A tantalum-titanium-zirconium high-entropy alloy and a preparation method thereof

The production of a tantalum-titanium-zirconium high-entropy alloy through magnetic sputtering addresses the corrosion and stability challenges in nuclear power equipment, providing improved high-temperature resistance and mechanical strength for nuclear power components.

CN116083773BActive Publication Date: 2025-07-15XI AN JIAOTONG UNIV
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Patent Information

Application Number
CN202310266303.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-03-17
Publication Date
2025-07-15
Estimated Expiration
2043-03-17

AI Technical Summary

Technical Problem

When nuclear power equipment components are in service under high temperature, high oxygen and irradiation environments, the existing materials have insufficient oxidation, radiation and high temperature resistance, resulting in corrosion and failure problems.

Method used

Magneto-controlled sputtering technology is used to prepare tantalum titanium zirconium high-entropy alloy on the matrix. The alloy element content is regulated by co-sputtering of different target materials to form a uniform amorphous structure. Combined with vacuum annealing treatment, the stability and oxidation resistance of the alloy are improved.

Benefits of technology

The prepared tantalum titanium zirconium high-entropy alloy has excellent mechanical strength and high temperature stability, and can maintain an amorphous structure above 500°C, significantly improving the oxidation and radiation resistance of nuclear power equipment components.

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Abstract

The present invention discloses a tantalum-titanium-zirconium high-entropy alloy and a preparation method thereof. The tantalum-titanium-zirconium high-entropy alloy is prepared on a substrate by a magnetron sputtering method in a vacuum environment; the sum of the atomic percentages of titanium and zirconium in the tantalum-titanium-zirconium high-entropy alloy is greater than 50%. The obtained substrate is cooled to room temperature in a vacuum and finally vacuum annealed to obtain an annealed tantalum-titanium-zirconium high-entropy alloy. This tantalum-titanium-zirconium high-entropy alloy has a greater atomic disorder at high temperatures, and the alloy structure is still amorphous and becomes more stable, having high thermal stability and the ability to resist high-temperature oxidation. At the same time, Ta, Ti, and Zr elements are prone to form a dense oxide film and have characteristics such as amorphous, single-phase, and low free enthalpy, which all contribute to the excellent corrosion resistance of the high-entropy alloy.
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Description

Technical Field

[0001] The present invention belongs to the field of metal structural materials, and particularly relates to a tantalum-titanium-zirconium high-entropy alloy and a preparation method thereof. Background Art

[0002] With the rapid development of science and technology, the development and utilization of clean energy have received increasing attention from countries. Nuclear power is an efficient and environmentally friendly clean energy and an energy project that countries around the world are vigorously investing in. However, the equipment components used in the nuclear power field serve in an oxidative, high-temperature, and irradiated environment for a long time, which puts increasingly high requirements on the antioxidant, anti-irradiation, and high-temperature resistance properties of materials. Not only are high-temperature strength and stability required for equipment materials, but also good high-temperature oxidation and anti-irradiation properties are required.

[0003] Due to the complex working conditions of equipment components in the nuclear power industry, accompanied by high temperature, high oxygen, and strong corrosion environments, this may cause irreparable damage to precision equipment, and even cause personal injury and property losses. Therefore, the precision equipment components in the nuclear power industry must be effectively protected to avoid damage to the equipment components caused by the working environment.

[0004] For example, in the third-generation water reactor nuclear power plant, the steam corrosion of zirconium-based nuclear cladding tubes in a high-temperature water environment may generate hydrogen and trigger a hydrogen explosion, such as the Fukushima nuclear power plant accident; in the fourth-generation lead-bismuth reactor, the lead-bismuth corrosion of steel-based nuclear cladding in a lead-bismuth environment, and the lead-bismuth element has a corrosive effect on the Ni element in the steel nuclear cladding tube, resulting in the failure of the steel. Therefore, the nuclear cladding tubes in nuclear power plants need to be treated with anti-corrosion protection, and adding a TaTiZr coating on the surface of the nuclear cladding tube can effectively prevent corrosion from occurring. Summary of the Invention

[0005] Aiming at the problems existing in the prior art, the present invention provides a tantalum-titanium-zirconium high-entropy alloy and a preparation method thereof. The prepared tantalum-titanium-zirconium high-entropy alloy has a uniform microstructure and excellent mechanical strength, effectively improving the service life of the material.

