CN111690834A - Preparation method of nickel-based high-temperature alloy with gradient oxygen content - Google Patents

Preparation method of nickel-based high-temperature alloy with gradient oxygen content Download PDF

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CN111690834A
CN111690834A CN202010320369.6A CN202010320369A CN111690834A CN 111690834 A CN111690834 A CN 111690834A CN 202010320369 A CN202010320369 A CN 202010320369A CN 111690834 A CN111690834 A CN 111690834A
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oxygen content
gradient
alloy
female
oxide
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于连旭
段修涛
王晓蓉
缪晓宇
马步洋
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Nanjing Guore Metal Materials Research Institute Co ltd
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Nanjing Guore Metal Materials Research Institute Co ltd
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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
    • 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
    • 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
    • C22C19/057—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being less 10%

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  • Engineering & Computer Science (AREA)
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  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention relates to a preparation method of an alloy, in particular to a preparation method of a nickel-based high-temperature alloy with gradient oxygen content, and belongs to the technical field of alloy smelting. The invention adopts a method of vacuum induction melting master alloy, selecting special oxide, and adding the oxide to release dissolved oxygen in inert atmosphere. The method has simple process, and can prepare the high-temperature alloy material with basically constant nitrogen content and monotonously changing oxygen content gradient. The oxygen content in the alloy is artificially controlled to be in gradient distribution, and experimental basis is provided for researching the influence of the oxygen content on the material.

