CN117867359A - Refractory high-entropy superalloy with good room-temperature tensile plasticity and preparation method thereof - Google Patents
Refractory high-entropy superalloy with good room-temperature tensile plasticity and preparation method thereof Download PDFInfo
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- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 57
- 239000002184 metal Substances 0.000 claims abstract description 57
- 239000000956 alloy Substances 0.000 claims abstract description 38
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 37
- 238000005266 casting Methods 0.000 claims abstract description 25
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 21
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 16
- 150000002739 metals Chemical class 0.000 claims abstract description 14
- 238000004321 preservation Methods 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 14
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 238000005097 cold rolling Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
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- 239000002994 raw material Substances 0.000 claims description 49
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 34
- 229910052802 copper Inorganic materials 0.000 claims description 34
- 239000010949 copper Substances 0.000 claims description 34
- 239000010453 quartz Substances 0.000 claims description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 24
- 239000010936 titanium Substances 0.000 claims description 17
- 229910052719 titanium Inorganic materials 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 16
- 238000005086 pumping Methods 0.000 claims description 16
- 238000003723 Smelting Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- IADRPEYPEFONML-UHFFFAOYSA-N [Ce].[W] Chemical compound [Ce].[W] IADRPEYPEFONML-UHFFFAOYSA-N 0.000 claims description 12
- 238000005498 polishing Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000010791 quenching Methods 0.000 claims description 7
- 230000000171 quenching effect Effects 0.000 claims description 7
- 244000137852 Petrea volubilis Species 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
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- 229910052758 niobium Inorganic materials 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 241001062472 Stokellia anisodon Species 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 229910052715 tantalum Inorganic materials 0.000 claims description 5
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 claims description 3
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- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000003754 machining Methods 0.000 claims description 2
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 239000000306 component Substances 0.000 description 4
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- 238000013461 design Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
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- 230000018109 developmental process Effects 0.000 description 2
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
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- 239000000758 substrate Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
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Abstract
The invention provides a refractory high-entropy superalloy with good room-temperature tensile plasticity and a preparation method thereof, wherein the refractory high-entropy superalloy consists of Al, nb, ti and Zr elements, and has a general formula of AlNbTiZr; the atomic percentages of the elements in the refractory high-entropy superalloy are respectively as follows: 5% -10%, nb:30% -40%, ti:30% -40%, zr:20% -30%. The preparation method of the refractory high-entropy superalloy comprises the following steps: firstly, mixing four simple substance metals of weighed Al, nb, ti and Zr, carrying out vacuum arc melting on the mixture, carrying out suction casting forming to obtain an as-cast alloy plate, and then sequentially carrying out cold rolling and heat preservation treatment on the as-cast alloy plate to obtain refractory high-entropy alloy AlNbTiZr. The invention has reasonable conception, and the prepared alloy has good mechanical property and high yield strength and tensile plasticity.
Description
Technical Field
The invention relates to the field of alloy material design, in particular to a refractory high-entropy superalloy with good room-temperature tensile plasticity and a preparation method thereof.
Background
Aircraft engines are the core components of all aircraft, and play a decisive role in the service performance and safety of the aircraft. With the development of high thrust weight and high power ratio engines, aircraft are increasingly demanding in terms of heat resistant components. Conventional metals and alloys may face more serious challenges in the face of future aircraft developments. In recent years, high-entropy alloys, particularly refractory high-entropy alloys having a body-centered cubic structure, have attracted considerable attention. Such alloys generally have a plurality of principal elements, and the content of each principal element is at or near equiatomic ratio. The refractory high-entropy alloy is a high-entropy alloy designed based on elements (Ti, zr, hf, V, nb, ta, cr, mo, W) in fourth, fifth and sixth groups of the periodic table. Compared with the traditional alloy, the alloy has higher composition design space and hopefully meets more severe design requirements. Meanwhile, the melting point of the refractory high-entropy alloy is generally higher, so that the refractory high-entropy alloy is beneficial to realizing service in a higher-temperature environment. Driven by this concept, we successfully introduced the classical gamma-gamma' super structure in nickel-based alloys into refractory high-entropy alloys, forming a refractory high-entropy superalloy with nano-precipitates. Superalloys generally refer to a class of alloys that has a volume fraction of ordered phase particles similar to conventional nickel-based alloys, and a coherent or semi-coherent relationship between the particles and the substrate.