[0006] The present invention is realized through the following technical solutions:

[0007] A preparation method of a tantalum-titanium-zirconium high-entropy alloy, comprising the following steps:

[0008] Step 1, in a vacuum environment, a tantalum-titanium-zirconium high-entropy alloy is prepared on a substrate by a magnetron sputtering method;

[0009] In the tantalum-titanium-zirconium high-entropy alloy, the sum of the atomic percentages of titanium and zirconium is greater than 50%, the sputtering power is 200 W, and the deposition pressure is 1.0 Pa;

[0010] Step 2, the substrate obtained in Step 1 is cooled to room temperature in a vacuum to obtain a tantalum-titanium-zirconium high-entropy alloy;

[0011] Step 3: Vacuum anneal the tantalum-titanium-zirconium high-entropy alloy obtained in Step 2 to obtain an annealed tantalum-titanium-zirconium high-entropy alloy.

[0012] Preferably, in Step 1, after the substrate is cleaned and dried, magnetron co-sputtering is carried out in a vacuum environment.

[0013] Preferably, the method for cleaning and drying the substrate is as follows:

[0014] The polished substrate is ultrasonically cleaned in acetone and alcohol for 10 minutes in sequence, and then dried. The roughness of the polished surface of the substrate is less than 0.8 nm.

[0015] Preferably, the method of magnetron sputtering in Step 1 is that two TaTiZr alloy targets are co-sputtered using a DC power supply.

[0016] Preferably, the vacuum degree of the vacuum environment in Step 1 is less than 4.0×10 -4 Pa.

[0017] Preferably, during the magnetron co-sputtering process, the deposition temperature is room temperature, the substrate rotation speed is 15 r / min, and the deposition time is 16000 s.

[0018] Preferably, the vacuum degree of the vacuum annealing in Step 3 is below 7×10 -4 Pa, the annealing temperature is room temperature - 500 °C, and the annealing time is 2 h.

[0019] A tantalum-titanium-zirconium high-entropy alloy, in which the sum of the atomic percentages of titanium and zirconium is greater than 50%, and the tantalum-titanium-zirconium high-entropy alloy is an amorphous structure.

[0020] Preferably, the nanoindentation hardness of the tantalum-titanium-zirconium high-entropy alloy is 6 GPa - 8 GPa.

[0021] Compared with the prior art, the present invention has the following beneficial technical effects:

[0022] The preparation method of the tantalum-titanium-zirconium high-entropy alloy provided by the present invention utilizes the advantages of magnetron sputtering technology to regulate the content of alloying elements through co-sputtering of different targets. In the tantalum-titanium-zirconium high-entropy alloy, the sum of the atomic percentages of titanium and zirconium is greater than 50%. Due to the relatively large number of components in the tantalum-titanium-zirconium high-entropy alloy, the mixing entropy is also relatively large, the Gibbs free energy is relatively low, and the system is relatively stable. At high temperatures, the tantalum-titanium-zirconium high-entropy alloy will have a greater degree of atomic disorder, and the alloy structure is still amorphous and becomes more stable, with high thermal stability and the ability to resist high-temperature oxidation. Ta, Ti, and Zr elements are prone to form a dense oxide film and have characteristics such as amorphous, single-phase, and low free enthalpy, which all contribute to excellent corrosion resistance, and the prepared tantalum-titanium-zirconium high-entropy alloy has uniform element distribution, an amorphous structure, and excellent properties. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 XRD result diagram of the alloys of the tantalum-titanium-zirconium high-entropy alloy of the present invention with different annealing systems;

