CN115094272A - Zirconium-nickel-copper-aluminum-tantalum intermediate alloy and preparation method thereof - Google Patents
Zirconium-nickel-copper-aluminum-tantalum intermediate alloy and preparation method thereof Download PDFInfo
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- CN115094272A CN115094272A CN202210810417.9A CN202210810417A CN115094272A CN 115094272 A CN115094272 A CN 115094272A CN 202210810417 A CN202210810417 A CN 202210810417A CN 115094272 A CN115094272 A CN 115094272A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C16/00—Alloys based on zirconium
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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Abstract
The invention relates to the technical field of intermediate alloy materials, and provides a zirconium-nickel-copper-aluminum-tantalum intermediate alloy which comprises the following components in percentage by mass: 60.0 to 70.0 percent of zirconium, 6.0 to 8.0 percent of nickel, 9.0 to 12.0 percent of copper, 12.0 to 16.0 percent of tantalum and the balance of aluminum. The invention limits the components and the content of the intermediate alloy, neutralizes the melting point difference and the density difference among the elements, and leads the density and the melting point of the intermediate alloy provided by the invention to be closer to the density and the melting point of a nickel matrix.
Description
Technical Field
The invention belongs to the technical field of intermediate alloy materials, and particularly relates to a zirconium-nickel-copper-aluminum-tantalum intermediate alloy and a preparation method thereof.
Background
The high-temperature alloy is based on iron, nickel and cobalt, can be used in a high-temperature environment, can bear severe mechanical stress and has good surface stability. Wherein the nickel-based high-temperature alloy is a high-temperature alloy which takes nickel as a matrix (the content is generally more than 50 percent), has higher strength and good oxidation resistance and fuel gas corrosion resistance within the temperature range of 650-1000 ℃, and is Cr 20 Ni 80 Developed on the basis of the alloy, in order to meet the requirements of high-temperature heat strength at about 1000 ℃ and oxidation resistance and corrosion resistance in a gas medium, a certain amount of strengthening elements are required to be added: zirconium, copper, aluminum, and tantalum.
In the prior art, zirconium, copper, aluminum and tantalum are usually directly added into a smelting system in a simple substance form, and due to the melting point and density difference among zirconium, nickel, copper, aluminum and tantalum, element burning loss and refractory element component segregation are caused, so that the comprehensive performance of the nickel-based high-temperature alloy is reduced.
Therefore, how to avoid the burning loss of the elements and the segregation of the refractory elements becomes a technical problem to be solved by those skilled in the art.
Disclosure of Invention
In view of this, the present invention provides a zirconium-nickel-copper-aluminum-tantalum intermediate alloy. The zirconium-nickel-copper-aluminum-tantalum intermediate alloy provided by the invention is used as a raw material to provide the strengthening elements of zirconium, copper, aluminum and tantalum required by the preparation of the nickel-based superalloy, so that the burning loss of the elements and the component segregation of refractory elements can be avoided.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a zirconium-nickel-copper-aluminum-tantalum intermediate alloy which comprises the following components in percentage by mass: 60.0 to 70.0 percent of zirconium, 6.0 to 8.0 percent of nickel, 9.0 to 12.0 percent of copper, 12.0 to 16.0 percent of tantalum and the balance of aluminum.
The invention also provides a preparation method of the zirconium-nickel-copper-aluminum-tantalum intermediate alloy, which comprises the following steps:
(1) mixing zirconium dioxide, nickel oxide, copper oxide, aluminum and tantalum pentoxide to obtain a mixture;
(2) carrying out thermite reaction on one part of the mixture obtained in the step (1), adding the rest part of the mixture obtained in the step (1) in the thermite reaction process, and continuously carrying out thermite reaction to obtain a primary zirconium-nickel-copper-aluminum-tantalum alloy;
(3) sequentially adding one part and part of zirconium in the primary zirconium-nickel-copper-aluminum-tantalum alloy obtained in the step (2) and the rest part of the primary zirconium-nickel-copper-aluminum-tantalum alloy obtained in the step (2) into a heated container to perform vacuum induction melting to obtain a melt;
(4) and (4) adding the rest part of zirconium into the melt obtained in the step (3), continuing vacuum induction melting, and then sequentially carrying out vacuum induction refining and cooling to obtain the zirconium-nickel-copper-aluminum-tantalum alloy.
Preferably, the zirconium dioxide, nickel oxide, copper oxide, aluminum and tantalum pentoxide in step (1) are dried.
Preferably, the drying temperature is 110-120 ℃, and the drying time is 6-20 h.
Preferably, the mass ratio of zirconium dioxide, nickel oxide, copper oxide, aluminum and tantalum pentoxide in the step (1) is (2.80-2.93): (0.52-0.58): (0.6-1.0): (1.56-1.60): 1.00.
preferably, a part of the mixed material in the step (2) is 45-55% of the total mass of the mixed material.
Preferably, part of the zirconium in the step (3) accounts for 60-80% of the total mass of the zirconium.
Preferably, the mass ratio of the total mass of part of zirconium in the step (3) and the rest of zirconium in the step (4) to the mass ratio of the primary zirconium-nickel-copper-aluminum-tantalum alloy obtained in the step (2) is (0.50-1.00): (1.50-2.00).
Preferably, the power of the vacuum induction refining in the step (4) is 95-105 kW.
Preferably, the cooling in step (4) is performed under vacuum.
