CN111910095B - Smelting preparation method of nickel-based single crystal superalloy master alloy - Google Patents
Smelting preparation method of nickel-based single crystal superalloy master alloy Download PDFInfo
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Abstract
The invention discloses a smelting preparation method of a nickel-based single crystal superalloy master alloy, and belongs to the technical field of alloy smelting. Putting raw material elements with higher melting points into a melting crucible in sequence, and firstly carrying out primary melting, furnace shaking and refining; then adding Ni-C and Al, and then carrying out secondary smelting and furnace shaking; and finally, carrying out third smelting and fourth smelting, and pouring to obtain the nickel-based single crystal superalloy master alloy. The nickel-based single crystal superalloy master alloy obtained by the method is easy to accurately control the alloy components, and meanwhile, the content of N, O and other elements in the alloy can be effectively reduced, and the potential of the alloy is fully exerted.
Description
Technical Field
The invention belongs to the technical field of high-temperature alloy smelting, and particularly relates to a smelting preparation method of a nickel-based single-crystal high-temperature alloy master alloy.
Background
The nickel-based single crystal superalloy is a main preparation material of high-pressure turbine blades of aeroengines and gas turbines. Along with the development of the nickel-based single crystal superalloy, the nickel-based single crystal superalloy has higher and higher alloying degree, the components of the nickel-based single crystal superalloy are easy to form segregation, and trace elements are difficult to control; in particular to a high-generation nickel-base single crystal superalloy, the high-temperature performance of which is more sensitive to gas content and impurity element content. Therefore, the single crystal superalloy master alloy has strict standards, requires accurate control of alloy elements, and removes harmful impurity elements such as O, N, S and the like as much as possible.
Vacuum induction melting is a main method for preparing the nickel-based single crystal superalloy master alloy, and the melting, refining, alloying and casting of the alloy are carried out under the vacuum condition, so that the inclusions caused by alloy oxidation in the high-temperature melting process can be reduced. Al is the main precipitation strengthening element in the nickel-based single crystal superalloy, the melting point of the Al is only 660 ℃, the melting temperature of the nickel-based single crystal superalloy usually exceeds 1500 ℃, so that the Al is seriously volatilized and burnt at high temperature, and particularly, the sputtering of a melt can be caused by improper feeding sequence.
The high-generation nickel-base single crystal superalloy contains a large amount of high refractory elements (such as W melting point 3430 ℃, Re melting point 3180 ℃, Ta melting point 2996 ℃ and Mo melting point 2617 ℃), and a higher smelting temperature is required to be loaded when the alloy is fully melted to obtain a uniform melt structure; meanwhile, the higher vacuum degree during alloy smelting can promote the discharge of part of gas elements. However, the volatilization of Al is also accelerated at a high refining temperature, and the volatilization of elements having a high saturated vapor pressure, such as Cr and Al, is accelerated at a high refining temperature of 1650 ℃ in patent publication No. CN 1360071A. In addition, long-term high-temperature smelting can aggravate the reaction between alloy elements and a smelting crucible, and introduce impurities, so that the fatigue and the durability of the alloy are obviously reduced, and the service life of the crucible is also shortened. Therefore, on the premise of not increasing the cost of alloy raw materials, how to effectively reduce the elimination of light elements and accurately control volatile elements to improve the metallurgical quality of the nickel-based single crystal superalloy has important significance for improving the performance of the single crystal superalloy.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for preparing a nickel-based single crystal superalloy master alloy by smelting, which can improve the metallurgical quality of the alloy.