Disclosure of Invention
Aiming at the technical problems in the background technology, the invention provides a refractory high-entropy superalloy with reasonable conception, good mechanical property, high yield strength and tensile plasticity and good room-temperature tensile plasticity and a preparation method thereof.
In order to solve the technical problems, the refractory high-entropy superalloy with good room-temperature tensile plasticity provided by the invention consists of Al, nb, ti and Zr elements, and has a general formula of AlNbTiZr; the atomic percentages of the elements in the refractory high-entropy superalloy are respectively as follows: 5% -10%, nb:30% -40%, ti:30% -40%, zr:20% -30%.
The refractory high entropy superalloy with good room temperature stretch plasticity, wherein: the refractory high-entropy superalloy has a room temperature yield strength of 1120MPa and a plastic deformation of 11.0%.
A process for preparing refractory high-entropy superalloy with good room-temp stretch plasticity includes such steps as mixing the weighed Al, nb, ti and Zr, vacuum arc smelting, suction casting to obtain cast alloy sheet, cold rolling and thermal insulating.
The preparation method of the refractory high-entropy superalloy with good room temperature tensile plasticity comprises the following steps:
(1) Selecting blocky raw materials of four simple substance metals of Al, nb, ti and Zr, polishing the surfaces of the blocky raw materials of the four simple substance metals, cleaning the surfaces by using an ultrasonic cleaner, weighing the materials, and cleaning the surfaces by using the ultrasonic cleaner again;
(2) Sequentially placing the weighed blocky raw materials of four simple substances of metals into a vacuum arc furnace according to the sequence of Al, ti, zr and Nb, and then introducing protective gas for smelting to obtain button ingots;
(3) Cutting 10-15 g of raw materials from the obtained button ingot, polishing the cut marks, cleaning the button ingot by using an ultrasonic cleaning machine, then repeating the step (2) to smelt the button ingot, and then placing the cut raw materials into a copper mold for suction casting;
(4) Removing the copper mould, taking out the metal sheet obtained after suction casting, and rolling the metal sheet at room temperature;
(5) Polishing the rolled metal sheet, cleaning the metal sheet by an ultrasonic cleaner, packaging the metal sheet, filling the metal sheet into a quartz tube, and sealing the quartz tube after filling high-purity argon and vacuumizing in a vacuum system;
(6) And (3) preserving the heat of the quartz tube sealed with the metal sheet for 2-5 hours at 600-700 ℃, taking out the metal sheet from the quartz tube after the heat preservation is finished, throwing the metal sheet into water for quenching, and obtaining the refractory high-entropy superalloy after the quenching is finished.
The preparation method of the refractory high-entropy superalloy with good room temperature tensile plasticity comprises the following steps: in the step (1), the atomic percentages of the bulk raw materials of the four simple substance metals of Al, nb, ti and Zr are respectively: 5% -10%, nb:30% -40%, ti:30% -40%, zr:20% -30%;
the purity of the blocky raw materials of the four simple substance metals of Al, nb, ti and Zr in the step (1) is higher than 99.9 weight percent, and the weight error of each time is not higher than +/-0.005 g;
the metal sheet is rolled to 0.35-0.45 mm at room temperature, and the nominal deformation is 80%;
the refractory high-entropy superalloy obtained in step (6) has a room temperature yield strength of 1120MPa and a plastic deformation of 11.0%.
