CN115852184A - Method for preparing master alloy by remelting and recovering high-temperature alloy powder - Google Patents

Method for preparing master alloy by remelting and recovering high-temperature alloy powder Download PDF

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CN115852184A
CN115852184A CN202211575142.1A CN202211575142A CN115852184A CN 115852184 A CN115852184 A CN 115852184A CN 202211575142 A CN202211575142 A CN 202211575142A CN 115852184 A CN115852184 A CN 115852184A
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alloy
remelting
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李徐刚
栾吉哲
李爱民
刘家鹏
崔利民
罗保帅
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Avic Shangda Superalloy Materials Co ltd
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Abstract

The invention relates to the technical field of powder metallurgy, and particularly discloses a method for preparing master alloy by remelting high-temperature alloy powder, which comprises the following steps: proportioning according to the components of the high-temperature alloy, wherein the high-temperature alloy powder accounts for 10-50% of the total mass of the proportioning; charging: wrapping and packaging the high-temperature alloy powder return material by using an aluminum foil, then putting the high-temperature alloy return material wrapped by the aluminum foil into a vacuum induction melting furnace, and adding a small metal material to cover the powder return material until a crucible is filled with the high-temperature alloy powder return material; melting: after the charging is finished, vacuumizing to less than 30Pa, filling argon to a certain pressure, introducing the electrically melted furnace burden, vacuumizing to less than 1Pa after the furnace burden is melted, and continuously adding the rest material blocks and the molten materials until the furnace burden is completely melted; refining and alloying: after furnace burden is completely melted, refining and degassing are carried out at higher refining temperature and higher vacuum degree, and after the components of molten steel meet the alloy requirements, casting is carried out to obtain the high-temperature alloy remelting master alloy.