The technical scheme adopted by the invention for solving the technical problems is as follows: a smelting preparation method of a nickel-based single crystal superalloy master alloy is characterized by comprising the following steps:
(1) the method comprises the following steps of charging for the first time, charging raw materials according to target nickel-based single crystal superalloy components, wherein the raw materials in a melting crucible sequentially comprise, from bottom to top, 60-70% of nickel, 100% of cobalt, 100% of chromium, 100% of tungsten, 100% of molybdenum, 100% of rhenium, 100% of ruthenium, 100% of niobium, 100% of hafnium, 100% of tantalum and 30-40% of nickel;
(2) smelting for the first time, initially heating to 1500-1540 ℃, keeping the temperature for 5-10 minutes, and then shaking the furnace for 3-5 times; continuously heating to 1600-1620 ℃, and preserving the heat for 3-5 minutes to finish refining; cooling to 1550-1570 ℃, preserving heat for 5-10 minutes, and then cutting off power to cool to complete solidification to complete first smelting;
(3) and (3) charging for the second time: 100% nickel-carbon alloy (Ni-C) and 100% aluminum were charged into a melting crucible, followed by charging 10 in a vacuum induction melting furnace3～104Pa argon gas;
(4) smelting for the second time: heating to 1520-1540 ℃, preserving heat for 3-5 minutes, and shaking the furnace for 3-5 times; then, cutting off power and reducing the temperature to 1370-1390 ℃ to form a film, and finishing the second smelting;
(5) smelting for the third time: heating to 1520-1540 ℃ in 5-8 minutes, preserving heat for 3-5 minutes, and shaking the furnace for 3-5 times; then, cutting off power and reducing the temperature to 1370-1390 ℃ to form a film, and finishing the third smelting;
(6) fourth smelting: and heating to 1470-1500 ℃ in 5-8 minutes, preserving the heat for 1-3 minutes, finishing the fourth smelting, and pouring to form a master alloy ingot.
Preferably, the initial temperature rise process in the step (2) is to start the energization heating after the vacuum degree is lower than 0.1Pa, heat the temperature to 850-950 ℃ in 50-60 minutes, keep the temperature for 20 minutes, and continue the heating for 30 minutes until the temperature reaches 1500-1540 ℃.
Preferably, in the step (4), the temperature of the newly added mixed material of Ni-C and aluminum is raised to 1520-1540 ℃ within 12-15 minutes, and the vacuum of the vacuum smelting furnace is restored to be lower than 0.1Pa in the process of cutting off power and reducing the temperature to form a film.
The invention puts the raw material elements with higher melting point into a melting crucible in sequence, and firstly carries out primary melting, furnace shaking and refining; then adding Ni-C and Al, and then carrying out secondary smelting and furnace shaking; and finally, carrying out third smelting and fourth smelting, and pouring to obtain the nickel-based single crystal superalloy master alloy. The nickel-based single crystal superalloy master alloy obtained by the method is easy to accurately control the alloy components, and meanwhile, the content of N, O and other elements in the alloy can be effectively reduced, and the potential of the alloy is fully exerted.
The invention has the beneficial effects that: by reasonably designing the stacking sequence of the raw materials in the melting crucible, the elements such as Ni, Co and the like can be promoted to be firstly melted in a large amount, then Cr with higher saturated vapor pressure is melted, and then the elements such as W, Re, Mo and the like with high melting points are slowly diffused and melted, so that the refining temperature and time are effectively reduced, and the splashing of the raw materials is reduced; the burning loss of vulnerable elements is effectively reduced by adding Ni-C, Al and other raw materials after the cooling film is completely solidified, meanwhile, filling inert gas to increase the smelting pressure, and combining measures of slowly raising the temperature, controlling the highest heating temperature and the like; through the cyclic process of multiple furnace shaking, three times of cooling and heating, the N content and other gases are effectively removed; compared with other smelting technologies, the method improves the component precision and the cleanliness of the alloy and obtains better lasting performance under the conditions of not improving the purity grade of raw materials and not adopting electromagnetic stirring or other purification technologies.
Drawings
FIG. 1 is a flow chart of a method for preparing a nickel-based single crystal superalloy master alloy by smelting.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the 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.