[0024] Figure 2 TEM microstructure and diffraction spot pictures of the alloys of the tantalum-titanium-zirconium high-entropy alloy of the present invention with different annealing systems

[0025] Figure 3 EDS scanning element distribution diagram of the microstructure of the alloys of the tantalum-titanium-zirconium high-entropy alloy of the present invention with different annealing systems;

[0026] Figure 4 Load-displacement curves of the alloys of the tantalum-titanium-zirconium high-entropy alloy of the present invention with different annealing systems;

[0027] Figure 5 Nano-indentation hardness results of the alloys of the tantalum-titanium-zirconium high-entropy alloy of the present invention with different annealing systems. DETAILED DESCRIPTION OF THE INVENTION

[0028] The following further describes the present invention in detail with reference to the drawings, which is an explanation rather than a limitation of the present invention.

[0029] A tantalum-titanium-zirconium high-entropy alloy, in which the sum of the atomic contents of titanium and zirconium in the tantalum-titanium-zirconium high-entropy alloy is greater than 50%, is prepared by a magnetron sputtering co-sputtering method. The structure of the tantalum-titanium-zirconium high-entropy alloy is an amorphous structure, and the temperature at which this amorphous structure is maintained is as high as 500 °C.

[0030] The present invention also provides a preparation method of a tantalum-titanium-zirconium high-entropy alloy, which includes the following steps;

[0031] Step 1: Take a single-sided polished single-crystalline silicon substrate, ultrasonically clean it in chemically pure acetone and ethanol for 10 minutes in sequence, and then quickly dry it with warm air to make its surface clean without stains and dust attachment. The surface roughness of the single-crystalline silicon substrate after ultrasonic treatment is less than 0.8 nm. Ultrasonic cleaning of the polished single-crystalline silicon substrate is beneficial to improving the bonding strength between the alloy and the substrate.

[0032] Step 2: Fix the ultrasonically cleaned single-crystalline silicon substrate to the substrate plate and automatically transport it into the magnetron sputtering coating chamber by mechanical means. Evacuate to a background vacuum of less than 4.0×10 -4 Pa.

[0033] Step 3: Deposit and prepare a TaTiZr high-entropy alloy on the silicon substrate by magnetron co-sputtering.

[0034] Among them, the sum of the atomic contents of titanium and zirconium in the TaTiZr alloy target is greater than 50%. The DC power supply power is 200 W, the deposition pressure is 1.0 Pa, the deposition temperature is room temperature, the substrate plate rotation speed is 15 r / min, the deposition time is 16,000 s, and the thickness of the obtained TaTiZr high-entropy alloy is 4.5 μm.

[0035] Step 4: Slowly cool the TaTiZr high-entropy alloy deposited in Step 3 to room temperature in the high-vacuum coating chamber.

[0036] Due to the long-term bombardment of the substrate by sputtered atoms during the deposition process, the prepared TaTiZr high-entropy alloy has a certain temperature rise. After the deposition is completed, it is slowly cooled in the high-vacuum coating chamber and then taken out, which can ensure that the internal stress of the sample is small and the surface is not oxidized by air.

[0037] Step 5: Put the TaTiZr alloy into a vacuum annealing furnace, evacuate to a background vacuum of less than 7.0×10 -4 Pa, and anneal at 500 °C for 2 h at room temperature to obtain the final TaTiZr high-entropy alloy.

[0038] Deposit the TaTiZr alloy on the surface of a ultrasonically cleaned and clean single-crystalline silicon wafer by magnetron co-sputtering. The principle is to generate Ar by ionizing Ar gas. +Ions are accelerated under the attraction of the cathode potential to bombard the cathode target (TaTiZr), sputtering out target atoms and secondary electrons. The target atoms are deposited on the anode substrate in the opposite direction, and the movement direction of the secondary electrons in the orthogonal electromagnetic field is perpendicular to the electric field and the magnetic field, presenting a cycloid motion trajectory, enhancing the collision with Ar molecules and increasing the probability of Ar ionization. The outstanding advantages of this technology are high ionization rate, fast deposition rate, low working temperature, adjustable element content, and it is not easy to cause agglomeration and back-sputtering of target elements, resulting in non-uniform microstructure. Finally, it is naturally cooled to room temperature in a high-vacuum coating chamber to avoid oxidation when exposed to air quickly, and the deposited atoms are fully diffused to form a TaTiZr alloy.