Description

Preparation method of nickel-based high-temperature alloy with gradient oxygen content
Technical Field
The invention relates to a preparation method of an alloy, in particular to a preparation method of a nickel-based high-temperature alloy with gradient oxygen content, and belongs to the technical field of alloy smelting.
Background
The indexes of the content of oxygen (O) and nitrogen (N) of gas elements of special alloys applied in complex fields such as high-temperature alloys and the like are generally strict, so that a master alloy material is prepared by using high-purity raw materials through vacuum induction melting. When producing parts, cutting a proper amount of master alloy, then casting into a casting after vacuum induction melting. From the viewpoint of scientific research, the systematic research on the influence of the oxygen content on the material requires the preparation of an alloy material with stable N content and other main elements and gradient oxygen content. However, in the vacuum induction melting process, O is very easy to form carbon monoxide gas (CO) with carbon (C) and the like in the alloy and volatile oxides are removed from the alloy, and N is also removed along with CO bubbles, generally O, N is reduced synchronously, and oxygen is difficult to control to be in gradient distribution.
Disclosure of Invention
The invention aims to provide a preparation method of a nickel-based high-temperature alloy with gradient oxygen content aiming at the defect that oxygen in the alloy can not be distributed in a gradient manner in the prior art, so as to obtain an alloy material with basically fixed nitrogen content and monotonously changing oxygen content gradient.
The invention solves the technical problem by the following technical scheme: a preparation method of a nickel-based superalloy with gradient oxygen content comprises the following steps:
firstly, preparing a master alloy by using a vacuum induction melting technology, and testing the O content O in the master alloy by adopting an infrared methodFemale(wt%) making the oxygen content of the master alloy below the minimum value of the design gradient;
second, selecting MxOy with chemical formula kChemistryCalculating the oxygen content as (16 × y/(16 × y + M × x)), wherein M is the atomic weight of M element, and oxide with the melting point lower than 1550 ℃ of refining temperature is used as the oxygen increasing agent;
thirdly, smelting according to a die, and cutting the equal weight MFemale(g) The quantity of the same furnace mother alloy material is designed gradient interval;
fourthly, remelting the material, carrying out an oxidizer burning loss test, and adding the weight M of the oxideOxide compound(g) According to self-closureActual oxygen content of gold OSeed of Japanese apricotDetermining the oxygen yield v of the oxide, irrespective of the deoxidation of the remelted mother alloyIs collectedPercent, the formula is
vIs collected＝MFemale·(OSeed of Japanese apricot-OFemale)/(MOxide compound·kChemistry)·100％；
Fifthly, the target design value of the O content is ODesign of(wt%) based on the weight M of the remelted alloy chargeFemale(g) Calculating the weight M of the oxide to be addedOxide compound(g) The relation formula of oxygen content conservation obtained according to the oxygen content yield is
ODesign of·MFemale＝MOxide compound·kChemistry·vIs collected+OFemale·MFemale；
MOxide compound＝MFemale·(ODesign of-OFemale)/(kChemistry·vIs collected)；
Sixthly, M is weighedOxide compound(g) Preparing the oxide of (4) into a material bag;
and seventhly, melting and cleaning the master alloy raw material by adopting a conventional vacuum induction remelting process, introducing inert gas, adding a material bag, melting and cleaning, and directly pouring into a casting mold to obtain the oxygen gradient alloy material with basically fixed nitrogen content.
In order to achieve the purpose of the invention, the following experiments are carried out to screen suitable oxides, common oxides are shown in table 1, and the principle of selecting the oxides is as follows: (1) the oxide should be non-toxic and harmless. (2) The metal element cannot be an impurity element in the material, such as PbO, Bi2O3Etc. are not applicable. (3) If the melting point is above 1550 ℃ which is the refining temperature, the added oxides may remain foreign inclusions, such as TiO2、Ta2O5、NiO、Al2O3、Cr2O3And is not suitable for use. (4) WO3It is not suitable for use because it sublimates at 850 deg.C and volatilizes out. (5) FeO has a suitable melting point, but is highly transformed into Fe in air3O4The melting point is increased, and the method is not suitable for application, and the nickel-based alloy is not suitable for introducing iron content. The metal element should beThe elements of the main components of the high-temperature alloy do not fluctuate greatly after being added, and MoO is selected in the invention3As an oxygen increasing agent.
TABLE 1
Substance(s) Melting Point C Substance(s) Melting Point C Substance(s) Melting Point C
PbO 890 Nb2O5 1511 NiO 1980
MoO3 795 Fe3O4 1596 Al2O3 2045
FeO 1380 TiO2 1825 Cr2O3 2279
WO3 1470 Ta2O5 1877
In selecting MoO3Then, the yield of O after the oxide is added is also considered, and the yield of the fourth step is 3-15%. Based on the selection of the consideration of controlling the yield, argon Ar is filled into the vacuum environment before the oxide is added so as to inhibit the volatilization of the oxide; the material bag in the sixth step is prepared by sealing oxides in a base metal block or a master alloy block with one open end. The excessive negative pressure can cause potential safety hazard to equipment, the pressure of the invention is between-0.01 and-0.07 MPa, and the material bag is added before pouring.
The N content and other main elements in the alloy obtained by the method have small fluctuation, and the oxygen content presents certain gradient distribution.
The invention adopts vacuum induction remelting high-temperature alloy master alloy, reduces the power after refining the alloy, leads inert gas Ar gas to protect, leads the pressure to reach negative pressure of-0.01 to-0.07 MPa, and then adds MoO3，MoO3The adding amount is calculated according to the introduced oxygen yield of 3-10%, after standing for about 1 minute, the temperature is raised to the casting temperature, and the casting is carried out according to the conventional process. The method has simple process, and can prepare the high-temperature alloy material with basically constant nitrogen content and monotonously changing oxygen content gradient. The oxygen content in the alloy is artificially controlled to be in gradient distribution, and experimental basis is provided for researching the influence of the oxygen content on the material.
Drawings
FIG. 1 is a diagram illustrating dross formation in an alloy melt according to a first embodiment of the invention.
FIG. 2 is a diagram showing dross states of alloy melts in comparative examples.
Detailed Description
The preparation method of the oxygen gradient alloy comprises the following steps:
(1) preparing a master alloy by adopting vacuum induction melting, and testing the O content O in the master alloy by adopting an infrared methodFemale(wt%) to ensure that the oxygen content gradient of the master alloy is below the minimum value of the designed gradient O content alloy.