The preparation method of the refractory high-entropy superalloy with good room temperature tensile plasticity comprises the following specific processes of:
(2.1) sequentially placing the weighed four metal block raw materials into a raw material station on a copper crucible of a vacuum arc furnace according to the sequence of Al, ti, zr and Nb;
(2.2) closing the furnace door of the vacuum arc furnace, sequentially opening a mechanical pump and a molecular pump of a vacuum pumping system of the vacuum arc furnace, and pumping the vacuum degree in the vacuum arc furnace to 1.5 multiplied by 10 -3 The following are set forth;
(2.3) introducing argon with purity of more than 99.99wt% into the vacuum arc furnace as protective gas, and maintaining the pressure in the vacuum arc furnace at 0.06Mpa;
(2.4) adjusting the position of the tip of the tungsten-cerium electrode of the vacuum arc furnace to be 2-5 mm above the titanium ingot on the arc striking station of the copper crucible, and directly increasing the current of the tungsten-cerium electrode of the vacuum arc furnace to 480-500A to smelt the titanium ingot after the arc striking is successful, so as to further reduce the oxygen-nitrogen concentration in the furnace, wherein the smelting time is not less than 2 minutes; after smelting is finished and the titanium ingot is cooled, showing metallic light color again to ensure that the titanium ingot does not turn yellow or blue;
(2.5) repeating the arc striking operation in the step (2.4), then moving the tip of the tungsten-cerium electrode to be about 10mm above a raw material station on the copper crucible, increasing the current of a vacuum arc furnace to 480-500A, melting all raw materials in the raw material station on the copper crucible, then starting timing to keep the raw material molten state for 3 minutes, then standing and cooling and solidifying on the raw material station of the copper crucible, and simultaneously, introducing cooling circulating water under the copper crucible, wherein the water temperature of the circulating water is kept at 19-25 ℃;
(2.6) after smelting is completed, overturning the button ingot cooled and solidified on a raw material station of the copper crucible by using a manipulator;
(2.7) repeating the arc striking, smelting and overturning operation procedures in the step (2.6) at least 8 times to ensure that the components of the button ingot are uniform; after the button ingot is uniformly smelted, cooling the button ingot to room temperature, waiting for 5-8 minutes, reducing the temperature of the button ingot to room temperature, removing waste gas in the vacuum arc furnace, opening a furnace door of the vacuum arc furnace, and taking out the button ingot.
The preparation method of the refractory high-entropy superalloy with good room temperature tensile plasticity comprises the following specific processes of:
cutting 10-15 g of raw materials from the obtained button ingot by utilizing wire electric discharge machining, polishing the cut marks by using sand paper, and cleaning by using an ultrasonic cleaner;
(3.2) repeating the steps (2.1) - (2.4) until the titanium ingot is not discolored, placing the cut raw materials on a suction casting station on a copper crucible of a vacuum arc furnace by using a manipulator, completing arc striking operation, moving the tip of a tungsten cerium electrode to the position above the suction casting station, and increasing the current of the vacuum arc furnace until the button ingot is completely melted; under the condition of ensuring that the raw materials are sufficiently melted, a suction casting valve below a suction casting station is pressed down, and molten metal is sucked into a copper mold of a vacuum arc furnace for suction casting, so that a plate-shaped cast alloy, namely a metal sheet, is obtained.
The preparation method of the refractory high-entropy superalloy with good room temperature tensile plasticity comprises the following steps: the length, width and thickness of the cavity of the copper mold are 60mm, 10mm and 2mm.
The preparation method of the refractory high-entropy superalloy with good room temperature tensile plasticity comprises the following specific processes of:
(5.1) polishing the surface of the rolled plate by sand paper, and cleaning by an ultrasonic cleaning machine;
(5.2) wrapping the plate with a tantalum thin film with the thickness of 0.025mm, putting the tantalum thin film into a quartz tube, and then, putting the quartz tube into a vacuum pumping system of a vacuum arc furnace, starting a pump group of the vacuum pumping system to pump vacuum, closing a vacuum valve of the vacuum pumping system, filling argon with the purity of 0.8 atmosphere being more than 99.99wt%, and then, pumping vacuum;
and (5.3) repeating the air charging and vacuumizing process in the step (5.2) for 6 times, and sealing the quartz tube after the last vacuumizing process is finished.
The preparation method of the refractory high-entropy superalloy with good room temperature tensile plasticity comprises the following specific processes of:
(6.1) heating the box-type resistance furnace to 650 ℃ for heat preservation, and then placing the quartz tube with the sealed metal sheet into the box-type resistance furnace for heat preservation for 2 hours;
and (6.2) after heat preservation, taking out the quartz tube, quickly breaking the quartz tube, taking out the wrapped metal plate, and throwing the wrapped metal plate into water for quenching.
