CN114635049B - Production method of high-purity nickel-niobium intermediate alloy - Google Patents

Production method of high-purity nickel-niobium intermediate alloy Download PDF

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CN114635049B
CN114635049B CN202210313688.3A CN202210313688A CN114635049B CN 114635049 B CN114635049 B CN 114635049B CN 202210313688 A CN202210313688 A CN 202210313688A CN 114635049 B CN114635049 B CN 114635049B
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nickel
niobium
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intermediate alloy
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CN114635049A (en
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孙岳来
王晓蓉
贾明
邓军
马步洋
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Metalink Special Alloys Corp
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/02—Alloys based on vanadium, niobium, or tantalum

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Abstract

The invention provides a production method of a high-purity nickel-niobium intermediate alloy. The invention adopts the nickel-niobium intermediate alloy produced by the aluminothermic reduction process as the raw material and adopts a vacuum induction furnace to produce the high-purity nickel-niobium intermediate alloy. The method comprises the following specific steps: (1) charging: vacuumizing, and adding the nickel-niobium intermediate alloy produced by the thermal reduction process into a feeding chamber; (2) melting period: heating the furnace material to be clear; (3) refining: starting refining when the temperature reaches a refining temperature; (4) deslagging: adding a slagging agent to remove slag; (5) pouring: alloy casting is performed when the temperature reaches the casting temperature. The nickel-niobium intermediate alloy produced by the method has good component consistency, low inclusion content and low content of harmful gas elements such as oxygen/nitrogen, and solves the problems of alloy component segregation, more inclusions and non-uniform oxygen elements produced by the aluminothermic reduction process.