(2) Selecting proper high-purity oxide material, and calculating the oxygen content to be k according to the chemical formula of the oxideChemistry。
(3) Smelting according to a die, cutting and taking the equal weight MFemale(g) The quantity of the same furnace mother alloy material is designed gradient interval.
(4) Remelting the material, carrying out a pseudo-selective oxide burn-out test, adding the weight M of the oxideOxide compound(g) According to the actual oxygen content O of the self-alloySeed of Japanese apricotThe yield v of the oxide oxygen is determined without considering the deoxidation condition of the remelting of the master alloy (the remelting process of each furnace is the same, the deoxidation condition is the same)Is collected。
vIs collected＝MFemale·(OSeed of Japanese apricot-OFemale)/(MOxide compound·kChemistry)
(5) The target design value of the O content is ODesign of(wt%). According to the weight M of the remelted alloy materialFemale(g) Calculating the weight M of the oxide to be addedOxide compound(g) Obtaining the relation of oxygen content conservation according to the oxygen content burning loss rate as follows:
Odesign of·MFemale＝MOxide compound·kChemistry·vIs collected+OFemale·MFemale；
MOxide compound＝MFemale·(ODesign of-OFemale)/(kChemistry·vIs collected)。
(6) Weighing MOxide compound(g) The oxide of (3) is sealed in a nickel block having one open end.
(7) And placing the coated oxide material into a feeder, melting and cleaning the mother alloy raw material by adopting a conventional vacuum induction remelting process, introducing argon protective atmosphere, adding the oxide material bag before pouring, and directly pouring the alloy material into a casting mould after melting and cleaning to prepare the oxygen gradient alloy material with basically fixed nitrogen content.
See in particular the examples below
Example 1
This example prepares a nickel-base superalloy with a gradient oxygen content as follows:
(1) the alloy contains Mo element, and MoO is selected3As an oxygen increasing agent, an alloy having an oxygen content of 16 × 3/(96+16 × 3) ═ 0.33 was designed according to the formula, and an oxygen gradient of 0.0015% and 0.0020% was designed.
(2) 60kg of K417G master alloy is vacuum induction smelted by an alumina crucible, the chemical composition is (Cr8.7, Co10.1, Mo3.15, Al5.4, Ti4.5, B0.013, V0.73, C0.16 and Ni residue), the content of O, N is tested, the O content is 0.0009 percent, and the N content is 0.0005 percent;
(3) a process test of the burning loss rate is carried out, 4.5kg of master alloy material is remelted according to a conventional remelting process, and argon is filled to-0.04 MPa. 0.4g of MoO is added in the later stage of refining3The obtained O content was 0.0012%, and the increment was 0.0002%, i.e., the yield was 10%.
(4) 6 ppm and 11ppm of O are needed to be added, two 5kg of sub-alloys are cut, the burning loss rate is 90 percent, and MoO is needed3The amount of (c) is 5000 x (0.0015% -0.0009%)/(0.33 x 10%)/(0.90 g) and 5000 x (0.0020% -0.0009%)/(0.33 x 10%)/(1.7 g). Sealed with Ni blocks and injected into a feeder.
(5) When remelting, after refining, regulating power to 10KW, introducing Ar gas for protection, controlling pressure in furnace to-0.05 MPa, injecting MoO into feeder3The Ni block of (1). After adding, the power is increased to 30KW to dissolve the oxide and the nickel block in the melt (as shown in figure 1), after maintaining for 1min, the power is reduced, and after the melt reaches the casting temperature of 1420 ℃, the casting is completed.
(6) Remelting a furnace alloy, and performing remelting and pouring according to a normal process;
(7) sampling, testing and analyzing: the oxygen content was 0.0009%, 0.0014% and 0.0019%, respectively. The nitrogen content was 0.0005%, 0.0006%, 0.0007%, and the dross state of the alloy melt was as shown in FIG. 1, and the alloy melt was uniform and free of dross.
Comparative example 1
The comparative example prepared a nickel-base superalloy as follows:
(1) using MoO3When the oxygen increasing agent is used, the content of the chemical formula O is 16/(16+55) ═ 0.23, and the sub-alloy with the gradient of increasing O of 20 ppm and 30ppm is prepared;
(2) the high-temperature alloy master alloy material is adopted, the chemical components are (Cr9.0, Co10.0, Mo3.15, Al5.4, Ti4.5, B0.015, V0.75, C0.16 and Ni residue), the content of O, N is tested, the content of O is 0.0011 percent, and the content of N is 0.0011 percent;
(3) about 4.5kg of master alloy material is taken, and MoO is added according to the oxygen burning loss rate of 90 percent3The amounts of 2.6g and 4.0g, respectively, were sealed with Ni blocks and charged into a feeder.
(4) When remelting, after refining, the power is reduced to 10KW, the vacuum environment is maintained to be less than 1Pa, and a feeder injects Ni blocks with NiO. After adding, increasing power to 30KW to dissolve oxide and nickel block in the melt, maintaining for 1min, reducing power, and finishing pouring after the melt reaches the pouring temperature of 1420 ℃.
(5) Sampling, testing and analyzing: the oxygen content was 0.0012% and 0.0017%, respectively, and the gradient of the oxygen content and the design deviation were large, indicating that it is not advantageous to obtain a controllable oxygen gradient if the vacuum level is maintained high after the addition of the oxide.
Comparative example 2
The comparative example prepared a nickel-base superalloy as follows:
(1) when NiO is used as an oxygen increasing agent, the content of the chemical formula O is 16/(16+59) ═ 0.21, and the sub-alloys with the O increasing gradient of 20 ppm, 30ppm and 40ppm are prepared;
(2) the high-temperature alloy master alloy material is adopted, the chemical components are (Cr9.0, Co10.0, Mo3.15, Al5.4, Ti4.5, B0.015, V0.75, C0.16 and Ni residue), the content of O, N is tested, the content of O is 0.0012 percent, and the content of N is 0.0011 percent;
(3) about 4.5kg of master alloy material was charged with 3.4g, 6.2g and 9.0g of Ni0, respectively, calculated on the basis of the oxygen burnout rate of 90%, sealed with Ni blocks and charged into a charging hopper. .
(4) When remelting, after refining, the power is reduced to 10KW, Ar gas is introduced for protection, and when the pressure in the furnace is controlled to be increased to-0.05 MPa, a feeder injects Ni blocks with NiO. After adding, increasing power to 30KW to dissolve oxide and nickel block in the melt, maintaining for 1min, reducing power, and finishing pouring after the melt reaches the pouring temperature of 1420 ℃.
(5) Sampling, testing and analyzing: the oxygen contents were 0.0013%, 0.0014%, and 0.0011%, respectively, and an oxygen gradient alloy could not be prepared, and the oxygen content and the addition amount were not related. The oxide has high melting point and is not easy to melt in the alloy melt in the preparation process, so that a large amount of dross (shown in figure 2) exists on the surface of the alloy, and the oxide floats on the surface of the melt.
In addition to the above, other embodiments of the present invention are possible. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.