Example one
A method for smelting and preparing a nickel-based single crystal superalloy master alloy, in particular to a method for smelting a master alloy of a fourth generation nickel-based single crystal superalloy, which comprises the following steps:
(1) charging for the first time: the raw materials are filled according to the components of the target nickel-based single crystal superalloy, and the sequence from the bottom to the top in a melting crucible is as follows: 60% Ni, 100% Co, 100% Cr, 100% W, 100% Mo, 100% Re, 100% Ru, 100% Nb, 100% Hf, 100% Ta, 40% Ni; charging Ni-C and Al into a charging mechanism; (purity of all elemental starting materials not less than 99.95 wt.%)
(2) Smelting for the first time: after the vacuum degree reaches 0.08Pa, starting to electrify and heat, heating to 900 ℃ in 60 minutes, and preserving heat for 20 minutes; heating for 30 minutes, heating to 1530 ℃, keeping the temperature for 10 minutes, and then shaking the furnace for 3 times; continuously heating to 1615 ℃, and preserving heat for 3 minutes to finish refining; cooling to 1560 ℃, preserving heat for 6 minutes, then cutting off power, cooling to complete solidification, and finishing the first smelting;
(3) and (3) charging for the second time: adding Ni-C and Al in a feeding mechanism into a melting crucible, and then charging 5.5 multiplied by 10 into a vacuum induction melting furnace3Pa argon gas;
(4) smelting for the second time: heating the newly added mixed material to 1530 ℃ within 13 minutes, preserving the heat for 5 minutes, and shaking the furnace for 4 times; then, the power is cut off and the temperature is reduced to 1380 ℃ to form a film, thus finishing the second smelting. In the process of cutting off power and cooling to form a film, simultaneously extracting the vacuum of the vacuum smelting furnace to be 0.05 Pa;
(5) smelting for the third time: heating to 1530 ℃ in 7 minutes, keeping the temperature for 5 minutes, and shaking the furnace for 4 times; then, cutting off the power and reducing the temperature to 1380 ℃ to form a film, and finishing the third smelting;
(6) fourth smelting: raising the temperature to 1480 ℃ in 5 minutes, preserving the heat for 2 minutes, finishing the fourth smelting, and starting to cast and mold the master alloy ingot.
Example two
A method for smelting and preparing a nickel-based single crystal superalloy master alloy, in particular to a method for smelting a master alloy of a TMS138 nickel-based single crystal superalloy, which comprises the following steps:
(1) charging for the first time: the raw materials are filled according to the components of the target nickel-based single crystal superalloy, and the sequence from the bottom to the top in a melting crucible is as follows: 70% Ni, 100% Co, 100% Cr, 100% W, 100% Mo, 100% Re, 100% Ru, 100% Nb, 100% Hf, 100% Ta, 30% Ni; charging Ni-C and Al into a charging mechanism;
(2) smelting for the first time: after the vacuum degree reaches 0.06Pa, starting to electrify and heat, heating to 860 ℃ within 55 minutes, and keeping the temperature for 20 minutes; heating for 30 minutes, heating to 1530 ℃, keeping the temperature for 10 minutes, and then rocking the furnace for 4 times; continuously heating to 1610 ℃, preserving heat for 4 minutes and finishing refining; cooling to 1560 ℃, preserving heat for 8 minutes, then cutting off power, cooling to complete solidification, and finishing the first smelting;
(3) and (3) charging for the second time: adding Ni-C and Al in a feeding mechanism into a melting crucible, and then charging into a vacuum induction melting furnace by 3 multiplied by 103Pa argon gas;
(4) smelting for the second time: heating the newly added mixed material to 1535 ℃ within 14 minutes, preserving the heat for 4 minutes, and shaking the furnace for 3 times; then, the power is cut off and the temperature is reduced to 1380 ℃ to form a film, thus finishing the second smelting. In the process of cutting off power and cooling to form a film, simultaneously extracting the vacuum of the vacuum smelting furnace to be 0.05 Pa;
(5) smelting for the third time: heating to 1530 ℃ in 8 minutes, preserving the heat for 4 minutes, and shaking the furnace for 3 times; then, cutting off the power and reducing the temperature to 1380 ℃ to form a film, and finishing the third smelting;
(6) fourth smelting: raising the temperature to 1480 ℃ in 5 minutes, preserving the heat for 2 minutes, finishing the fourth smelting, and starting to cast and mold the master alloy ingot.