The invention provides a zirconium-nickel-copper-aluminum-tantalum intermediate alloy which comprises the following components in percentage by mass: 60.0 to 70.0 percent of zirconium, 6.0 to 8.0 percent of nickel, 9.0 to 12.0 percent of copper, 12.0 to 16.0 percent of tantalum and the balance of aluminum. The invention limits the components and the content of the intermediate alloy, neutralizes the melting point difference and the density difference among the elements, and leads the density and the melting point of the intermediate alloy provided by the invention to be closer to the density and the melting point of a nickel matrix. Experimental results show that the nickel-based high-temperature alloy prepared from the zirconium-nickel-copper-aluminum-tantalum intermediate alloy has uniform metal content in the upper part, the middle part and the lower part.
Detailed Description
The invention provides a zirconium-nickel-copper-aluminum-tantalum intermediate alloy which comprises the following components in percentage by mass: 60.0 to 70.0 percent of zirconium, 6.0 to 8.0 percent of nickel, 9.0 to 12.0 percent of copper, 12.0 to 16.0 percent of tantalum and the balance of aluminum.
According to the mass percentage, the zirconium-nickel-copper-aluminum-tantalum intermediate alloy provided by the invention comprises 60.0-70.0% of zirconium, preferably 61.0-69.0%, and more preferably 65.0%. The invention adds zirconium element and controls the content in the range to purify the crystal boundary, improve the high temperature characteristic and increase the high temperature fracture strength.
According to the mass percentage, the zirconium-nickel-copper-aluminum-tantalum intermediate alloy provided by the invention comprises 6.0-8.0% of nickel, preferably 65-7.5%, and more preferably 7.0%. In the invention, nickel exists as a basic element, and the use amount of the nickel element is controlled in the range, which is beneficial to obtaining the zirconium-nickel-copper-aluminum-tantalum intermediate alloy with uniform components.
The zirconium-nickel-copper-aluminum-tantalum intermediate alloy provided by the invention comprises 9.0-12.0% of copper, preferably 9.5-11.5%, and more preferably 10.5% by mass. The invention can improve the corrosion resistance of the high-temperature alloy to reducing acid and salt by adding the copper element and controlling the content of the copper element within the range.
The zirconium-nickel-copper-aluminum-tantalum intermediate alloy provided by the invention comprises 12.0-16.0% of tantalum, preferably 12.5-15.5%, and more preferably 14.0% by mass. According to the invention, the plasticity and toughness of the high-temperature alloy can be improved by adding the tantalum element and controlling the content of the tantalum element within the range.
The zirconium-nickel-copper-aluminum-tantalum intermediate alloy provided by the invention comprises the balance of aluminum, and the high-temperature oxidation resistance and the aging hardening can be improved by adding the aluminum element into the zirconium-nickel-copper-aluminum-tantalum intermediate alloy.
The zirconium-nickel-copper-aluminum-tantalum intermediate alloy provided by the invention also contains inevitable impurities. In the invention, the impurity content of the zirconium-nickel-copper-aluminum-tantalum intermediate alloy is less than 0.2 percent by mass. Since the purity of the raw material providing the required elements cannot be 100%, small amounts of unavoidable impurities are present in the zirconium-nickel-copper-aluminum-tantalum master alloy.
The invention limits the components and the content of the zirconium-nickel-copper-aluminum-tantalum intermediate alloy, neutralizes the melting point difference and the density difference among the elements, and ensures that the density and the melting point of the zirconium-nickel-copper-aluminum-tantalum intermediate alloy provided by the invention are closer to the density and the melting point of a nickel matrix.
The invention also provides a preparation method of the zirconium-nickel-copper-aluminum-tantalum intermediate alloy, which comprises the following steps:
(1) mixing zirconium dioxide, nickel oxide, copper oxide, aluminum and tantalum pentoxide to obtain a mixture;
(2) carrying out thermite reaction on one part of the mixture obtained in the step (1), adding the rest part of the mixture obtained in the step (1) in the thermite reaction process, and continuously carrying out thermite reaction to obtain a primary zirconium-nickel-copper-aluminum-tantalum alloy;
(3) sequentially adding one part and part of zirconium in the primary zirconium-nickel-copper-aluminum-tantalum alloy obtained in the step (2) and the rest part of the primary zirconium-nickel-copper-aluminum-tantalum alloy obtained in the step (2) into a heated container to perform vacuum induction melting to obtain a melt;
(4) and (4) adding the rest of zirconium into the melt obtained in the step (3), continuing vacuum induction smelting, and then sequentially carrying out vacuum induction refining and cooling to obtain the zirconium-nickel-copper-aluminum-tantalum alloy.
Zirconium dioxide, nickel oxide, copper oxide, aluminum and tantalum pentoxide are mixed to obtain a mixture. The invention adopts the oxides of zirconium, nickel, copper and tantalum and the simple substance of aluminum to carry out metal smelting by using thermite reaction.
In the present invention, the zirconium dioxide, nickel oxide, copper oxide, aluminum and tantalum pentoxide are preferably dried. In the invention, the drying temperature is preferably 110-120 ℃, and more preferably 112-111 ℃; the drying time is preferably 6-20 hours, and more preferably 8-15 hours. The invention limits the drying temperature and time within the range, can remove moisture absorbed by the material, and ensures the material to be dried, thereby reducing the separated impurity gases such as hydrogen, nitrogen, oxygen and the like in the smelting process.
In the invention, the purities of the zirconium dioxide, the nickel oxide, the copper oxide, the aluminum and the tantalum pentoxide are all more than or equal to 99.00 percent. In the present invention, the aluminum is preferably a particulate elemental aluminum; the zirconium dioxide, nickel oxide, copper oxide and tantalum pentoxide are preferably in powder form. The present invention does not specifically specify the particle size of the granular or powdery particles, and may use the particle size of the commercially available industrial raw material well known to those skilled in the art.