Claims (7)

1. A preparation method of a nickel-based superalloy with gradient oxygen content comprises the following steps:
firstly, preparing a master alloy by using a vacuum induction melting technology, and testing the O content O in the master alloy by adopting an infrared methodFemale(wt%) making the oxygen content of the master alloy below the minimum value of the design gradient;
second, selecting MxOy with chemical formula kChemistryCalculating the oxygen content as (16 × y/(16 × y + M × x)), wherein M is the atomic weight of M element, and oxide with the melting point lower than 1550 ℃ of refining temperature is used as the oxygen increasing agent;
thirdly, smelting according to a die, and cutting the equal weight MFemale(g) The quantity of the same furnace mother alloy material is designed gradient interval;
fourthly, remelting the material, carrying out an oxidizer burning loss test, and adding the weight M of the oxideOxide compound(g) According to the actual oxygen content O of the self-alloySeed of Japanese apricotDetermining the oxide irrespective of the deoxidation condition of the remelted mother alloyYield of oxygen vIs collectedPercent, the formula is
vIs collected＝MFemale·(OSeed of Japanese apricot-OFemale)/(MOxide compound·kChemistry)·100％；
Fifthly, the target design value of the O content is ODesign of(wt%) based on the weight M of the remelted alloy chargeFemale(g) Calculating the weight M of the oxide to be addedOxide compound(g) The relation formula of oxygen content conservation obtained according to the oxygen content yield is
ODesign of·MFemale＝MOxide compound·kChemistry·vIs collected+OFemale·MFemale；
MOxide compound＝MFemale·(ODesign of-OFemale)/(kChemistry·vIs collected)；
Sixthly, M is weighedOxide compound(g) Preparing the oxide of (4) into a material bag;
and seventhly, melting and cleaning the master alloy raw material by adopting a conventional vacuum induction remelting process, introducing inert gas, adding a material bag, melting and cleaning, and directly pouring into a casting mold to obtain the oxygen gradient alloy material with basically fixed nitrogen content.
2. The method of preparing a nickel-base superalloy with a gradient oxygen content of claim 1, comprising: the oxide of the second step is MoO3。
3. The method of preparing a nickel-base superalloy with a gradient oxygen content of claim 1, comprising: the yield of the fourth step is 3-15%.
4. The method of claim 1 for preparing a nickel-base superalloy with a gradient oxygen content, comprising: the material bag in the sixth step is prepared by sealing oxides in a base metal block or a master alloy block with one open end.
5. The method of preparing a nickel-base superalloy with a gradient oxygen content of claim 1, comprising: in the seventh step, the inert gas is argon, and the pressure is between-0.01 MPa and-0.07 MPa.
6. Method for the preparation of a nickel-base superalloy with a gradient oxygen content according to claim 4, characterized in that: the packet is added before casting.
7. The method of preparing a nickel-base superalloy with a gradient oxygen content of claim 1, comprising: the N content and other main elements in the obtained alloy have small fluctuation, and the oxygen content presents certain gradient distribution.
CN202010320369.6A 2020-04-22 2020-04-22 Preparation method of nickel-based high-temperature alloy with gradient oxygen content Pending CN111690834A (en)

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Publication number Priority date Publication date Assignee Title
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JPH04236732A (en) * 1991-01-17 1992-08-25 Mitsubishi Heavy Ind Ltd Method for controlling oxygen content in melting titanium and titanium alloy with electron beam
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CN103333991A (en) * 2013-07-03 2013-10-02 东北大学 Ferritic alloy for adjusting content of dissolved oxygen in molten steel, and preparation and usage method thereof
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