By adopting the technical scheme, the invention has the following beneficial effects:
the preparation method of the refractory high-entropy superalloy with good room temperature tensile plasticity is reasonable in conception, four metal simple substances of Al, nb, ti and Zr are firstly smelted by a vacuum arc furnace, an as-cast alloy sheet is obtained by suction casting and molding, then 80% of the as-cast alloy sheet is cold-rolled, and finally the refractory high-entropy superalloy with excellent technological characteristics and mechanical properties and nano precipitated phases is obtained by heat preservation treatment at 650 ℃.
The AlNbTiZr non-equal atom high entropy alloy prepared by the preparation method has a unique BCC+B2 microstructure, and is similar to a classical gamma-gamma' super structure in Ni-based superalloy; meanwhile, the prepared alloy has good strength-plastic combination at room temperature, good mechanical property, high yield strength and tensile plasticity, 1120MPa of room temperature yield strength and 11.0% of plastic deformation, and great application potential in heat-resistant parts of an aeroengine.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings which are required in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are some embodiments of the invention and that other drawings may be obtained from these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method of preparing a refractory high entropy superalloy of the present invention having good room temperature stretch plasticity;
FIG. 2 is a schematic illustration of a HADDF-STEM and EDS of a refractory high entropy superalloy of the present invention having good room temperature stretch plasticity;
FIG. 3 is a graphical representation of stress-strain curves for refractory high-entropy superalloys with good room temperature stretch plasticity in accordance with the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention is further illustrated with reference to specific embodiments.
As shown in FIG. 1, the refractory high-entropy superalloy with good room-temperature tensile plasticity consists of Al, nb, ti and Zr elements, and has a general formula of AlNbTiZr; the atomic percentages of the elements in the refractory high-entropy superalloy are respectively as follows: 5% -10%, nb:30% -40%, ti:30% -40%, zr:20% -30%.
The refractory high-entropy alloy of the invention has a room temperature yield strength of 1120MPa and a plastic deformation of 11.0%.
As shown in fig. 1, the refractory high-entropy alloy of the present invention has nano precipitated phases, i.e., nano-scale precipitated phases in the form of spheres.
As shown in fig. 2, the preparation method of the refractory high-entropy superalloy with good room temperature tensile plasticity provided in the embodiment specifically includes the following steps:
(1) Selecting bulk raw materials of four simple substance metals of Al, nb, ti and Zr, grinding surface oxide skin by using a file, and then cleaning by using an ultrasonic cleaner. The purity of the raw materials is higher than 99.9 and wt percent. The mass of each button ingot melted is 70 g, and the mass of each element weighed each time can be calculated according to the mass. Wherein the alloy parent ingot comprises 5-10% of aluminum, 30-40% of niobium and titanium and 20-30% of zirconium. The atomic percent is converted into specific weighing mass, the three positions are accurate to decimal places, and the mass error of each weighing is not higher than +/-0.005 g. And after weighing, cleaning again by using an ultrasonic cleaner.
(2) And (3) sequentially placing weighed metal block raw materials into raw material stations on a copper crucible of a vacuum arc furnace according to the sequence of Al, ti, zr and Nb. Closing a furnace door of the vacuum arc furnace, sequentially opening a mechanical pump and a molecular pump of a vacuumizing system of the vacuum arc furnace, and vacuumizing the vacuum arc furnace to 1.5X10 -3 The following is given. And then introducing high-purity argon (the purity is more than 99.99 wt%) into the vacuum arc furnace as a protective gas, and maintaining the pressure in the vacuum arc furnace at 0.06 MPa. And then, adjusting the position of the tip of the tungsten-cerium electrode of the vacuum arc furnace to 2-5 mm above the titanium ingot on the arc striking station of the copper crucible, and directly increasing the current of the tungsten-cerium electrode of the vacuum arc furnace to 480-500A to smelt the titanium ingot after the arc striking is successful, so as to further reduce the oxygen-nitrogen concentration in the furnace, wherein the smelting time is not less than 2 minutes. After the smelting is finished and the titanium ingot is cooled, the metallic light color is displayed again, so that the titanium ingot is ensured not to turn yellow or blue. And repeating the arc striking operation, then moving the tip of the tungsten-cerium electrode to about 10mm above the raw material station, increasing the current of the vacuum arc furnace to 480-500A, and melting all raw materials in the raw material station on the copper crucible. And then, starting timing and keeping the raw material in a molten state for 3 minutes, and then standing, cooling and solidifying on a raw material station of the copper crucible, wherein cooling circulating water is introduced under the copper crucible, and the water temperature of the circulating water is kept at 19-25 ℃. And after smelting is completed, overturning the button ingot cooled and solidified on the raw material station of the copper crucible by using a mechanical arm. The same arc striking, smelting and overturning operation procedures are repeated for at least 8 times, so that the components of the button ingot are ensured to be uniform. After the button ingot is evenly smeltedAnd (3) cooling the button ingot to room temperature, waiting for 5-8 minutes, cooling the button ingot to room temperature, removing waste gas in the vacuum arc furnace, opening a furnace door of the vacuum arc furnace, and taking out the button ingot.
