Oxygen-doped TiZr-based single-phase refractory high-entropy alloy and preparation method thereof

Abstract

The present application relates to a kind of oxygen-doped TiZr-based single-phase refractory high-entropy alloys and its preparation method, it relates to refractory high-entropy alloy preparation technical field, preparation method includes the following steps: step one: design the atomic content of each element in alloy Ti, Zr, Nb, V and the atomic content of doped O element, then, according to the atomic content of each chemical element designed raw material is weighed;Step two: the raw material weighed in step one is melted, and oxygen-doped TiZr-based single-phase refractory high-entropy alloy ingot is prepared;Step three: oxygen-doped TiZr-based single-phase refractory high-entropy alloy ingot obtained in step two is carried out large plastic deformation treatment;Step four: oxygen-doped TiZr-based single-phase refractory high-entropy alloy ingot obtained by step three treatment is carried out medium temperature tempering treatment.The preparation method provided by the present application is simple and easy to operate, without complex deformation processing and aging treatment, only simple melting is combined with cold rolling deformation, and the mechanical properties of refractory high-entropy alloy can be greatly improved.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of refractory high-entropy alloy preparation, and particularly relates to an oxygen-doped TiZr-based single-phase refractory high-entropy alloy and a preparation method thereof. BACKGROUND

[0002] Refractory high-entropy alloys are expected to become new types of aerospace engine materials and nuclear reactor materials due to their high strength, high hardness, low neutron cross section, high wear resistance, and excellent oxidation resistance and high-temperature creep resistance. TiZr-based refractory high-entropy alloys have excellent room-temperature plasticity and have attracted extensive attention, but their strength is usually lower than 1 GPa. It is a challenge to significantly improve the strength while maintaining a certain plasticity. Common alloy strengthening methods such as precipitation strengthening, solid solution strengthening, and deformation strengthening are also applicable to refractory high-entropy alloys. For example, the addition of 7.5% Al in TiZrNb can increase the strength from 680 MPa to 930 MPa, which is due to the B2 phase strengthening caused by the addition of Al; the addition of 500 ppm B in TiZrNb can increase the strength from 621 MPa to 739 MPa; and AlMoNbHfTi can obtain a strength of 1.2 GPa through cold rolling deformation.

[0003] However, these strengthening methods usually inevitably lead to a decrease in plasticity, because whether it is a second phase or an interstitial atom, it will play a role in pinning dislocations during deformation. The large accumulation of dislocations leads to stress concentration, which, under the action of external load, causes premature fracture of the material as a crack source. It is a difficult problem to break the strength-plasticity strategy.

[0004] In recent years, it has been found that the addition of oxygen in refractory high-entropy alloys can improve the strength while rarely damaging the plasticity, because the ordered oxygen complex generated by the addition of oxygen can promote the cross-slip of dislocations while hindering the movement of dislocations, thereby achieving the purpose of considering both strength and plasticity. However, these single strengthening methods have limited strengthening effect, which makes it difficult to prepare ultra-high-strength refractory high-entropy alloys. Therefore, it is crucial to significantly improve the strength while maintaining a part of room-temperature plasticity for the preparation of ultra-high-strength refractory high-entropy alloys. SUMMARY

[0005] The purpose of the present application is to provide an oxygen-doped TiZr-based single-phase refractory high-entropy alloy and a preparation method thereof, so as to solve the problem that single strengthening method is difficult to prepare ultra-high-strength refractory high-entropy alloys.

[0006] The present application achieves the above-mentioned purpose by the following technical solutions:

[0007] The application provides an oxygen-doped TiZr-based single-phase refractory high-entropy alloy, which comprises Ti, Zr, Nb, V and O elements, wherein the sum of the atomic contents of the Ti, Zr, Nb and V elements is equal to 100%, and the sizes of the atomic contents of the Ti, Zr, Nb and V elements satisfy Ti >= Zr > Nb > V.

[0008] As a further optimization scheme of the application, the Ti element is 25 at.% to 40 at.%, the Zr element is 25 at.% to 40 at.%, the Nb element is 15 at.% to 30 at.% and the V element is 5 at.% to 15 at.% in terms of atomic percentage. Specifically, the contents of Ti and Zr are increased to obtain large lattice distortion and accommodate more oxygen atoms. If the content of Nb is too high, the density of the alloy will be greatly increased, and if the content of Nb is too low, the formation of the single-phase body-centered cubic structure will be adversely affected, therefore, the content of Nb is selected to be 15 at.% to 30 at.%, the V has a good strengthening effect, but if the content of V is higher than 15%, the V is prone to precipitate in the grain boundary to reduce plasticity, therefore, the content of V is controlled to be 5 at.% to 15 at.%.