[0039] Example 1

[0040] A method for preparing a tantalum-titanium-zirconium high-entropy alloy, comprising the following steps;

[0041] Step 1: Ultrasonically clean the single-crystal silicon substrate in analytical pure acetone and ethanol for 10 minutes each in turn, and then quickly dry it with warm air.

[0042] Step 2: Fix the single-crystal silicon substrate on the substrate holder, and mechanically and automatically send it into the magnetron sputtering vacuum coating chamber, and pump it to a background vacuum of less than 4.0×10 -4 Pa.

[0043] Step 3: Adopt the method of co-sputtering with a magnetron sputtering DC and RF power supply to deposit a TaTiZr high-entropy alloy on the ultrasonically cleaned single-crystal silicon substrate;

[0044] Among them, the atomic ratio of the TaTiZr alloy target is Ta: 30.1%, Ti: 36.8%, Zr: 33.1%, the DC power supply power is 200W, the deposition pressure is 1.0Pa, the deposition temperature is room temperature, the substrate holder rotation speed is 15r / min, and the deposition time is 16000s.

[0045] Step 4: Naturally cool the single-crystal silicon substrate obtained in Step 3 in the high-vacuum coating chamber for 2-3 hours to room temperature and then take it out to obtain a Ta-30at%Ti-30at%Zr high-entropy alloy with a thickness of 4.5μm.

[0046] Step 5: Put the TaTiZr alloy obtained in Step 4 into a vacuum annealing furnace and anneal it at 400°C for 2 hours to obtain an annealed Ta-30at%Ti-30at%Zr high-entropy alloy with a thickness of 4.5μm.

[0047] Perform microstructure characterization and mechanical property testing on the prepared Ta-30at%Ti-30at%Zr high-entropy alloy. The alloy structure is amorphous, the Ta, Ti, and Zr elements of the alloy are evenly distributed, and its hardness measured by nanoindentation under a 10000μN load is 6.97±0.03GPa.

[0048] Example 2

[0049] A preparation method of tantalum-titanium-zirconium high-entropy alloy, comprising the following steps;

[0050] Step 1, ultrasonically clean the single-crystal silicon substrate in analytical pure acetone and ethanol for 10 minutes each in sequence, and then quickly dry it using warm air.

[0051] Step 2, fix the single-crystal silicon substrate on the substrate plate, and mechanically and automatically send it into the magnetron sputtering vacuum coating chamber, and pump it to a background vacuum degree below 4.0×10 -4 Pa.

[0052] Step 3, co-sputter TaTiZr high-entropy alloy on the ultrasonically cleaned single-crystal silicon substrate using a magnetron sputtering DC and RF power supply;

[0053] Among them, the atomic ratio of the TaTiZr alloy target is Ta: 30.1%, Ti: 36.8%, Zr: 33.1%, the DC power supply power is 200 W, the deposition gas pressure is 1.0 Pa, the deposition temperature is room temperature, the substrate plate rotation speed is 15 r / min, and the deposition time is 16000 s.

[0054] Step 4, naturally cool the single-crystal silicon substrate obtained in Step 3 in the high-vacuum coating chamber for 2 - 3 hours to room temperature and then take it out, to obtain Ta-30at%Ti-30at%Zr high-entropy alloy with a thickness of 4.5 μm.

[0055] Step 5, put the TaTiZr high-entropy alloy obtained in Step 4 into a vacuum annealing furnace, and anneal it at 500 °C for 2 hours to obtain the annealed Ta-30at%Ti-30at%Zr high-entropy alloy.