(3) And cutting 10-15 g of raw materials from the obtained button ingot by utilizing wire electric discharge cutting, polishing the cut marks by using sand paper, and cleaning by using an ultrasonic cleaning machine. And (2) repeating the step until the titanium ingot is not discolored, and placing the cut raw materials on a suction casting station on a copper crucible of a vacuum arc furnace by using a manipulator. And (3) completing arc striking operation, moving the tip of the tungsten-cerium electrode to the position above the suction casting station, and increasing the current of the vacuum arc furnace until the button ingot is completely melted. Under the condition of ensuring that the raw materials are sufficiently melted, a suction casting valve below a suction casting station is pressed down, and molten metal is sucked into a copper mold of a vacuum arc furnace for suction casting, so that a plate-shaped cast alloy, namely a metal sheet with the thickness of 2mm is obtained. The cavity size of the copper mold used for suction casting was 60mm×10mm×2mm (length×width×thickness).
(4) Removing the copper mould, and taking out the metal sheet obtained after suction casting; rolling the metal sheet to 0.35-0.45 mm at room temperature, wherein the nominal deformation is 80%, and preserving the temperature of the deformed metal sheet at 650 ℃ for 2-5 hours; wherein the rotational speed of the rolling mill is 200mm/s when the rolling mill is idling; the sheet metal in this example was cold rolled to 0.4mm at room temperature.
(5) And polishing the surface of the rolled plate by using sand paper, and cleaning by using an ultrasonic cleaning machine. Then wrapping a plate material with a tantalum thin film with the thickness of 0.025mm (wrapping and sealing an alloy in a vacuum quartz tube by using a Ta thin film to avoid oxidization), putting the plate material into a quartz tube with proper size, and then, putting the quartz tube into a vacuum pumping system of a vacuum arc furnace, starting a pump group of the vacuum pumping system to pump vacuum, closing a vacuum valve of the vacuum pumping system, and filling high-purity argon gas with the pressure of 0.8 atmosphere (the purity is more than 99.99wt percent), and then, pumping vacuum; the process of inflating and vacuumizing is repeated for 6 times, and the quartz tube is sealed after the last vacuumizing is finished.
(6) The deformed metal sheet is insulated for 2-5 hours at 600-700 ℃ (the best implementation value is 650 ℃), in the embodiment, the box-type resistance furnace is heated to 650 ℃ for heat preservation, and then the quartz tube with the sealed plate is placed into the furnace for heat preservation for 2 hours; after the heat preservation is finished, taking out the quartz tube, quickly breaking the quartz tube, taking out the wrapped metal sheet, throwing into water and quenching; after the experiment is finished, the surface of the metal sheet still has good metallic luster.
HAADF-STEM (scanning transmission electron microscopic analysis) was performed on the obtained refractory high-entropy alloy, and room temperature tensile test was performed. In the HAADF-STEM of fig. 1, a globular nanoscale precipitate phase was observed and there was significant component segregation with the matrix. From FIG. 3, it can be determined that the refractory high-entropy alloy has a room temperature yield strength of 1120MPa and a plastic deformation of 11.0%.