Table 1 key element content (mass fraction wt.%) of inventive examples
Example master alloy melting was performed for two fourth generation nickel based single crystal superalloys. As can be seen from Table 1, the control of Cr and Al as the easily-burnt elements is precise, and the O, N content is less than 10 ppm. The single crystal high temperature alloy master alloy obtained by the two embodiments is subjected to subsequent single crystal preparation and heat treatment, the lasting life of the single crystal alloy under the test condition of 1100 ℃/137MPa exceeds 380h, and the obtained single crystal has excellent performance. The invention does not increase purification measures and technologies, obviously improves the metallurgical quality of the alloy, and can be used for smelting the single crystal high-temperature alloy master alloy.
The foregoing detailed description is intended to illustrate and not limit the invention, which is intended to be within the spirit and scope of the appended claims, and any changes and modifications that fall within the true spirit and scope of the invention are intended to be covered by the following claims.
Claims (2)
1. A smelting preparation method of a nickel-based single crystal superalloy master alloy is characterized by comprising the following steps:
(1) the method comprises the following steps of charging for the first time, charging raw materials according to target nickel-based single crystal superalloy components, wherein the raw materials in a melting crucible sequentially comprise, from bottom to top, 60-70% of nickel, 100% of cobalt, 100% of chromium, 100% of tungsten, 100% of molybdenum, 100% of rhenium, 100% of ruthenium, 100% of niobium, 100% of hafnium, 100% of tantalum and 30-40% of nickel;
(2) smelting for the first time, initially heating to 1500-1540 ℃, keeping the temperature for 5-10 minutes, and then shaking the furnace for 3-5 times; continuously heating to 1600-1620 ℃, and preserving the heat for 3-5 minutes to finish refining; cooling to 1550-1570 ℃, preserving heat for 5-10 minutes, and then cutting off power to cool to complete solidification to complete first smelting;
(3) and (3) charging for the second time: 100% of nickel-carbon alloy and 100% of aluminum are added into a melting crucible, and then 10% is charged into a vacuum induction melting furnace3~104Pa argon gas;
(4) smelting for the second time: heating to 1520-1540 ℃, preserving heat for 3-5 minutes, and shaking the furnace for 3-5 times; then, cutting off power and reducing the temperature to 1370-1390 ℃ to form a film, and finishing the second smelting;
(5) smelting for the third time: heating to 1520-1540 ℃ in 5-8 minutes, preserving heat for 3-5 minutes, and shaking the furnace for 3-5 times; then, cutting off power and reducing the temperature to 1370-1390 ℃ to form a film, and finishing the third smelting;
(6) fourth smelting: heating to 1470-1500 ℃ in 5-8 minutes, preserving heat for 1-3 minutes, finishing the fourth smelting, and pouring to form a master alloy ingot;
in the step (4), the temperature of the mixture of the newly added nickel-carbon alloy and the aluminum is raised to 1520-1540 ℃ within 12-15 minutes, and the vacuum of the vacuum smelting furnace is restored to be lower than 0.1Pa in the process of power failure, temperature reduction and film forming.
2. The method for preparing the nickel-based single crystal superalloy master alloy according to claim 1, wherein the method comprises the following steps: and (3) starting electrifying and heating after the vacuum degree is lower than 0.1Pa, heating to 850-950 ℃ in 50-60 minutes, preserving the heat for 20 minutes, and continuously heating to 1500-1540 ℃ in 30 minutes.
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