In the invention, the mass ratio of the zirconium dioxide, the nickel oxide, the copper oxide, the aluminum and the tantalum pentoxide is preferably (2.80-2.93): (0.52-0.58): (0.6-1.0): (1.56-1.60): 1.00, more preferably (2.89 to 2.91): (0.54-0.56): (0.7-0.9): (1.57-1.59): 1.00. the invention limits the mass ratio of the zirconium dioxide, the nickel oxide, the copper oxide, the aluminum and the tantalum pentoxide to the above range, and the grade of the obtained first-grade zirconium-nickel-copper-aluminum-tantalum alloy is as follows: 50.0% of zirconium, 10.0% of nickel, 15.0% of copper, 20.0% of tantalum and the balance of aluminum.
The operation of the mixing is not specially specified in the invention, and the raw materials are uniformly mixed by adopting a mixing mode which is well known to a person skilled in the art.
After the mixture is obtained, part of the mixture is preferably subjected to thermite reaction, the rest part of the mixture is added in the thermite reaction process, and the thermite reaction is continued to obtain the primary zirconium-nickel-copper-aluminum-tantalum alloy.
In the present invention, a part of the mixed material is preferably 45% to 55%, more preferably 50% of the total mass of the mixed material. The invention limits the feeding mode and the dosage of the mixture in the range, can ensure that the reaction is always in a controllable state by carrying out the aluminothermic reduction reaction, ensures that the alloy and the slag are separated more fully by continuously boiling the alloy liquid, reduces impurities such as Fe, Si and the like and aluminum oxide inclusions, ensures that the alloy ingot is more uniform, and reduces segregation. The first-grade zirconium-nickel-copper-aluminum-tantalum alloy with low impurities and good uniformity can be obtained.
In the invention, the temperature of the thermite reaction is preferably 1820-1920 ℃, and is more preferably 1850-1900 ℃; the time of the thermite reaction is preferably 32-42 s, and more preferably 36-39 s. In the invention, the thermite reaction time refers to the time of the whole thermite reaction process for obtaining the primary zirconium-nickel-copper-aluminum-tantalum alloy, and the time for carrying out the thermite reaction on the two parts of raw materials is not strictly divided. In the invention, in the thermit reaction process, aluminum is used as a reducing agent, other oxides are respectively reduced into metal simple substances of zirconium, nickel, copper and tantalum, aluminum is oxidized into aluminum oxide, and a large amount of heat energy is released to melt the metal simple substance chromium to form zirconium-nickel-copper-aluminum-tantalum alloy liquid; the aluminum oxide formed by oxidizing the aluminum floats on the surface of the primary zirconium-nickel-copper-aluminum-tantalum alloy liquid, and is naturally separated and removed from the primary zirconium-nickel-copper-aluminum-tantalum alloy after being cooled.
After the thermite reaction is finished, the invention preferably sequentially cools, removes impurities, finishes, crushes and selects the product after the thermite reaction to obtain the first-grade zirconium-nickel-copper-aluminum-tantalum alloy.
In the present invention, the cooling is preferably furnace cooling. The furnace cooling mode is not specially specified, and the furnace cooling mode known by the person skilled in the art is adopted for cooling. The time for cooling along with the furnace is not specially specified, and the cooling to the room temperature is realized.
The impurity removal mode is not specially specified, and the cooled slag layer and the oxide film on the surface of the alloy ingot can be removed according to the impurity removal mode well known by the technical personnel in the field.
The finishing crushing mode is not specially specified, and the zirconium-nickel-copper-aluminum-tantalum alloy ingot is finished and crushed into blocks of 5-50mm by adopting a finishing crushing mode well known by the technical personnel in the field.
In the present invention, the sorting preferably includes magnetic sorting and manual sorting. The invention has no special regulation on the magnetic separation and manual selection modes, magnetic impurities, oxide-containing films, nitride film alloys and other impurities are selected according to the magnetic separation and manual selection modes known by the technical personnel in the field, and the qualified parts are selected manually to be used as the zirconium-nickel-copper-aluminum-tantalum alloy.
After the primary zirconium-nickel-copper-aluminum-tantalum alloy is obtained, part of the obtained primary zirconium-nickel-copper-aluminum-tantalum alloy, part of zirconium and the rest of the obtained primary zirconium-nickel-copper-aluminum-tantalum alloy are sequentially added into a heated container to be subjected to vacuum induction melting to obtain a melt. In the present invention, the heating vessel is preferably a crucible. The crucible is not particularly specified in the present invention, and a crucible for high-temperature heating known to those skilled in the art may be used. In the invention, the part of zirconium is positioned in the middle of the material, so that the zirconium can be more easily melted in the heating process, and meanwhile, in order to avoid excessive simple substance of zirconium and difficulty in complete melting, the zirconium serving as the simple substance of zirconium is added in two times, so that the alloy liquid is fully melted, and the alloy ingot is more uniform.
In the present invention, the zirconium is preferably commercially available zirconium sponge.
In the present invention, the vacuum induction melting is preferably performed in a medium frequency vacuum induction furnace. In the present invention, the crucible used in the vacuum induction melting process is preferably a corundum crucible. In the present invention, the corundum crucible is hard and refractory. In the present invention, the purity of the corundum crucible is preferably not less than 99.00%. The invention limits the purity of the corundum crucible to the range, and can reduce the content of impurity elements in the alloy. In the present invention, the knotted lining of the corundum crucible is preferably prepared by using the aluminothermic slag (alumina) in the above technical scheme. According to the invention, the furnace lining for knotting the corundum crucible is prepared by selecting the furnace slag (aluminum oxide) of the aluminothermic reaction in the technical scheme, so that reaction raw materials can be fully utilized, and the cost is saved. The preparation method of the furnace lining for knotting the corundum crucible has no special requirement, and the method well known in the field can be adopted.