Description

Production method of high-purity nickel-niobium intermediate alloy
Technical Field
The invention belongs to the field of vacuum metallurgy, and particularly relates to a production method of a high-purity nickel-niobium intermediate alloy.
Background
With the continuous development of industries such as aeroengines, gas turbines, petrochemical industry and the like, the usage amount of high-temperature alloy is increased year by year. The demand for high temperature alloy raw materials is also increasing. Niobium is an important strengthening element of the high-temperature alloy, and the niobium is added into the high-temperature alloy and mainly enters a gamma' phase to form Ni 3 (Al, Ti, Nb), the increased number of gamma 'phase, increased gamma' phase inversion domain boundary, increased gamma 'phase particle size, and increased order, thereby enhancing the precipitation strengthening effect of gamma' phase.
Because the pure niobium raw material has the problems of high melting point (the melting point is 2468 ℃), difficult purification, high price, easy segregation in use and the like, a nickel-niobium intermediate alloy (NiNb) with lower melting point is usually selected in the production of high-temperature alloy 65 Melting point 1291 ℃ C.) as the starting material. At present, most of nickel-niobium master alloys are produced by adopting an aluminothermic reduction process, for example, in patent applications with publication numbers of CN104141083A, CN103255330A and the like, aluminum powder is adopted as a reducing agent to react with niobium pentoxide and nickel oxideThe alloy produced by the original reaction has the problems of component segregation, more inclusions and non-uniform oxygen elements. Because of the inheritance of the material, the niobium-containing high-temperature alloy produced by adopting the raw material can bring more inclusions, so that the yield of high-temperature alloy parts is reduced, and meanwhile, the component segregation of the niobium element in the raw material can also cause the chemical components and the design components of the smelted high-temperature alloy to be different, so that the alloy performance is unstable, and the tissue stability and the service life of the high-temperature alloy are reduced. The patent application with publication number CN104988341A uses pure nickel and high-purity niobium as raw materials to produce nickel-niobium alloy through vacuum induction furnace, but it has the problem of high cost of raw materials and is difficult to expand the market.
Based on the above, in order to improve the component uniformity of the nickel-niobium master alloy and reduce the inclusion content and the content of oxygen and nitrogen elements, it is necessary to design and develop a production method of a high-purity nickel-niobium master alloy.
Disclosure of Invention
The invention aims to provide a production method of a high-purity nickel-niobium intermediate alloy, which can improve the component uniformity of the nickel-niobium intermediate alloy and reduce the inclusion content and the content of oxygen and nitrogen elements.
In order to achieve the purpose, the invention provides the following technical scheme:
a method of producing a high purity nickel niobium master alloy, performed in a vacuum induction furnace, comprising the steps of:
(1) charging: closing the furnace and vacuumizing, and adding nickel-niobium intermediate alloy from the feeding chamber when the vacuum degree is less than or equal to 2 Pa;
(2) melting period: heating the furnace materials until the furnace materials are completely melted;
(3) and (3) refining period: after clearing, heating to the refining temperature and starting refining for a period of time, wherein the vacuum degree is kept to be less than or equal to 2 Pa;
(4) deslagging: after refining, cutting off power, cooling to a deslagging temperature, filling argon, adding a deslagging agent from a feeding chamber, and keeping for a period of time;
(5) and (3) pouring period: before casting, vacuumizing, the vacuum degree is less than or equal to 5Pa, performing alloy casting when the temperature reaches the casting temperature, cooling in a furnace to a certain temperature, and then breaking the air to take ingots.
Preferably, the nickel niobium master alloy used is a nickel niobium master alloy produced by an aluminothermic reduction process.
Further, the mass percentage of the niobium element of the nickel-niobium intermediate alloy added in the step (1) is 60-68%.
In some schemes, in the step (3), the refining temperature is 1500-1560 ℃, and the refining time is 10-20 min.
In some embodiments, in the step (4), the deslagging temperature is 1440 ℃ to 1480 ℃, argon gas is filled into the furnace at 10000Pa to 30000Pa, and the holding time is 5min to 10 min.
In other embodiments, in the step (4), the added slag removing agent is a nickel-calcium intermediate alloy, the addition amount of calcium element is 0.1-1.0% of the weight of the high-purity nickel-niobium intermediate alloy, and the calcium content in the nickel-calcium intermediate alloy is 5-50%.
Preferably, in the step (5), the casting temperature is 1480-1520 ℃.
More preferably, in step (5), the pre-dummy nickel-niobium master alloy ingot should be cooled to below 300 ℃.
Compared with the prior art, the nickel-niobium intermediate alloy produced by the production method of the high-purity nickel-niobium intermediate alloy has good component consistency, low inclusion content and low content of harmful gas elements such as oxygen/nitrogen, and solves the problems of alloy component segregation, more inclusions and uneven oxygen elements produced by an aluminothermic reduction process.
Specifically, the method of the invention has the following beneficial effects:
1. the vacuum induction melting can effectively improve the component segregation of the nickel-niobium intermediate alloy produced by the aluminothermic reduction process, and simultaneously can reduce the content of impurity elements such as Pb, Sb, Se, Te, Tl and the like with high saturated vapor pressure under the high vacuum condition, thereby improving the purity of the nickel-niobium intermediate alloy.
2. The invention provides a nickel-niobium intermediate alloy deslagging process, which can effectively reduce the content of impurities in the alloy.
3. The nickel-niobium intermediate alloy produced by the method has the advantages of good component consistency, low inclusion content and low content of harmful gas elements such as oxygen/nitrogen, and the like, and can improve the yield and prolong the service life of high-temperature alloy castings.
4. The method has the advantages of low cost, simple process and easy operation, and can realize industrial stable production and popularization.
Drawings
FIG. 1 is a photomicrograph (x 100) of the texture of a nickel niobium master alloy produced by a thermite reduction process;
FIG. 2 is a photomicrograph (x 100) of the microstructure of a nickel niobium master alloy produced using the method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to specific embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a production method of a high-purity nickel-niobium intermediate alloy, which provides a raw material with stable components and low impurity element content for high-temperature alloy production.
The method of the invention adopts the nickel-niobium intermediate alloy produced by the aluminothermic reduction process as the raw material and adopts a vacuum induction furnace to produce the high-purity nickel-niobium intermediate alloy.
In one representative embodiment, the specific process steps of the method of the present invention are as follows:
(1) charging: closing the furnace and vacuumizing, and when the vacuum degree is less than or equal to 2Pa, adding nickel-niobium intermediate alloy with the mass percentage of niobium element of 60-68% produced by an aluminothermic reduction process into a feeding chamber;
(2) melting period: heating the furnace materials until the furnace materials are completely melted;
(3) and (3) refining period: after clearing, heating to 1500-1560 ℃ and starting refining, wherein the refining time depends on the capacity of a vacuum induction furnace, the refining time of a 250Kg vacuum induction furnace is 10-20 min, and the vacuum degree is less than or equal to 2 Pa;
(4) deslagging: and after refining is finished, power is cut off, the temperature is reduced to 1440-1480 ℃, argon is filled at 10000-30000 Pa, and a slag removing agent is added from a feeding chamber and kept for 5-10 min. The slag removing agent is a nickel-calcium intermediate alloy, the addition amount of calcium is 0.1-1.0% of the weight ratio of the alloy, and the calcium content in the nickel-calcium intermediate alloy is 5-50%;
(5) and (3) pouring period: vacuumizing before casting, wherein the vacuum degree is less than or equal to 5Pa, performing alloy casting when the temperature reaches 1480-1520 ℃, cooling in a furnace to below 300 ℃, and then breaking the air to obtain ingots.
The nickel-niobium intermediate alloy produced by the production method of the high-purity nickel-niobium intermediate alloy has good component consistency, low inclusion content and low content of harmful gas elements such as oxygen/nitrogen, and solves the problems of segregation of alloy components, more inclusions and non-uniform oxygen elements produced by an aluminothermic reduction process.
The present invention will be described in further detail with reference to specific examples. In the embodiment, a nickel-niobium intermediate alloy with the mass percentage of niobium element of 60-68% produced by an aluminothermic reduction process is used as a raw material, and a 250Kg vacuum induction furnace is adopted to produce the high-purity nickel-niobium intermediate alloy.
Example 1:
the specific implementation steps are as follows:
1. charging: closing the furnace and vacuumizing, and when the vacuum degree is less than or equal to 2Pa, adding nickel-niobium intermediate alloy with the niobium element mass percentage of 60-68% produced by an aluminothermic reduction process into a feeding chamber, wherein the specific chemical components are shown in Table 1.
2. Melting period: the power is sent and the temperature is raised until the furnace burden is melted and cleared.
3. And (3) refining period: after clearing, heating to 1500 ℃ and then starting refining, wherein the refining time depends on the capacity of the vacuum induction furnace, the refining time is 20min, and the vacuum degree is less than or equal to 2 Pa.
4. Deslagging: after refining, the power is cut off and the temperature is reduced to 1440 ℃, argon is filled into 10000Pa, and a deslagging agent is added from a feeding chamber and kept for 5 min. The slag removing agent is nickel-calcium intermediate alloy, the addition amount of calcium element is 0.1-1.0% of the weight ratio of the alloy, and the calcium content in the nickel-calcium intermediate alloy is 5% -50%
5. And (3) pouring period: before casting, vacuumizing, vacuum degree is less than or equal to 5Pa, alloy casting is carried out when the temperature reaches 1480 ℃, and ingot taking is carried out after cooling in a furnace to below 300 ℃.
Then, the alloy components were sampled from the upper, middle, and lower portions of the ingot, respectively, and the specific results are shown in table 2.
TABLE 1 chemical composition (wt%) of Ni-Nb master alloy produced by aluminothermic reduction process
Element(s) Nb Ni Al Si Fe P Pb Bi