The invention has reasonable conception, and the prepared refractory high-entropy alloy has good mechanical property, high yield strength and high tensile plasticity.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. The refractory high-entropy superalloy with good room-temperature tensile plasticity is characterized in that the refractory Gao Shangchao alloy consists of Al, nb, ti and Zr elements, and has a general formula of AlNbTiZr; the atomic percentages of the elements in the refractory high-entropy superalloy are respectively as follows: 5% -10%, nb:30% -40%, ti:30% -40%, zr:20% -30%.
2. A refractory high entropy superalloy with good room temperature stretch plasticity as in claim 1, wherein: the refractory high-entropy superalloy has a room temperature yield strength of 1120MPa and a plastic deformation of 11.0%.
3. A preparation method of refractory high-entropy super alloy with good room temperature stretch plasticity is characterized by comprising the following steps: firstly, mixing four simple substance metals of weighed Al, nb, ti and Zr, carrying out vacuum arc melting on the mixture, carrying out suction casting forming to obtain an as-cast alloy plate, and then sequentially carrying out cold rolling and heat preservation treatment on the as-cast alloy plate to obtain refractory high-entropy alloy AlNbTiZr.
4. A method for preparing a refractory high entropy superalloy with good room temperature stretch plasticity as claimed in claim 3, wherein the method comprises the steps of:
(1) Selecting blocky raw materials of four simple substance metals of Al, nb, ti and Zr, polishing the surfaces of the blocky raw materials of the four simple substance metals, cleaning the surfaces by using an ultrasonic cleaner, weighing the materials, and cleaning the surfaces by using the ultrasonic cleaner again;
(2) Sequentially placing the weighed blocky raw materials of four simple substances of metals into a vacuum arc furnace according to the sequence of Al, ti, zr and Nb, and then introducing protective gas for smelting to obtain button ingots;
(3) Cutting 10-15 g of raw materials from the obtained button ingot, polishing the cut marks, cleaning the button ingot by using an ultrasonic cleaning machine, then repeating the step (2) to smelt the button ingot, and then placing the cut raw materials into a copper mold for suction casting;
(4) Removing the copper mould, taking out the metal sheet obtained after suction casting, and rolling the metal sheet at room temperature;
(5) Polishing the rolled metal sheet, cleaning the metal sheet by an ultrasonic cleaner, packaging the metal sheet, filling the metal sheet into a quartz tube, and sealing the quartz tube after filling high-purity argon and vacuumizing in a vacuum system;
(6) And (3) preserving the heat of the quartz tube sealed with the metal sheet for 2-5 hours at 600-700 ℃, taking out the metal sheet from the quartz tube after the heat preservation is finished, throwing the metal sheet into water for quenching, and obtaining the refractory high-entropy superalloy after the quenching is finished.
5. The method for preparing a refractory high entropy superalloy with good room temperature stretch plasticity as defined in claim 4, wherein: in the step (1), the atomic percentages of the bulk raw materials of the four simple substance metals of Al, nb, ti and Zr are respectively: 5% -10%, nb:30% -40%, ti:30% -40%, zr:20% -30%;
the purity of the blocky raw materials of the four simple substance metals of Al, nb, ti and Zr in the step (1) is higher than 99.9 weight percent, and the weight error of each time is not higher than +/-0.005 g;
the metal sheet is rolled to 0.35-0.45 mm at room temperature, and the nominal deformation is 80%;
the refractory high-entropy superalloy obtained in step (6) has a room temperature yield strength of 1120MPa and a plastic deformation of 11.0%.