In the present invention, the zirconium portion is preferably 60 to 80%, more preferably 70% of the total weight of zirconium. In the invention, the mass ratio of the total mass of the part of zirconium and the rest of zirconium to the mass of the primary zirconium-nickel-copper-aluminum-tantalum alloy is preferably (0.50-1.00): (1.50 to 2.00), more preferably 0.75: 1.75.
in the present invention, both the vacuum induction melting and the vacuum induction refining are preferably performed in a medium frequency vacuum induction melting furnace. In the invention, the medium-frequency vacuum induction smelting furnace has high thermal efficiency and quick smelting, and is not easy to introduce impurities in vacuum operation, thereby having little pollution to the environment.
In the present invention, the initial degree of vacuum in the vacuum induction melting is preferably 15Pa or less, and more preferably 14Pa or less. The invention can reduce the content of O, N gas-phase impurities in the finally prepared intermediate alloy by controlling the vacuum degree.
In the invention, the power of the vacuum induction melting is preferably 75-85 kW, and more preferably 80 kW. In the present invention, the power of the vacuum induction melting is preferably increased to the required power in a gradient increasing manner. In the embodiment of the invention, the gradient is preferably increased in a manner that the initial power is adjusted to be 20kW, the power is adjusted to be 30kW after 10min, and the power is adjusted to be 80kW after 20 min.
After the melt is obtained, the invention adds the residual zirconium into the obtained melt, continues the vacuum induction melting, and then carries out the vacuum induction refining and cooling in sequence to obtain the zirconium-nickel-copper-aluminum-tantalum alloy.
In the present invention, the vacuum induction melting and the vacuum induction refining are preferably both performed in a vacuum induction melting furnace, and the only difference between them is the power setting of the vacuum induction melting furnace. The invention realizes the melting of materials through vacuum induction melting, leads the zirconium-nickel-copper-aluminum-tantalum intermediate alloy to be more fully and uniformly melted through vacuum induction refining, and plays the role of purifying and removing impurities.
In the invention, the power of the vacuum induction refining is preferably 95-105 kW, and more preferably 100 kW. In the invention, the temperature of the vacuum induction refining is preferably 1850-1890 ℃, and more preferably 1860-1880 ℃. In the invention, the time of the vacuum induction refining is preferably 5-9 min, and more preferably 6-8 min. The invention can make the refining temperature slightly higher than the melting point of the alloy by controlling the temperature so as to achieve the refining purpose; the zirconium-nickel-copper-aluminum-tantalum intermediate alloy can be more fully and uniformly melted through vacuum induction refining, and the effects of purifying and removing impurities are achieved.
After the vacuum induction refining is finished, the reaction system after the vacuum induction refining is preferably subjected to vacuum pumping, power regulation and cooling in sequence. In the present invention, the degree of vacuum to which the vacuum is applied is preferably 15Pa or less, and more preferably 14Pa or less. The invention removes oxygen element in the melt by vacuum pumping to obtain the zirconium-nickel-copper-aluminum-tantalum alloy liquid.
In the invention, the power for adjusting the power is preferably 75-85 kW, and more preferably 80 kW. The invention avoids the overhigh temperature in the furnace by reducing the power of the vacuum induction melting furnace.
In the present invention, the cooling is preferably performed under vacuum conditions. The invention can reduce O, N and other gas impurities by a vacuum cooling mode.
The cooling method is not particularly limited in the present invention, and a cooling method known to those skilled in the art may be used. In the embodiment of the present invention, the cooling specifically includes: and pouring the product after vacuum induction refining into a water-cooled copper crucible for cooling to obtain the zirconium-nickel-copper-aluminum-tantalum intermediate alloy. The water-cooled copper crucible of the present invention is not particularly limited, and a water-cooled copper crucible known in the art may be used. In the invention, the cooling time is preferably 6-20 h, and more preferably 8-15 h. The present invention limits the cooling time within the above range, and is favorable to cooling the material fully.
The preparation method of the zirconium-nickel-copper-aluminum-tantalum intermediate alloy provided by the invention has the advantages that the components of the zirconium-nickel-copper-aluminum-tantalum intermediate alloy are uniform, the impurity content is low, and the loss of raw materials is small through the control of thermite reaction and a special material distribution mode during smelting. When the high-temperature alloy is smelted, the homogenization of the components of the high-temperature alloy is facilitated, the component segregation is prevented, the element burning loss is reduced, and the quality of the high-temperature alloy is improved.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
The zirconium-nickel-copper-aluminum-tantalum intermediate alloy comprises the following components in percentage by mass: 60.0% of zirconium, 8.0% of nickel, 12.0% of copper, 16.0% of tantalum and the balance of aluminum.