Raw material 1-upper part 66.52 Surplus 0.36 0.034 0.022 0.0048 <0.001 <0.001
Feedstock 1-middle part 67.01 Surplus 0.03 0.033 0.018 0.0039 <0.001 <0.001
Raw material 1-lower part 68.25 Surplus 0.08 0.035 0.02 0.0045 <0.001 <0.001
Element(s) Sb Se Te Tl C S O N
Raw material 1-upper part 0.0017 <0.001 <0.001 <0.001 0.0036 0.0018 0.260 0.012
Feedstock 1-middle part 0.0015 <0.001 <0.001 <0.001 0.0042 0.0015 0.037 0.011
Raw material 1-lower part 0.0020 <0.001 <0.001 <0.001 0.0056 0.0022 0.11 0.014
Table 2 chemical composition (wt%) of the nickel niobium master alloy produced by the process of example 1
Element(s) Nb Ni Al Si Fe P Pb Bi
Example 1-upper part 67.06 Surplus 0.012 0.037 0.016 0.0041 <0.0005 <0.00005
Example 1 middle part 66.92 Surplus 0.013 0.036 0.018 0.0036 <0.0005 <0.00005
Example 1 lower part 67.07 Surplus 0.010 0.037 0.017 0.0019 <0.0005 <0.00005
Element(s) Sb Se Te Tl C S O N
Example 1-Upper part <0.0005 <0.0005 <0.0001 <0.0001 0.0032 0.0003 0.019 0.0069
Example 1 middle part <0.0005 <0.0005 <0.0001 <0.0001 0.0030 0.0002 0.017 0.0067
Example 1 lower part <0.0005 <0.0005 <0.0001 <0.0001 0.0029 0.0002 0.016 0.0066
Example 2:
the specific implementation steps are as follows:
1. charging: closing the furnace and vacuumizing, and when the vacuum degree is less than or equal to 2Pa, adding nickel-niobium intermediate alloy with the niobium element mass percentage of 60-68% produced by the aluminothermic reduction process into the feeding chamber, wherein the specific chemical components are shown in Table 3.
2. Melting period: the power is sent and the temperature is raised until the furnace burden is melted and cleared.
3. And (3) refining period: after clearing, heating to 1560 ℃ and starting refining, wherein the refining time depends on the capacity of a vacuum induction furnace, the refining time of a 250Kg vacuum induction furnace is 10min, and the vacuum degree is less than or equal to 2 Pa.
4. Deslagging: after refining, cutting off power, cooling to 1480 deg.C, charging argon gas 30000Pa, adding slag-removing agent from the charging chamber, and maintaining for 10 min. The slag removing agent is a nickel-calcium intermediate alloy, the addition amount of calcium is 0.1-1.0% of the weight ratio of the alloy, and the calcium content in the nickel-calcium intermediate alloy is 5-50%.
5. And (3) pouring period: before casting, vacuumizing, vacuum degree is less than or equal to 5Pa, alloy casting is carried out when the temperature reaches 1520 ℃, and ingot taking is carried out after cooling in a furnace to below 300 ℃.
Then, the alloy compositions were sampled from the upper, middle and lower portions of the ingot, and the results are shown in table 4.
TABLE 3 chemical composition (wt%) of Ni-Nb master alloy produced by aluminothermic reduction process
Element(s) Nb Ni Al Si Fe P Pb Bi
Raw material 2-upper part 66.75 Surplus 0.660 0.052 0.025 0.0052 <0.001 <0.001
Feedstock 2-middle part 65.86 Surplus 0.042 0.029 0.031 0.0038 <0.001 <0.001
Raw material 2-lower part 64.52 Surplus 0.124 0.031 0.038 0.0034 <0.001 <0.001
Element(s) Sb Se Te Tl C S O N
Raw material 2-upper part 0.0044 <0.001 <0.001 <0.001 0.0072 0.0016 0.17 0.06
In the raw material 2-Part (A) 0.0012 <0.001 <0.001 <0.001 0.0061 0.0012 0.02 0.0058
Raw material 2-lower part 0.0018 <0.001 <0.001 <0.001 0.0052 0.0020 0.08 0.015
Table 4 chemical composition (wt%) of the nickel niobium master alloy produced by the process of example 2
Element(s) Nb Ni Al Si Fe P Pb Bi
Example 2-upper part 65.85 Surplus 0.035 0.043 0.028 0.0038 <0.0005 <0.00005
Example 2 middle part 65.76 Surplus 0.033 0.043 0.031 0.0039 <0.0005 <0.00005
Example 2 lower part 65.94 Surplus 0.038 0.042 0.029 0.0038 <0.0005 <0.00005
Element(s) Sb Se Te Tl C S O N
Example 2-upper part <0.0005 <0.0005 <0.0001 <0.0001 0.0053 0.0002 0.015 0.0042
Example 2 middle part <0.0005 <0.0005 <0.0001 <0.0001 0.0050 0.0003 0.014 0.0041
Example 2 lower part <0.0005 <0.0005 <0.0001 <0.0001 0.0048 0.0002 0.012 0.0038
Comparative analysis was performed from the results of examples 1 and 2. As shown in tables 1 and 3, the nickel-niobium master alloy produced by the thermite reduction process has a problem that Nb element is segregated and impurity elements such as Al, O, and N are not uniform. After the smelting by the method of the invention is adopted, as can be seen from tables 2 and 4, the segregation problem of the Nb element is solved, the component consistency of different parts of impurity elements such as Al, O, N and the like is better, and the impurity elements such as Al, S, O, N, Sb and the like are greatly reduced.
Comparing the metallographic phase of the nickel-niobium intermediate alloy produced by the aluminothermic reduction process with that of the nickel-niobium intermediate alloy produced by the method of the present invention, as shown in fig. 1 and 2, the nickel-niobium intermediate alloy produced by the aluminothermic reduction process contains more inclusions, while the nickel-niobium intermediate alloy produced by the method of the present invention contains fewer inclusions, which indicates that the process of the present invention can significantly improve the purity of the nickel-niobium intermediate alloy.
In conclusion, the nickel-niobium intermediate alloy produced by the method has good component consistency, low inclusion content and low content of harmful gas elements such as oxygen/nitrogen, and solves the problems of alloy component segregation, more inclusions and non-uniform oxygen element produced by the aluminothermic reduction process.
The details of the present invention are well known to those skilled in the art.
Finally, it is to be noted that: although the present invention has been described in detail with reference to examples, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (6)

