;Metal raw
Material is pre-processed in 5vol.% aqueous hydrochloric acid solutions, removes oxide on surface, and pretreatment time is 25-35min, and alcohol is washed
Process at 60 DEG C in an oven after net and dry 30-90min;
Step 2, pretreated raw material carry out dispensing according to the composition of high-alloying foundry alloy, obtain mixed material.Mixing is former
Material carries out vacuum induction melting;Ceramic crucible is adopted in fusion process, and it is after furnace charge is melting down plus high-power, make on bath temperature
1670 DEG C are risen to, 2wt.% carbon blocks are added, 25-35min is incubated, magnetic stirrer is stirred molten bath used in fusion process
Mix, oxygen is fully removed, be added followed by the Al and Ti and 0.01wt.%B of 1wt.%, be incubated 8-12min, cooling afterwards,
Argon gas is filled with, molten steel is poured and is built up foundry alloy consutrode rod;
Step 3, slag charge is heated to after molten condition, in pouring crystallizer into, crystallizer is copper cold-crucible, by step 2
The foundry alloy consutrode rod for preparing is slowly drop down in the slag charge for melting, after the energization starting the arc, adjustment remelting voltage to 30-
50V, electric current 3000-5000A, consutrode is delayed fusing by resistance heat, after the molten steel after fusing and slag charge reaction, purification, is being tied
Brilliant device bottom crystal, obtains pure, uniform, any surface finish foundry alloy ESR ingot;Jing after vacuum electroslag remelting, foundry alloy oxygen contains
Amount is less than 150ppm, and sulfur content is less than 20ppm;
Step 4, mother alloy ingot surface scale is removed, broken with the worn-off of cooling system and the high-speed disc of protective atmosphere
Crushed in device;Powder after to crushing is screened, and obtains master alloy powder.
2. the preparation method of a kind of Ni-based foundry alloy of low oxygen content high-alloying according to claim 1 and powder, it is special
Levy and be:The composition of described high-alloying foundry alloy is:Ni-9.15wt.%Al-19.23wt.%Cr-6.62wt.%Mo-
3.31wt.%Nb-1.15wt.%Ti-0.15wt.%Zr-0.02wt.%B-0.18wt.%C;The liquid of nickel-base alloy foundry alloy
It is 1135 DEG C mutually to form temperature.
3. the preparation method of a kind of Ni-based foundry alloy of low oxygen content high-alloying according to claim 1 and powder, it is special
Levy and be:Slag charge proportioning described in step 3 is 15-20wt.%CaO, 3-5wt.%Ca, 8-10wt.%CeO, 10-15wt.%
Al2O3, 3-5wt.%TiO2, surplus CaF2。
4. the preparation method of a kind of Ni-based foundry alloy of low oxygen content high-alloying according to claim 1 and powder, it is special
Levy and be:Mill device described in step 4 is cooled down using cooling water, is protected using high-purity argon gas, grinding ring internal diameter
It is 5 with the ratio of grinding block diameter:1.
5. the preparation method of a kind of Ni-based foundry alloy of low oxygen content high-alloying according to claim 1 and powder, it is special
Levy and be:The final oxygen content of the master alloy powder described in step 4 is less than 200ppm, and sulfur content is less than 20ppm, is mingled with material
Amount is less than 0.002wt.%, average grain diameter≤20 μm of powder particle.
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CN109161697A (en) * | 2018-10-26 | 2019-01-08 | 北京科技大学 | A method of non-metallic inclusion in control powder metallurgy high-temperature alloy master alloy |
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CN109295330A (en) * | 2018-10-26 | 2019-02-01 | 北京科技大学 | A kind of method of nitride field trash in refinement ni-base wrought superalloy |
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CN109295330B (en) * | 2018-10-26 | 2020-06-19 | 北京科技大学 | Method for refining nitride inclusions in nickel-based wrought superalloy |
CN110760718A (en) * | 2019-11-25 | 2020-02-07 | 北京科技大学 | Preparation method of high-tungsten high-cobalt nickel alloy high-purity fine-grain bar |
CN111118304A (en) * | 2020-01-06 | 2020-05-08 | 江苏远航精密合金科技股份有限公司 | Preparation method of high-purity nickel strip foil for electronic industry |
CN111926198A (en) * | 2020-06-04 | 2020-11-13 | 广东华鳌合金新材料有限公司 | Method for controlling surface quality and secondary shrinkage cavity size of K418 master alloy vacuum induction melting electrode |
CN112296343A (en) * | 2020-09-04 | 2021-02-02 | 武汉科技大学 | Method for preparing superfine metal powder by smelting hollow electrode |
CN112296343B (en) * | 2020-09-04 | 2023-05-26 | 武汉科技大学 | Method for preparing superfine metal powder by hollow electrode smelting |
CN116287812A (en) * | 2023-05-24 | 2023-06-23 | 江苏美特林科特殊合金股份有限公司 | Smelting method of aluminum-free high-temperature alloy |
CN116287812B (en) * | 2023-05-24 | 2023-07-21 | 江苏美特林科特殊合金股份有限公司 | Smelting method of aluminum-free high-temperature alloy |
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