The preparation method of the zirconium-nickel-copper-aluminum-tantalum intermediate alloy in the embodiment comprises the following specific steps:
(1) respectively drying zirconium dioxide, nickel oxide, copper oxide, aluminum particles and tantalum pentoxide at the temperature of 110 ℃ for 6 hours;
weighing 67.58kg of zirconium dioxide, 12.71kg of nickel oxide, 18.75kg of copper oxide, 36.80kg of aluminum particles and 23.31kg of tantalum pentoxide, and filling the materials into a roller mixer to be fully and uniformly mixed to obtain a mixture; wherein the mass ratio of zirconium dioxide, nickel oxide, copper oxide, aluminum particles and tantalum pentoxide is 2.90: 0.55: 0.80: 1.58: 1.00;
(2) putting 50 percent (79.58kg) of the mass of the mixture obtained in the step (1) into a sintered corundum crucible, igniting the mixture to carry out aluminothermic reaction, adding the rest 50 percent (79.58kg) of the mixture from the top of a reaction furnace in the reaction process, continuously carrying out the aluminothermic reaction at the temperature of 1820 ℃ for 32s, cooling for 12h, dismantling the crucible, taking out an alloy ingot, removing a slag layer and an oxide film on the surface of the alloy ingot, crushing and finishing to 5-50mm, and carrying out magnetic separation and manual selection to obtain a primary zirconium-nickel-copper-aluminum-tantalum alloy; the grade of the primary zirconium-nickel-copper-aluminum-tantalum alloy comprises 50.0 percent of zirconium, 10.0 percent of nickel, 15.0 percent of copper, 20.0 percent of tantalum and the balance of aluminum;
(3) adding 40.00kg of partial first-stage zirconium-nickel-copper-aluminum-tantalum alloy (accounting for 50 percent of the total mass of the required first-stage zirconium-nickel-copper-aluminum-tantalum alloy), 14.00kg of zirconium sponge (accounting for 70 percent of the total mass of the required zirconium sponge) at the bottom of the crucible in sequence, and finally adding 40.00kg of the rest first-stage zirconium-nickel-copper-aluminum-tantalum alloy for vacuum induction melting; the specific operation of vacuum induction melting is as follows: vacuumizing the medium-frequency vacuum induction smelting furnace to below 15Pa, removing gas in the furnace, setting the initial power to be 20kW, adjusting the power to be 30kW after 10min, and adjusting the power to be 80kW after 20min until the alloy is completely melted to obtain melt;
(4) adding the remaining 6.00kg of sponge zirconium into the melt obtained in the step (3) through a secondary feeding device, continuously carrying out vacuum induction melting, and carrying out vacuum induction refining after all the sponge zirconium is melted; the operation of the vacuum induction refining is as follows: adjusting the power of a vacuum induction furnace to 100kW, refining for 9min under the conditions of 100kW power and 1890 ℃, vacuumizing the medium-frequency vacuum induction smelting furnace to below 15Pa again, and removing oxygen elements in the melt to obtain zirconium-nickel-copper-aluminum-tantalum alloy liquid;
(5) adjusting the power of the medium-frequency vacuum induction smelting furnace to 80kW, inclining the crucible, slowly and stably pouring the zirconium-nickel-copper-aluminum-tantalum alloy liquid into the water-cooled crucible, and keeping vacuum cooling for 6h to obtain the zirconium-nickel-copper-aluminum-tantalum intermediate alloy.
Example 2
The zirconium-nickel-copper-aluminum-tantalum intermediate alloy comprises the following components in percentage by mass: 62.5% of zirconium, 7.5% of nickel, 11.2% of copper, 15.1% of tantalum and the balance of aluminum.
The preparation method of the zirconium-nickel-copper-aluminum-tantalum intermediate alloy in the embodiment comprises the following specific steps:
(1) respectively drying zirconium dioxide, nickel oxide, copper oxide, aluminum particles and tantalum pentoxide at the temperature of 114 ℃ for 8 hours;
weighing 67.58kg of zirconium dioxide, 12.71kg of nickel oxide, 18.75kg of copper oxide, 36.80kg of aluminum particles and 23.31kg of tantalum pentoxide, and putting the materials into a roller mixer to be fully and uniformly mixed to obtain a mixture; wherein the mass ratio of zirconium dioxide, nickel oxide, copper oxide, aluminum particles and tantalum pentoxide is 2.90: 0.55: 0.80: 1.58: 1.00;
(2) and (2) putting 50% (79.58kg) of the mass of the mixture obtained in the step (1) into a sintered corundum crucible, igniting the mixture to carry out aluminothermic reaction, adding the rest 50% (79.58kg) of the mixture from the top of a reaction furnace in the reaction process, continuously carrying out the aluminothermic reaction at the temperature of 1840 ℃ for 34s, cooling for 13h, dismantling the crucible, taking out an alloy ingot, removing a slag layer and an oxidation film on the surface of the alloy ingot, crushing and finishing to 5-50mm, and carrying out magnetic separation and manual selection to obtain the primary zirconium-nickel-copper-aluminum-tantalum alloy. The grade of the primary zirconium-nickel-copper-aluminum-tantalum alloy comprises 50.0 percent of zirconium, 10.0 percent of nickel, 15.0 percent of copper, 20.0 percent of tantalum and the balance of aluminum;
(3) adding 37.50kg of a part of first-stage zirconium-nickel-copper-aluminum-tantalum alloy (accounting for 50% of the total mass of the required first-stage zirconium-nickel-copper-aluminum-tantalum alloy) and 17.50kg of sponge zirconium (accounting for 70% of the total mass of the required sponge zirconium) at the bottom of the crucible in sequence, and finally adding 37.50kg of the rest first-stage zirconium-nickel-copper-aluminum-tantalum alloy for vacuum induction melting; the specific operation of vacuum induction melting is as follows: vacuumizing the intermediate-frequency vacuum induction smelting furnace to below 14Pa, removing gas in the furnace, setting the initial power to be 20kW, adjusting the power to be 30kW after 10min, and adjusting the power to be 80kW after 20min until the alloy is completely melted to obtain a melt;
(4) adding the remaining 7.50kg of sponge zirconium into the melt obtained in the step (3) through a secondary feeding device, and after all the sponge zirconium is melted, carrying out vacuum induction refining; the operation of the vacuum induction refining is as follows: adjusting the power of the vacuum induction furnace to 100kW, refining for 8min at the power of 100kW and the temperature of 1880 ℃, vacuumizing the medium-frequency vacuum induction melting furnace to below 14Pa again, and removing oxygen elements in the melt to obtain a zirconium-nickel-copper-aluminum-tantalum alloy liquid;
(5) adjusting the power of the medium-frequency vacuum induction melting furnace to 80kW, inclining the crucible, slowly and stably pouring the zirconium-nickel-copper-aluminum-tantalum alloy liquid into a water-cooled crucible, and keeping vacuum cooling for 7h to obtain the zirconium-nickel-copper-aluminum-tantalum intermediate alloy.