[0056] Carry out microstructure characterization and mechanical property testing on the prepared Ta-30at%Ti-30at%Zr alloy. The alloy structure is amorphous, and the Ta, Ti, and Zr elements in the alloy are evenly distributed. Under a nano-indentation load of 10000 μN, its hardness is measured to be 7.61 ± 0.05 GPa.

[0057] Example 3

[0058] A preparation method of tantalum-titanium-zirconium high-entropy alloy, comprising the following steps;

[0059] Step 1, ultrasonically clean the single-crystal silicon substrate in analytical pure acetone and ethanol for 10 minutes each in sequence, and then quickly dry it using warm air.

[0060] Step 2, fix the single-crystal silicon substrate on the substrate plate, and mechanically and automatically send it into the magnetron sputtering vacuum coating chamber, and pump it to a background vacuum degree below 4.0×10 -4 Pa.

[0061] Step 3: Deposit TaTiZr high-entropy alloy on the ultrasonically cleaned single-crystalline silicon substrate by co-sputtering with DC and RF magnetron sputtering power supplies;

[0062] Among them, the atomic ratio of the TaTiZr alloy target is Ta: 49%, Ti: 27%, Zr: 24%. Two alloy targets are used for co-sputtering. The DC power supply power is 200 W, the deposition pressure is 1.0 Pa, the deposition temperature is room temperature, the substrate rotation speed is 15 r / min, and the deposition time is 16000 s.

[0063] Step 4: Naturally cool the single-crystalline silicon substrate obtained in Step 3 in a high-vacuum coating chamber for 3 hours to room temperature and then take it out to obtain TaTiZr high-entropy alloy with a thickness of 4.5 μm.

[0064] Step 5: Put the TaTiZr alloy obtained in Step 4 into a vacuum annealing furnace and anneal it at room temperature for 2 hours to obtain the annealed TaTiZr high-entropy alloy.

[0065] Example 4

[0066] A method for preparing a tantalum-titanium-zirconium high-entropy alloy, comprising the following steps;

[0067] Step 1: Ultrasonically clean the single-crystalline silicon substrate in analytical pure acetone and ethanol for 10 min each in turn, and then quickly dry it with warm air.

[0068] Step 2: Fix the single-crystalline silicon substrate on the substrate holder and mechanically and automatically send it into the magnetron sputtering vacuum coating chamber, and pump it to a background vacuum of less than 4.0×10 -4 Pa.

[0069] Step 3: Deposit TaTiZr high-entropy alloy on the ultrasonically cleaned single-crystalline silicon substrate by co-sputtering with DC and RF magnetron sputtering power supplies;

[0070] Among them, the atomic ratio of the TaTiZr alloy target is Ta: 10%, Ti: 52.4%, Zr: 37.6%. Two alloy targets are used for co-sputtering. The DC power supply power is 200 W, the deposition pressure is 1.0 Pa, the deposition temperature is room temperature, the substrate rotation speed is 15 r / min, and the deposition time is 16000 s.

[0071] Step 4: Naturally cool the single-crystalline silicon substrate obtained in Step 3 in a high-vacuum coating chamber for 2 hours to room temperature and then take it out to obtain TaTiZr high-entropy alloy with a thickness of 4.5 μm.

[0072] Step 5: Put the TaTiZr alloy obtained in Step 4 into a vacuum annealing furnace and anneal it at 100 °C for 2 hours to obtain the annealed TaTiZr high-entropy alloy.

[0073] Example 5

[0074] A preparation method of tantalum-titanium-zirconium high-entropy alloy, comprising the following steps;

[0075] Step 1: Ultrasonically clean the single-crystal silicon substrate in analytical pure acetone and ethanol for 10 minutes each in sequence, and then quickly dry it with warm air.

[0076] Step 2: Fix the single-crystal silicon substrate on the substrate plate, and mechanically and automatically send it into the magnetron sputtering vacuum coating chamber, and pump it to a background vacuum of less than 4.0×10 -4 Pa.