6. The method for preparing a refractory high-entropy superalloy with good room temperature stretch plasticity according to claim 4 wherein the specific process of step (2) is:
(2.1) sequentially placing the weighed four metal block raw materials into a raw material station on a copper crucible of a vacuum arc furnace according to the sequence of Al, ti, zr and Nb;
(2.2) closing the furnace door of the vacuum arc furnace, sequentially opening a mechanical pump and a molecular pump of a vacuum pumping system of the vacuum arc furnace, and pumping the vacuum degree in the vacuum arc furnace to 1.5 multiplied by 10 -3 The following are set forth;
(2.3) introducing argon with purity of more than 99.99wt% into the vacuum arc furnace as protective gas, and maintaining the pressure in the vacuum arc furnace at 0.06Mpa;
(2.4) adjusting the position of the tip of the tungsten-cerium electrode of the vacuum arc furnace to be 2-5 mm above the titanium ingot on the arc striking station of the copper crucible, and directly increasing the current of the tungsten-cerium electrode of the vacuum arc furnace to 480-500A to smelt the titanium ingot after the arc striking is successful, so as to further reduce the oxygen-nitrogen concentration in the furnace, wherein the smelting time is not less than 2 minutes; after smelting is finished and the titanium ingot is cooled, showing metallic light color again to ensure that the titanium ingot does not turn yellow or blue;
(2.5) repeating the arc striking operation in the step (2.4), then moving the tip of the tungsten-cerium electrode to be about 10mm above a raw material station on the copper crucible, increasing the current of a vacuum arc furnace to 480-500A, melting all raw materials in the raw material station on the copper crucible, then starting timing to keep the raw material molten state for 3 minutes, then standing and cooling and solidifying on the raw material station of the copper crucible, and simultaneously, introducing cooling circulating water under the copper crucible, wherein the water temperature of the circulating water is kept at 19-25 ℃;
(2.6) after smelting is completed, overturning the button ingot cooled and solidified on a raw material station of the copper crucible by using a manipulator;
(2.7) repeating the arc striking, smelting and overturning operation procedures in the step (2.6) at least 8 times to ensure that the components of the button ingot are uniform; after the button ingot is uniformly smelted, cooling the button ingot to room temperature, waiting for 5-8 minutes, reducing the temperature of the button ingot to room temperature, removing waste gas in the vacuum arc furnace, opening a furnace door of the vacuum arc furnace, and taking out the button ingot.
7. The method for preparing a refractory high-entropy superalloy with good room temperature stretch plasticity according to claim 6 wherein the specific process of step (3) is:
cutting 10-15 g of raw materials from the obtained button ingot by utilizing wire electric discharge machining, polishing the cut marks by using sand paper, and cleaning by using an ultrasonic cleaner;
(3.2) repeating the steps (2.1) - (2.4) until the titanium ingot is not discolored, placing the cut raw materials on a suction casting station on a copper crucible of a vacuum arc furnace by using a manipulator, completing arc striking operation, moving the tip of a tungsten cerium electrode to the position above the suction casting station, and increasing the current of the vacuum arc furnace until the button ingot is completely melted; under the condition of ensuring that the raw materials are sufficiently melted, a suction casting valve below a suction casting station is pressed down, and molten metal is sucked into a copper mold of a vacuum arc furnace for suction casting, so that a plate-shaped cast alloy, namely a metal sheet, is obtained.
8. The method for preparing a refractory high entropy superalloy with good room temperature stretch plasticity according to claim 7 wherein: the length, width and thickness of the cavity of the copper mold are 60mm, 10mm and 2mm.
9. The method for preparing a refractory high-entropy superalloy with good room temperature stretch plasticity according to claim 4 wherein the specific process of step (5) is:
(5.1) polishing the surface of the rolled plate by sand paper, and cleaning by an ultrasonic cleaning machine;
(5.2) wrapping the plate with a tantalum thin film with the thickness of 0.025mm, putting the tantalum thin film into a quartz tube, and then, putting the quartz tube into a vacuum pumping system of a vacuum arc furnace, starting a pump group of the vacuum pumping system to pump vacuum, closing a vacuum valve of the vacuum pumping system, filling argon with the purity of 0.8 atmosphere being more than 99.99wt%, and then, pumping vacuum;
and (5.3) repeating the air charging and vacuumizing process in the step (5.2) for 6 times, and sealing the quartz tube after the last vacuumizing process is finished.
10. The method for preparing a refractory high-entropy superalloy with good room temperature stretch plasticity according to claim 4 wherein step (6) is performed as follows:
(6.1) heating the box-type resistance furnace to 650 ℃ for heat preservation, and then placing the quartz tube with the sealed metal sheet into the box-type resistance furnace for heat preservation for 2 hours;
and (6.2) after heat preservation, taking out the quartz tube, quickly breaking the quartz tube, taking out the wrapped metal plate, and throwing the wrapped metal plate into water for quenching.
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