1. A method for producing a high purity nickel niobium master alloy, performed in a vacuum induction furnace, characterized in that it comprises the following steps:
(1) charging: closing the furnace and vacuumizing, and adding nickel-niobium intermediate alloy from a feeding chamber when the vacuum degree is less than or equal to 2 Pa;
(2) melting period: heating the furnace material to be clear;
(3) and (3) refining period: after clearing, heating to the refining temperature and starting refining for a period of time, wherein the vacuum degree is kept to be less than or equal to 2 Pa;
(4) deslagging: after refining, cutting off power, cooling to a deslagging temperature, filling argon, adding a deslagging agent from a feeding chamber, and keeping for a period of time;
(5) and (3) pouring period: vacuumizing before casting, wherein the vacuum degree is less than or equal to 5Pa, performing alloy casting when the temperature reaches the casting temperature, cooling in a furnace to a certain temperature, then breaking the air to take ingots,
in the step (4), the deslagging temperature is 1440-1480 ℃, argon is filled into the furnace at 10000-30000 Pa, the holding time is 5-10 min, the added deslagging agent is a nickel-calcium intermediate alloy, the addition amount of calcium is 0.1-1.0% of the weight of the high-purity nickel-niobium intermediate alloy, and the calcium content in the nickel-calcium intermediate alloy is 5-50%.
2. The method for producing a high purity nickel niobium master alloy according to claim 1, wherein the nickel niobium master alloy used is a nickel niobium master alloy produced by an aluminothermic reduction process.
3. The method for producing the high-purity nickel-niobium master alloy as claimed in claim 1, wherein the mass percentage of the niobium element in the nickel-niobium master alloy added in the step (1) is 60-68%.
4. The method for producing the high-purity nickel-niobium intermediate alloy as claimed in claim 1, wherein in the step (3), the refining temperature is 1500 ℃ to 1560 ℃, and the refining time is 10min to 20 min.
5. The method for producing a high purity nickel-niobium master alloy according to claim 1, wherein in the step (5), the casting temperature is 1480 to 1520 ℃.
6. The method for producing a high purity nickel niobium master alloy according to claim 1, wherein in the step (5), the nickel niobium master alloy ingot before the blank is cooled to 300 ℃ or less.
CN202210313688.3A 2022-03-28 2022-03-28 Production method of high-purity nickel-niobium intermediate alloy Active CN114635049B (en)

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CN103255330B (en) * 2013-04-28 2015-07-08 江苏美特林科特殊合金有限公司 Nickel-niobium intermediate alloy and preparation method thereof
CN104674065A (en) * 2013-11-29 2015-06-03 大连融德特种材料有限公司 Production method of high-purity nickel niobium alloy
CN104988341A (en) * 2015-06-19 2015-10-21 承德天大钒业有限责任公司 Preparation method of nickel niobium alloy
CN113528924B (en) * 2021-07-23 2022-04-15 承德天大钒业有限责任公司 Nickel-niobium-chromium intermediate alloy and preparation method thereof

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