[0077] Step 3: Adopt the method of magnetron sputtering direct current sputtering to deposit TaTiZr high-entropy alloy on the ultrasonically cleaned single-crystal silicon substrate;

[0078] Among them, the atomic ratio of the TaTiZr alloy target is Ta: 25%, Ti: 42%, Zr: 33%, the direct current power supply power is 200W, the deposition pressure is 1.0Pa, the deposition temperature is room temperature, the substrate plate rotation speed is 15r / min, and the deposition time is 16000s.

[0079] Step 4: Naturally cool the single-crystal silicon substrate obtained in Step 3 in the high-vacuum coating chamber for 2-3 hours to room temperature and then take it out to obtain TaTiZr high-entropy alloy.

[0080] Step 5: Put the TaTiZr alloy obtained in Step 4 into a vacuum annealing furnace, anneal it at 200°C for 2 hours to obtain the annealed TaTiZr high-entropy alloy with a thickness of 4.5μm.

[0081] Comparative Example 1

[0082] A preparation method of tantalum-titanium-zirconium high-entropy alloy, comprising the following steps;

[0083] Step 1: Ultrasonically clean the single-crystal silicon substrate in analytical pure acetone and ethanol for 10 minutes each in sequence, and then quickly dry it with warm air.

[0084] Step 2: Fix the single-crystal silicon substrate on the substrate plate, and mechanically and automatically send it into the magnetron sputtering vacuum coating chamber, and pump it to a background vacuum of less than 4.0×10 -4 Pa.

[0085] Step 3: Adopt co-sputtering of magnetron sputtering direct current and radio frequency power supply to deposit TaTiZr alloy on the single-crystal silicon substrate;

[0086] Among them, the atomic ratio of the TaTiZr alloy target is Ta: 30.1%, Ti: 36.8%, Zr: 33.1%, the power of the DC power supply is 200 W, the deposition pressure is 1.0 Pa, the deposition temperature is room temperature, the substrate rotation speed is 15 r / min, and the deposition time is 16000 s.

[0087] Step 4: Naturally cool the single-crystalline silicon substrate obtained in Step 3 in a high-vacuum coating chamber for 2 - 3 hours to room temperature and then take it out to obtain a Ta-30at%Ti-30at%Zr alloy with a thickness of 4.5 μm.

[0088] Microstructure characterization and mechanical property testing were carried out on the prepared Ta-30at%Ti-30at%Zr alloy. The alloy structure is amorphous, and the Ta, Ti, and Zr elements in the alloy are evenly distributed. Its hardness measured by nanoindentation under a load of 10000 μN is 6.56 ± 0.03 GPa.

[0089] Figure 1 The XRD result diagrams of the tantalum-titanium-zirconium high-entropy alloy of the present invention under different annealing systems are shown in []. It can be seen from the XRD test results that only amorphous peaks exist, indicating that the structure is an amorphous structure; Figure 2 The TEM microstructure and diffraction spot pictures of the tantalum-titanium-zirconium high-entropy alloy of the present invention under different annealing systems are shown in []. It can be observed from the pictures that the atomic arrangement in the structure is disordered, and the diffraction ring is in the shape of an obvious halo, further proving that the microstructure is an amorphous structure; Figure 3 The EDS scanning element distribution diagrams of the microstructure of the tantalum-titanium-zirconium high-entropy alloy under different annealing systems are shown in []. The results show that the element distribution in the structure is uniform and no segregation occurs; Figure 4 The load-displacement curves of nanoindentation of the tantalum-titanium-zirconium high-entropy alloy under different annealing systems are shown in []. From this data, Figure 5 the hardness and elastic modulus values in [] are deduced; Figure 5 The nanoindentation hardness change trends of the tantalum-titanium-zirconium high-entropy alloy under different annealing systems are shown in []. The results prove that with the increase of the annealing temperature, the hardness value and elastic modulus value of the coating show an increasing trend, and the performance is significantly improved. According to the tantalum-titanium-zirconium high-entropy alloy of the present invention, the structure is an amorphous structure, and this amorphous structure can maintain a temperature as high as 500 °C. The internal alloy elements are evenly distributed. With the increase of the annealing temperature, the hardness of the alloy gradually increases, and the indentation depth gradually decreases. The tantalum-titanium-zirconium high-entropy alloy of the present invention has excellent mechanical properties such as high strength and good plastic deformation ability.