Example 3
The zirconium-nickel-copper-aluminum-tantalum intermediate alloy comprises the following components in percentage by mass: 65.0% of zirconium, 7.1% of nickel, 10.5% of copper, 14.0% of tantalum and the balance of aluminum.
The preparation method of the zirconium-nickel-copper-aluminum-tantalum intermediate alloy comprises the following specific steps of:
(1) respectively drying zirconium dioxide, nickel oxide, copper oxide, aluminum particles and tantalum pentoxide at the temperature of 116 ℃ for 10 hours;
weighing 67.58kg of zirconium dioxide, 12.71kg of nickel oxide, 18.75kg of copper oxide, 36.80kg of aluminum particles and 23.31kg of tantalum pentoxide, and filling the materials into a roller mixer to be fully and uniformly mixed to obtain a mixture; wherein the mass ratio of zirconium dioxide, nickel oxide, copper oxide, aluminum particles and tantalum pentoxide is 2.90: 0.55: 0.80: 1.58: 1.00;
(2) putting 50 percent (79.58kg) of the mass of the mixture obtained in the step (1) into a sintered corundum crucible, igniting the mixture to carry out aluminothermic reaction, adding the rest 50 percent (79.58kg) of the mixture from the top of a reaction furnace in the reaction process, continuously carrying out aluminothermic reaction at the temperature of 1860 ℃ for 36s, cooling for 14h, dismantling the crucible, taking out an alloy ingot, removing a slag layer and an oxidation film on the surface of the alloy ingot, crushing and finishing to 5-50mm, and carrying out magnetic separation and manual selection to obtain a primary zirconium-nickel-copper-aluminum-tantalum alloy; the grade of the primary zirconium-nickel-copper-aluminum-tantalum alloy comprises 50.0 percent of zirconium, 10.0 percent of nickel, 15.0 percent of copper, 20.0 percent of tantalum and the balance of aluminum;
(3) adding 35.00kg of partial first-stage zirconium-nickel-copper-aluminum-tantalum alloy (accounting for 50 percent of the total mass of the required first-stage zirconium-nickel-copper-aluminum-tantalum alloy) and 21.00kg of sponge zirconium (accounting for 70 percent of the total mass of the required sponge zirconium) at the bottom of the crucible in sequence, and finally adding 35.00kg of the rest first-stage zirconium-nickel-copper-aluminum-tantalum alloy for vacuum induction melting; the specific operation of vacuum induction melting is as follows: vacuumizing the medium-frequency vacuum induction melting furnace to below 13Pa to remove gas in the furnace, setting the initial power to be 20kW, adjusting the power to be 30kW after 10min, and adjusting the power to be 80kW after 20min until the alloy is completely melted to obtain melt;
(4) adding the remaining 9.00kg of sponge zirconium into the melt obtained in the step (3) through a secondary feeding device, and after all the sponge zirconium is melted, carrying out vacuum induction refining; the operation of the vacuum induction refining is as follows: adjusting the power of the vacuum induction furnace to 100kW, refining for 7min at the power of 100kW and the temperature of 1870 ℃, vacuumizing the medium-frequency vacuum induction melting furnace to below 13Pa again, and removing oxygen elements in the melt to obtain a zirconium-nickel-copper-aluminum-tantalum alloy liquid;
(5) adjusting the power of the medium-frequency vacuum induction smelting furnace to 80kW, inclining the crucible, slowly and stably pouring the zirconium-nickel-copper-aluminum-tantalum alloy liquid into the water-cooled crucible, and keeping vacuum cooling for 8h to obtain the zirconium-nickel-copper-aluminum-tantalum intermediate alloy.
Example 4
The zirconium-nickel-copper-aluminum-tantalum intermediate alloy comprises the following components in percentage by mass: 67.5% of zirconium, 6.5% of nickel, 9.8% of copper, 13.1% of tantalum and the balance of aluminum.