Description

Method for preparing master alloy by remelting and recovering high-temperature alloy powder
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a method for preparing master alloy by remelting high-temperature alloy powder.
Background
The high-temperature powder metallurgy technology has extremely wide application potential in the fields of biomedical treatment, laser cladding, automobile manufacturing, aerospace, creative design, industrial dies, scientific research and the like. The particle size ranges of the powders used in different fields of application differ, for example, in the conventional powder metallurgy field, 1-75 μm powder is generally used; in the field of injection molding, a powder of 1 μm is generally used; laser cladding typically uses 53 μm powder; additive manufacturing (i.e. 3D printing) typically uses 15 μm of powder. Whereas the alloy powder obtained by pulverization is generally in the 0.1 μm full size range, subject to the level of powder preparation technology, the yield of the target size range is usually only 20 to 50%, and if the high-temperature alloy metal powder outside the target size range can be utilized by remelting, a huge economic value will be realized.
At the present stage, a vacuum induction smelting furnace is usually adopted to remelt high-temperature alloy powder, micron-sized powder particles are very easy to be adsorbed into a high-vacuum pump in the high-vacuum smelting process to cause damage to a vacuum system of the smelting furnace, the larger the furnace body is, the more the powder charging amount is, the greater the damage to the vacuum system of the furnace body is, and the remelting production of the powder return materials at the present stage is carried out in a small smelting (less than 350 kg) crucible at the laboratory level, so that the industrial production is difficult to realize. Meanwhile, because the alloy powder is easy to adsorb and enter a vacuum pump, and the vacuum degree is difficult to be pumped for smelting, the control on harmful gases such as oxygen, nitrogen and the like is unstable, and the remelted finished product components do not meet the index requirements and are scrapped. In the prior art, a method of using a high molecular organic matter to bond powder, then briquetting the powder and then carrying out vacuum induction melting is adopted, but the method easily causes the content of elements such as carbon, nitrogen and the like in the alloy to increase, and simultaneously causes residues to be entrained in the alloy.
Disclosure of Invention
Aiming at the problems existing in the existing high-temperature alloy powder remelting, the invention provides a method for remelting and recycling high-temperature alloy powder to prepare a master alloy. The method is based on a vacuum induction smelting furnace, high-temperature alloy powder of more than 1 ton is smelted in one time, industrial production is realized, the content of impurity elements such as nitrogen, carbon and the like in remelted alloy is reduced, and meanwhile, the damage to the vacuum induction smelting furnace is small.
In order to realize the aim, the invention provides a method for preparing master alloy by remelting and recovering high-temperature alloy powder, which at least comprises the steps of proportioning, charging and melting, refining, alloying and pouring;
in the batching step, high-temperature alloy powder return materials, aluminum foils and alloy ingredient material blocks which account for 10% -50% of the weight of the alloy are prepared;
in the charging and melting step, a first melting stage and a second melting stage are included, wherein in the first melting stage, the aluminum foil is used for wrapping and packaging the high-temperature alloy powder return material, the high-temperature alloy powder return material is placed in a vacuum induction melting furnace, alloy components are added until the crucible is full, the high-temperature alloy powder return material is firstly vacuumized to be less than 30Pa, argon is filled to be 5000-7000Pa, and electric melting furnace burden is introduced; in the second melting stage, after the furnace burden in the first melting stage is melted, vacuumizing to less than 1Pa, and continuously adding the rest alloy ingredient blocks until the furnace burden is completely melted.
In the prior art, high-temperature alloy powder is added into a vacuum induction melting furnace and then is vacuumized, so that the powder is seriously absorbed by a vacuumizing device, a vacuum pump system of the vacuum induction furnace is damaged, and large-batch industrial production cannot be realized. According to the technical scheme, before loading, the powder is tightly wrapped by the aluminum foil and placed into a furnace, before electrifying, the furnace is firstly vacuumized to less than 30pa, and the contents of harmful gases such as H, O, N and the like in the furnace are purified; then, inert gas Ar is filled into the furnace to the vacuum degree P =5000-7000pa, and then the melting material is electrified. The operation has the advantages that: (1) the alloy powder is wrapped and packaged by the aluminum foil, so that the powder absorption of equipment in the vacuum-pumping process can be prevented, the equipment cannot be damaged (2) the phenomenon that the content of molten steel O and N is too high due to gas in the atmosphere during the melting of the metal powder is avoided. (3) Argon is filled to enable the furnace to form positive pressure, so that damage to a vacuum system caused by dust floating to enter a vacuum pump in the melting process of metal powder is prevented, and meanwhile, the phenomenon of powder splashing in the melting process can be avoided.
Preferably, in the method for preparing the master alloy by remelting and recovering the high-temperature alloy powder, in the steps of refining and alloying, the refining temperature is 1500-1520 ℃, the vacuum degree is less than 1Pa, and in the process of the refining period, alloy component blocks are supplemented according to the requirements of chemical components and analysis results.
Preferably, in the method for preparing the master alloy by remelting and recovering the high-temperature alloy powder, stirring is carried out for 7-13 minutes every 15-25 minutes in the refining and alloying steps, and the total refining time is not less than 60 minutes.