[0090] A preparation method of a tantalum-titanium-zirconium high-entropy alloy provided by the present invention. This refractory high-entropy alloy is composed of refractory metals such as Ta, Ti, and Zr. It has a high melting point, high strength, and excellent high-temperature resistance, and is particularly suitable for making protective coatings on the surfaces of precision equipment components. By using magnetron sputtering technology, the antioxidant refractory high-entropy alloy can be coated on the surfaces of other high-temperature-resistant materials or refractory high-entropy alloy substrates, effectively improving the antioxidant, high-temperature resistance, and anti-irradiation properties of the substrates, solving the problem of uneven distribution of alloy elements in the materials. The obtained alloy is an amorphous material with uniform element distribution. Through the annealing system, it is found that the amorphous maintaining ability is as high as 500 °C, effectively improving the comprehensive mechanical properties of the alloy material.

[0091] The above content is only to illustrate the technical idea of the present invention and cannot be used to limit the protection scope of the present invention. Any modification made on the basis of the technical solution according to the technical idea proposed by the present invention falls within the protection scope of the claims of the present invention.

Claims

1. A preparation method of a tantalum-titanium-zirconium high-entropy alloy, characterized in that, It includes the following steps: Step 1: In a vacuum environment, a tantalum-titanium-zirconium high-entropy alloy is prepared on a substrate by magnetron sputtering; Two TaTiZr alloy targets are co-sputtered using a DC power supply; In the tantalum-titanium-zirconium high-entropy alloy, the sum of the atomic percentages of titanium and zirconium is greater than 50%, the sputtering power is 200 W, and the deposition pressure is 1.0 Pa; Step 2: The substrate obtained in Step 1 is vacuum-cooled to room temperature to obtain a tantalum-titanium-zirconium high-entropy alloy; Step 3: The tantalum-titanium-zirconium high-entropy alloy obtained in Step 2 is vacuum-annealed to obtain an annealed tantalum-titanium-zirconium high-entropy alloy; The degree of vacuum for the vacuum annealing is below 7×10 -4 Pa, the annealing temperature is from room temperature to 500 °C, and the annealing time is 2 h; In the tantalum-titanium-zirconium high-entropy alloy, the sum of the atomic percentages of titanium and zirconium is greater than 50%, the tantalum-titanium-zirconium high-entropy alloy is an amorphous structure, and the nanoindentation hardness of the tantalum-titanium-zirconium high-entropy alloy is 6 GPa to 8 GPa.

2. The preparation method of a tantalum-titanium-zirconium high-entropy alloy according to claim 1, characterized in that, In Step 1, after the substrate is cleaned and dried, magnetron sputtering co-sputtering is carried out in a vacuum environment.

3. The preparation method of a tantalum-titanium-zirconium high-entropy alloy according to claim 2, characterized in that, The method for cleaning and drying the substrate is as follows: The polished substrate is ultrasonically cleaned in acetone and alcohol for 10 min in sequence, and then dried. The roughness of the polished surface of the substrate is less than 0.8 nm.

4. The preparation method of a tantalum-titanium-zirconium high-entropy alloy according to claim 1, characterized in that, The degree of vacuum in the vacuum environment described in Step 1 is less than 4.0×10 -4 Pa.

5. The preparation method of a tantalum-titanium-zirconium high-entropy alloy according to claim 4, characterized in that, During the magnetron sputtering co-sputtering process, the deposition temperature is room temperature, the base plate rotation speed is 15 r / min, and the deposition time is 16000 s.

Citation Information

Patent Citations

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