The preparation method of the zirconium-nickel-copper-aluminum-tantalum intermediate alloy comprises the following specific steps:
(1) respectively drying zirconium dioxide, nickel oxide, copper oxide, aluminum particles and tantalum pentoxide at 118 ℃ for 12 hours;
weighing 67.58kg of zirconium dioxide, 12.71kg of nickel oxide, 18.75kg of copper oxide, 36.80kg of aluminum particles and 23.31kg of tantalum pentoxide, and filling the materials into a roller mixer to be fully and uniformly mixed to obtain a mixture; wherein the mass ratio of zirconium dioxide, nickel oxide, copper oxide, aluminum particles and tantalum pentoxide is 2.90: 0.55: 0.80: 1.58: 1.00;
(2) putting 50 percent (79.58kg) of the mass of the mixture obtained in the step (1) into a sintered corundum crucible, igniting the mixture to carry out aluminothermic reaction, adding the rest 50 percent (79.58kg) of the mixture from the top of a reaction furnace in the reaction process, continuously carrying out aluminothermic reaction at the temperature of 1880 ℃ for 38s, cooling the mixture for 16h, dismantling the crucible, taking out an alloy ingot, removing a slag layer and an oxide film on the surface of the alloy ingot, crushing and finishing the mixture to 5-50mm, and carrying out magnetic separation and manual selection to obtain a primary zirconium-nickel-copper-aluminum-tantalum alloy with the grades of 50.0 percent of zirconium, 10.0 percent of nickel, 15.0 percent of copper, 20.0 percent of tantalum and the balance of aluminum;
(3) 32.50kg of a part of first-stage zirconium-nickel-copper-aluminum-tantalum alloy (accounting for 50 percent of the total mass of the required first-stage zirconium-nickel-copper-aluminum-tantalum alloy), 24.50kg of sponge zirconium (accounting for 70 percent of the total mass of the required sponge zirconium) are sequentially added to the bottom of the crucible, and 32.50kg of the rest first-stage zirconium-nickel-copper-aluminum-tantalum alloy is finally added for vacuum induction melting; the specific operation of vacuum induction melting is as follows: vacuumizing the medium-frequency vacuum induction melting furnace to below 12Pa, removing gas in the furnace, setting the initial power to be 20kW, adjusting the power to be 30kW after 10min, and adjusting the power to be 80kW after 20min until the alloy is completely melted to obtain melt;
(4) adding the remaining 10.50kg of sponge zirconium into the melt obtained in the step (3) through a secondary feeding device, and after the sponge zirconium is completely melted, carrying out vacuum induction refining; the operation of the vacuum induction refining is as follows: adjusting the power of the vacuum induction furnace to 100kW, refining for 8min at the power of 100kW and the temperature of 1880 ℃, vacuumizing the medium-frequency vacuum induction melting furnace to below 12Pa again, and removing oxygen elements in the melt to obtain a zirconium-nickel-copper-aluminum-tantalum alloy liquid;
(5) adjusting the power of the medium-frequency vacuum induction melting furnace to 80kW, inclining the crucible, slowly and stably pouring the zirconium-nickel-copper-aluminum-tantalum alloy liquid into a water-cooled crucible, and keeping vacuum cooling for 9h to obtain the zirconium-nickel-copper-aluminum-tantalum intermediate alloy.
Example 5
The zirconium-nickel-copper-aluminum-tantalum intermediate alloy comprises the following components in percentage by mass: 70.0% of zirconium, 6.0% of nickel, 9.0% of copper, 12.0% of tantalum and the balance of aluminum.
The preparation method of the zirconium-nickel-copper-aluminum-tantalum intermediate alloy comprises the following specific steps of:
(1) drying zirconium dioxide, nickel oxide, copper oxide, aluminum particles and tantalum pentoxide at 120 ℃ for 14 h;
weighing 67.58kg of zirconium dioxide, 12.71kg of nickel oxide, 18.75kg of copper oxide, 36.80kg of aluminum particles and 23.31kg of tantalum pentoxide, and filling the materials into a roller mixer to be fully and uniformly mixed to obtain a mixture; wherein the mass ratio of zirconium dioxide, nickel oxide, copper oxide, aluminum particles and tantalum pentoxide is 2.90: 0.55: 0.80: 1.58: 1.00;
(2) putting 50 percent (79.58kg) of the mass of the mixture obtained in the step (1) into a sintered corundum crucible, igniting the mixture to carry out aluminothermic reaction, adding the rest 50 percent (79.58kg) of the mixture from the top of a reaction furnace in the reaction process, continuously carrying out aluminothermic reaction at the temperature of 1920 ℃ for 42s, cooling the mixture for 18h, dismantling the crucible, taking out an alloy ingot, removing a slag layer and an oxide film on the surface of the alloy ingot, crushing and finishing the mixture to 5-50mm, and carrying out magnetic separation and manual selection to obtain a primary zirconium-nickel-copper-aluminum-tantalum alloy with the grades of 50.0 percent of zirconium, 10.0 percent of nickel, 15.0 percent of copper, 20.0 percent of tantalum and the balance of aluminum;
(3) adding 30.00kg of partial first-stage zirconium-nickel-copper-aluminum-tantalum alloy (accounting for 50 percent of the total mass of the required first-stage zirconium-nickel-copper-aluminum-tantalum alloy), 28.00kg of sponge zirconium (accounting for 70 percent of the total mass of the required sponge zirconium) at the bottom of the crucible in sequence, and finally adding 30.00kg of the rest first-stage zirconium-nickel-copper-aluminum-tantalum alloy for vacuum induction melting; the specific operation of vacuum induction melting is as follows: vacuumizing the medium-frequency vacuum induction melting furnace to below 10Pa, removing gas in the furnace, setting the initial power to be 20kW, adjusting the power to be 30kW after 10min, and adjusting the power to be 80kW after 20min until the alloy is completely melted to obtain melt;
(4) adding the remaining 12.00kg of sponge zirconium into the melt obtained in the step (3) through a secondary feeding device, and after all the sponge zirconium is melted, carrying out vacuum induction refining; the operation of the vacuum induction refining is as follows: adjusting the power of the vacuum induction furnace to 100kW, refining for 9min at the power of 100kW and at the temperature of 1890 ℃, vacuumizing the medium-frequency vacuum induction smelting furnace to below 10Pa again, and removing oxygen elements in the melt to obtain a zirconium-nickel-copper-aluminum-tantalum alloy liquid;
(5) adjusting the power of the medium-frequency vacuum induction melting furnace to 80kW, inclining the crucible, slowly and stably pouring the zirconium-nickel-copper-aluminum-tantalum alloy liquid into a water-cooled crucible, and keeping vacuum cooling for 10 hours to obtain the zirconium-nickel-copper-aluminum-tantalum intermediate alloy.
Performance detection
The chemical composition analysis was performed on zirconium-nickel-copper-aluminum-tantalum intermediate alloy ingots (cylinders) prepared in examples 1 to 5, in which two points (1, 2) were taken from the upper surface of the ingot, two points (3, 4) were taken from the lower surface of the ingot, and two points (5, 6) were taken from the middle portion of the ingot, and the results are shown in tables 1 to 5.