Preferably, the method for preparing the master alloy by remelting and recovering the superalloy powder comprises the step of charging alloy component blocks with low affinity with O and N, including alloy component blocks of Ni, cr, co, W and Mo, in the charging and melting steps.
The preferential addition of the alloy component blocks with lower affinity with O and N can reduce the introduction of O and N elements in the process of melting.
Preferably, in the method for preparing the master alloy by remelting and recovering the superalloy powder, elements such as Nb, ti, al, B, and Zr are added in the refining and alloying step.
By adding the raw materials such as Nb, al, ti and the like in the refining period, the range and the distribution uniformity of the raw materials such as Nb, al, ti and the like in the alloy ingot are effectively controlled, and the burning loss of the raw materials such as Nb, al, ti and the like is prevented.
Preferably, the method for remelting and recovering the high-temperature alloy powder to prepare the master alloy is characterized in that in the refining and alloying step, when the content of nitrogen in the molten material is determined to be more than or equal to 40ppm by sampling, the molten material is heated to 1580-1600 ℃ by electrifying, and the temperature is kept for 30-60 minutes to remove nitrogen; when the oxygen content in the melting material is measured to be more than or equal to 30ppm by sampling, C and Al are adjusted to target values according to the content of the C and Al elements for deoxidation.
Preferably, the method for preparing the master alloy by remelting and recovering the superalloy powder is characterized in that in the refining and alloying step, after the other components of the molten material meet the composition requirements, the B element blocks or particles are added.
In the present embodiment, the blending and alloying are performed during the refining. The advantages of this operation are: (1) the components are adjusted without waiting for the completion of refining, so that the smelting time is greatly reduced. (2) In the alloying component adjusting process, the content of harmful elements such as solution gas and the like is increased due to the addition of metal materials, and the operation can be carried out during the high-temperature high-vacuum refining to remove gas or burn off other harmful elements.
Preferably, the method for preparing the master alloy by remelting and recovering the high-temperature alloy powder comprises the step of pouring the molten material into an ingot mold after the temperature of the molten material is raised to 1530-1540 ℃ in the pouring step.
Preferably, the method for preparing the master alloy by remelting and recovering the superalloy powder comprises the steps of baking the ingot mould to 450-470 ℃, and preserving heat for 1.5 hours for use.
Preferably, the method for preparing the master alloy by remelting and recovering the high-temperature alloy powder comprises 20-30% of high-temperature alloy powder return materials.
This patent presents a more efficient denitrification process: if the N content exceeds the standard, the temperature is increased to 1580-1600 ℃, then the temperature is preserved for 30-60min under high vacuum (P < 1 Pa), and then sampling analysis is carried out, so that the overall N removal time is reduced, and the N content can be controlled to a lower level. The existing denitrification method of the scheme is to maintain high vacuum for a long time, when the charging amount is increased, the denitrification method takes a long time, and the furnace body is greatly damaged by maintaining high-temperature denitrification for a long time. The high-temperature denitrification method provided by the application has higher efficiency and small damage to the furnace body.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
This example provides a recycling method of a returned Inconel 718 ni-based superalloy powder, wherein the Inconel 718 alloy has the following components:
TABLE 1Inconel 718 alloy composition requirements
Figure BDA0003989088010000041
The vacuum melting method for remelting and recovering Inconel 718 high-temperature alloy powder comprises the following steps of:
a. preparing raw materials: the Inconel 718 alloy is prepared according to the components, 10% of metal powder return material is prepared in the smelting process, the surfaces of the used raw material and the return material are free of oil stains and oxidation, and the chemical components are accurate.
b. Charging: the high-temperature alloy powder return material is wrapped and packaged by aluminum foil, so that the packaging is tight and has no leakage; then, putting the high-temperature alloy return material wrapped by the aluminum foil into a vacuum induction melting furnace; adding alloy components of Ni, fe, mo and Cr into the block cover powder return material until the crucible is filled with the material, but the material should not exceed the crucible opening, so as to prevent the crucible opening from slagging;
c. melting: after the charging is finished, vacuumizing to 25Pa, filling argon to 6000Pa, and electrifying to melt the furnace material; after the furnace burden is melted, vacuumizing to less than 1Pa, and continuously adding the Nb metal blocks until the furnace burden is completely melted;
d. refining and alloying: after the furnace burden is completely melted, refining and degassing are carried out under the conditions of 1520 ℃ and the vacuum degree of less than 1Pa, and stirring is carried out for 10 minutes every 20 minutes in the refining process; adding Ti, al and C in the refining process, supplementing materials and adjusting components according to the analysis result of the components of the molten steel, wherein the total refining time is 90 minutes, then heating to 1580 ℃, preserving heat for 40 minutes to denitrify, and adjusting the content of C and Al to deoxidize;
e. pouring: and adding the B material block and adjusting the components after the rest components of the molten steel meet the alloy requirements, baking the steel ingot mould to 450 ℃, keeping the temperature for 1.5 hours, heating the molten steel to 1530 ℃, and pouring the molten steel into the steel ingot mould to obtain the Inconel 718 nickel-based high-temperature alloy remelting mother alloy, wherein the content of each component of the remelting mother alloy is as follows.
Table 2Inconel 718 nickel-base superalloy remelting master alloy composition table
Figure BDA0003989088010000051