TABLE 1 EXAMPLE 1 chemical composition analysis results of zirconium-nickel-copper-aluminum-tantalum master alloy ingot
Table 2 example 2 chemical composition analysis results of zirconium-nickel-copper-aluminum-tantalum intermediate alloy ingot
TABLE 3 EXAMPLE 3 chemical composition analysis results of zirconium-nickel-copper-aluminum-tantalum master alloy ingot
TABLE 4 example 4 chemical composition analysis results of zirconium-nickel-copper-aluminum-tantalum intermediate alloy ingot
TABLE 5 example 5 chemical composition analysis results of zirconium-nickel-copper-aluminum-tantalum intermediate alloy ingot
As can be seen from tables 1 to 5, the zirconium-nickel-copper-aluminum-tantalum intermediate alloy prepared in the embodiments 1 to 5 of the invention has high purity, uniform and stable components, less segregation and lower impurity content, and can better meet the production requirements of high-temperature alloys.
The chemical component analysis was performed on each of the zirconium-nickel-copper-aluminum-tantalum intermediate alloy ingots (cylinders) prepared in examples 1 to 5, and the optimal value results are shown in table 6.
TABLE 6 optimum results of zirconium-nickel-copper-aluminum-tantalum intermediate alloy ingots in examples 1-5
As can be seen from Table 6, the zirconium-nickel-copper-aluminum-tantalum master alloys prepared in the embodiments 1-5 of the present invention have uniform content and low impurity content, wherein Fe and Si are unavoidable impurities introduced by the raw materials.
Respectively smelting nickel-based high-temperature alloys by using the zirconium-nickel-copper-aluminum-tantalum intermediate alloy (A) provided by the embodiment 3 of the invention and a commercially available zirconium-nickel-copper-aluminum-tantalum high-temperature alloy (B) according to the same method; respectively obtaining a nickel-based superalloy A and a nickel-based superalloy B; the operation of smelting the nickel-based superalloy is carried out according to a conventional technology, and the specific flow is as follows: 1. mixing the raw materials with electrolytic nickel, performing intermediate frequency smelting 2, pouring the molten liquid obtained in the step one into a columnar shape 3, and smelting the columnar alloy by using an electric arc furnace to obtain the alloy.
The obtained nickel-base superalloy a and nickel-base superalloy B (cylinders) were sampled and subjected to chemical composition analysis, three points (1, 2, 3) were taken from the upper surface of the alloy ingot, three points (4, 5, 6) were taken from the lower surface of the alloy ingot, and three points (7, 8, 9) were taken from the middle section of the alloy ingot to perform composition analysis, and the results are shown in table 7.
TABLE 7 high-temp. alloy compositions smelted by two processes
As can be seen from Table 7, the nickel-based superalloy produced by the zirconium-nickel-copper-aluminum-tantalum intermediate alloy provided by the invention has the advantages of small segregation, uniform component content and low impurity content.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The zirconium-nickel-copper-aluminum-tantalum intermediate alloy comprises the following components in percentage by mass: 60.0 to 70.0 percent of zirconium, 6.0 to 8.0 percent of nickel, 9.0 to 12.0 percent of copper, 12.0 to 16.0 percent of tantalum and the balance of aluminum.
2. The method for preparing the zirconium-nickel-copper-aluminum-tantalum intermediate alloy as claimed in claim 1, which comprises the following steps:
(1) mixing zirconium dioxide, nickel oxide, copper oxide, aluminum and tantalum pentoxide to obtain a mixture;
(2) carrying out thermite reaction on one part of the mixture obtained in the step (1), adding the rest part of the mixture obtained in the step (1) in the thermite reaction process, and continuously carrying out thermite reaction to obtain a primary zirconium-nickel-copper-aluminum-tantalum alloy;
(3) sequentially adding one part and part of zirconium in the primary zirconium-nickel-copper-aluminum-tantalum alloy obtained in the step (2) and the rest part of the primary zirconium-nickel-copper-aluminum-tantalum alloy obtained in the step (2) into a heated container to perform vacuum induction melting to obtain a melt;
(4) and (4) adding the rest of zirconium into the melt obtained in the step (3), continuing vacuum induction smelting, and then sequentially carrying out vacuum induction refining and cooling to obtain the zirconium-nickel-copper-aluminum-tantalum alloy.
3. The method according to claim 2, wherein the zirconium dioxide, nickel oxide, copper oxide, aluminum and tantalum pentoxide in step (1) are dried.
4. The preparation method according to claim 3, wherein the drying temperature is 110-120 ℃ and the drying time is 6-20 h.
5. The preparation method according to claim 2, wherein the mass ratio of zirconium dioxide, nickel oxide, copper oxide, aluminum and tantalum pentoxide in the step (1) is (2.80-2.93): (0.52-0.58): (0.6-1.0): (1.56-1.60): 1.00.
6. the preparation method according to claim 2, wherein the part of the mixed material in the step (2) is 45-55% of the total mass of the mixed material.
7. The method according to claim 2, wherein the amount of zirconium in step (3) is 60 to 80% by mass based on the total mass of zirconium.
8. The preparation method according to claim 2, wherein the mass ratio of the total mass of the part of zirconium in the step (3) and the rest of zirconium in the step (4) to the mass ratio of the primary zirconium-nickel-copper-aluminum-tantalum alloy obtained in the step (2) is (0.50-1.00): (1.50-2.00).
9. The method according to claim 2, wherein the power of the vacuum induction refining in the step (4) is 95-105 kW.
10. The production method according to claim 2, wherein the cooling in the step (4) is performed under vacuum.
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