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Example 2
This example provides a method for recycling a powder return of Inconel 718 ni-based superalloy, where the Inconel 718 alloy has the following composition in table 1:
the vacuum melting method for remelting and recovering Inconel 718 high-temperature alloy powder comprises the following steps of:
a. preparing raw materials: the Inconel 718 alloy is prepared according to the components, 30% of metal powder return material is prepared in the smelting process, the surfaces of the used raw material and the return material are free of oil stains and oxidation, and the chemical components are accurate.
b. Charging: the high-temperature alloy powder return material is wrapped and packaged by aluminum foil, so that the packaging is tight and has no leakage; then, putting the high-temperature alloy return material wrapped by the aluminum foil into a vacuum induction melting furnace; adding alloy components of Ni, fe, mo and Cr into the block cover powder return material until the crucible is filled with the material, but the material should not exceed the crucible opening, so as to prevent the crucible opening from slagging;
c. melting: after the charging is finished, vacuumizing to 20Pa, filling argon to 7000Pa, and electrifying to melt the furnace material; after the furnace burden is melted, vacuumizing to less than 1Pa, and continuously adding the Nb metal blocks until the furnace burden is completely melted;
d. refining and alloying: after the furnace burden is completely melted, refining and degassing are carried out under the conditions that the temperature is 1510 ℃ and the vacuum degree is less than 1Pa, and stirring is carried out for 9 minutes every 25 minutes in the refining process; adding Ti, al and C in the refining process, supplementing materials and adjusting components according to the analysis result of the components of the molten steel, wherein the total refining time is 102 minutes, then heating to 1600 ℃, preserving heat for 30 minutes to denitrify, and adjusting the content of C and Al to deoxidize;
e. pouring: and adding the B material block and adjusting the components after the rest components of the molten steel meet the alloy requirements, baking the molten steel to 470 ℃, keeping the temperature for 1.5 hours, then heating the molten steel to 1540 ℃, pouring the molten steel into the ingot mold to obtain the Inconel 718 nickel-based high-temperature alloy remelting mother alloy, wherein the content of each component of the remelting mother alloy is as shown in the table below.
TABLE 3Inconel 718 Ni-based superalloy remelting master alloy composition table
Figure BDA0003989088010000061
Example 3
The embodiment provides a recycling method of a nickel-based superalloy powder return material with the trademark of Inconel 718, wherein the components of the Inconel 718 alloy are shown in the table 1:
the vacuum melting method for remelting and recovering Inconel 718 high-temperature alloy powder comprises the following steps of:
a. preparing raw materials: the Inconel 718 alloy is prepared according to the components, 50% of metal powder return material is prepared in the smelting process, the surfaces of the used raw material and the return material are free of oil stains and oxidation, and the chemical components are accurate.
b. Charging: the high-temperature alloy powder return material is wrapped and packaged by aluminum foil, so that the packaging is tight and has no leakage; then, putting the high-temperature alloy return material wrapped by the aluminum foil into a vacuum induction melting furnace; adding alloy components of Ni, fe, mo and Cr into the block cover powder return material until the crucible is filled with the material, but the material should not exceed the crucible opening, so as to prevent the crucible opening from slagging;
c. melting: after the charging is finished, vacuumizing to 23Pa, filling argon to 5000Pa, and electrifying to melt the furnace charge; after the furnace burden is melted, vacuumizing to less than 1Pa, and continuously adding the Nb metal blocks until the furnace burden is completely melted;
d. refining and alloying: after the furnace burden is completely melted, refining and degassing are carried out under the conditions that the temperature is 1500 ℃ and the vacuum degree is less than 1Pa, and stirring is carried out for 13 minutes every 25 minutes in the refining process; adding Ti, al and C in the refining process, supplementing materials and adjusting components according to the analysis result of the components of the molten steel, wherein the total refining time is 114 minutes, then heating to 1600 ℃, preserving heat for 50 minutes to denitrify, and adjusting the content of C and Al to deoxidize;
e. pouring: and adding the B material block and adjusting the components after the rest components of the molten steel meet the alloy requirements, baking the steel ingot mould to 460 ℃, preserving the heat for 1.5 hours, then heating the molten steel to 1540 ℃, and pouring the molten steel into the steel ingot mould to obtain the Inconel 718 nickel-based high-temperature alloy remelting mother alloy, wherein the content of each component of the remelting mother alloy is as follows.
Table 4Inconel 718 nickel-base high-temp. alloy remelting master alloy composition table
Figure BDA0003989088010000071
Example 4
This example provides a method for recycling a powder return of Inconel 718 ni-based superalloy, where the Inconel 718 alloy has the following composition in table 1:
the vacuum melting method for remelting and recovering Inconel 718 high-temperature alloy powder comprises the following steps of:
a. preparing raw materials: the Inconel 718 alloy is prepared according to the components, 10% of metal powder return material is prepared in the smelting process, the surfaces of the used raw material and the return material are free of oil stains and oxidation, and the chemical components are accurate.
b. Charging: the high-temperature alloy powder return material is wrapped and packaged by aluminum foil, so that the packaging is tight and leakage-free; then, putting the high-temperature alloy return material wrapped by the aluminum foil into a vacuum induction melting furnace; adding alloy components of Ni, fe, mo and Cr into the block cover powder return material until the crucible is filled with the material, but the material should not exceed the crucible opening, so as to prevent the crucible opening from slagging;
c. melting: after the charging is finished, vacuumizing to 25Pa, filling argon to 6000Pa, and electrifying to melt the furnace material; after the furnace burden is melted, vacuumizing to less than 1Pa, and continuously adding the Nb metal blocks until the furnace burden is completely melted;
d. refining and alloying: after the furnace burden is completely melted, refining and degassing are carried out under the conditions that the temperature is 1520 ℃ and the vacuum degree is less than 1Pa, and stirring is carried out for 10 minutes every 20 minutes in the refining process; adding Ti, al and C in the refining process, and supplementing materials and adjusting components according to the analysis result of the components of the molten steel, wherein the total refining time is 90 minutes;
e. pouring: and adding the B material block and adjusting the components after the rest components of the molten steel meet the alloy requirements, baking the steel ingot mould to 450 ℃, keeping the temperature for 1.5 hours, heating the molten steel to 1530 ℃, and pouring the molten steel into the steel ingot mould to obtain the Inconel 718 nickel-based high-temperature alloy remelting mother alloy, wherein the content of each component of the remelting mother alloy is as follows.
TABLE 5Inconel 718 Ni-based superalloy remelting master alloy composition table
Figure BDA0003989088010000081
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. A method for preparing master alloy by remelting and recovering high-temperature alloy powder is characterized by comprising the steps of proportioning, charging and melting, refining and alloying and pouring;
in the batching step, high-temperature alloy powder return materials, aluminum foils and alloy ingredient material blocks which account for 10% -50% of the weight of the alloy are prepared;
in the charging and melting step, a first melting stage and a second melting stage are included, wherein in the first melting stage, the aluminum foil is used for wrapping and packaging the high-temperature alloy powder return material, the high-temperature alloy powder return material is placed in a vacuum induction melting furnace, alloy components are added until the crucible is filled, the vacuum is firstly pumped to be less than 30Pa, argon is filled to be 5000-7000Pa, and electric melting furnace charge is introduced; in the second melting stage, after the furnace burden in the first melting stage is melted, vacuumizing to less than 1Pa, and continuously adding the rest alloy ingredient blocks until the furnace burden is completely melted.
2. The method for remelting and recovering superalloy powder to prepare a master alloy according to claim 1, wherein in the refining and alloying steps, the refining temperature is 1500 ℃ to 1520 ℃, the vacuum degree is less than 1Pa, and during the refining period, alloy component blocks are added according to the requirements of chemical components according to the analysis results.
3. The method for producing a master alloy by remelting and recovering superalloy powder according to claim 1, wherein in the refining and alloying step, stirring is performed for 7 to 13 minutes every 15 to 25 minutes, and the total refining time is not less than 60 minutes.
4. The method for producing a master alloy according to claim 1, wherein in the charging and melting step, the alloy constituent pieces having low affinity for O and N, including the alloy constituent pieces of Ni, cr, co, W and Mo, are charged.
5. The method for remelting and recovering superalloy powder to produce a master alloy according to claim 1, wherein Nb, ti, al, B, zr, and the like are added during the refining and alloying steps.
6. The method for remelting and recovering the high-temperature alloy powder to prepare a master alloy according to claim 1, wherein in the refining and alloying steps, when the content of nitrogen in the molten material is determined to be more than or equal to 40ppm by sampling, the molten material is heated to 1580-1600 ℃ by electrifying, and the temperature is kept for 30-60 minutes to remove nitrogen; when the oxygen content in the melting material is measured to be more than or equal to 30ppm by sampling, C and Al are adjusted to target values according to the content of the C and Al elements for deoxidation.
7. The method for remelting and recovering superalloy powder to produce a master alloy as in claim 5, wherein in the refining and alloying step, lumps or grains of B element are added after the remaining components of the molten material meet compositional requirements.
8. The method for producing a master alloy by remelting and recovering a superalloy powder according to claim 1, wherein in the casting step, the molten material is cast into an ingot mold after being heated to 1530-1540 ℃.
9. The method for producing a master alloy by remelting and recovering superalloy powder according to claim 1, wherein the ingot mold is baked to 450-470 ℃ and held for 1.5 hours.
10. The method of producing a master alloy by remelting and recovering superalloy powder according to claim 1, wherein the proportion of superalloy powder return is 20-30%.
CN202211575142.1A 2022-12-08 2022-12-08 Method for preparing master alloy by remelting and recovering high-temperature alloy powder Pending CN115852184A (en)

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Citations (4)

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Publication number Priority date Publication date Assignee Title
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CN114472885A (en) * 2022-04-18 2022-05-13 中航迈特粉冶科技(北京)有限公司 Recycling method of metal powder return
CN114855009A (en) * 2022-04-20 2022-08-05 中航上大高温合金材料股份有限公司 Vacuum induction smelting process for smelting alloy by using high-proportion returning charge

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109402428A (en) * 2018-10-26 2019-03-01 北京科技大学 A kind of preparation method of high cleanliness powder metallurgy high-temperature alloy master alloy
WO2021036226A1 (en) * 2019-08-28 2021-03-04 北京钢研高纳科技股份有限公司 Large-size high-niobium and high-temperature 706 alloy ingot and smelting process thereof
CN114472885A (en) * 2022-04-18 2022-05-13 中航迈特粉冶科技(北京)有限公司 Recycling method of metal powder return
CN114855009A (en) * 2022-04-20 2022-08-05 中航上大高温合金材料股份有限公司 Vacuum induction smelting process for smelting alloy by using high-proportion returning charge

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