[0009] Further, the atomic contents of the Ti, Zr, Nb and V elements are respectively 35 at.%, 30 at.%, 25 at.% and 10 at.%.

[0010] As a further optimization scheme of the application, in the step one, the oxygen is doped in the form of TiO2, and the atomic content of the doped oxygen in the alloy is 1 at.% to 2 at.% because the strengthening effect of a low content of oxygen is limited and a high content of oxygen will cause the alloy to be brittle.

[0011] As a further optimization scheme of the application, the oxygen-doped TiZr-based single-phase refractory high-entropy alloy is prepared by the following method: first, raw materials containing Ti, Zr, Nb, V and O elements are smelted to obtain an alloy ingot, and then the alloy ingot is subjected to large plastic deformation treatment and medium-temperature tempering treatment.

[0012] The application further provides a preparation method of the oxygen-doped TiZr-based single-phase refractory high-entropy alloy.

[0013] Step one: the atomic contents of Ti, Zr, Nb and V elements in the alloy and the atomic content of the doped oxygen element are designed, and then the raw materials are weighed according to the designed atomic contents of the chemical elements;

[0014] Step two: the raw materials weighed in step one are smelted to obtain an oxygen-doped TiZr-based single-phase refractory high-entropy alloy ingot;

[0015] Step three: large plastic deformation treatment is performed on the oxygen-doped TiZr-based single-phase refractory high-entropy alloy ingot obtained in step two;

[0016] Step four: medium-temperature tempering treatment is performed on the oxygen-doped TiZr-based single-phase refractory high-entropy alloy ingot obtained in step three.

[0017] As a further optimization scheme of the present application, in step three, the oxygen-doped TiZr-based single-phase refractory high-entropy alloy ingot is first cut into a cuboid shape by wire cutting to obtain a rectangular alloy sample, and then the rectangular alloy sample is subjected to a small amount of cold rolling deformation treatment at room temperature, and the deformation amount of each time is not higher than 20%.

[0018] As a further optimization scheme of the present application, in step three, the total thinning amount of the sample after cold rolling is 20%-90% of the thickness of the original sample.

[0019] As a further optimization scheme of the present application, in step four, the temperature range of the medium-temperature annealing treatment is 600-800 DEG C, and the time is 10-30 min. Under this process condition, the alloy ingot occurs dislocation recovery while avoiding complete recrystallization, so that a refractory high-entropy alloy with room-temperature strength and toughness is obtained.

[0020] The present application has the following beneficial effects:

[0021] (1) The oxygen-doped TiZr-based single-phase refractory high-entropy alloy obtained by the preparation method of the present application has the following advantages: first, the strength is greatly improved and can reach more than 1.4 GPa, and by adjusting the oxygen content and the deformation degree, the highest strength can reach about 1.8 GPa; second, it has certain room-temperature plasticity, and while the strength is greatly improved, it still maintains a room-temperature plasticity of more than 10%, achieving the balance of strength and plasticity at room temperature.

[0022] (2) The preparation method provided by the present application is simple and easy to implement, and does not require complex deformation processing and aging treatment. Only simple melting combined with cold rolling deformation can greatly improve the mechanical properties of the refractory high-entropy alloy.

[0023] (3) The oxygen-doped TiZr-based single-phase refractory high-entropy alloy prepared by the present application has a density of only about 6.3 g / cm 3 which is much lower than that of most refractory high-entropy alloys, and is more lightweight. The low density can enable the alloy to have higher specific yield strength (yield strength / density) at the same yield strength, and has good application prospects in the fields of aerospace engineering and the like. BRIEF DESCRIPTION OF DRAWINGS

[0024] Figure 1 is the Ti 35 Zr 30 Nb 25 V in Example 1 of the present application.10 XRD patterns of alloys and doping different oxygen contents;

[0025] Figure 2 Ti in Example 1 of the present application 35 Zr 30 Nb 25 V 10 Tensile stress-strain curves of 1O, Ti

[0026] Figure 3 Ti in Example 1 of the present application 35 Zr 30 Nb 25 V 10 -1O, Ti 35 Zr 30 Nb 25 V 10 -1O-20CR and Ti 35 Zr 30 Nb 25 V 10 Tensile stress-strain curves of 1O-60CR alloy samples

[0027] Figure 4 Ti in Example 1 of the present application 35 Zr 30 Nb 25 V 10 Tensile stress-strain curves of 3O alloy samples

[0028] Figure 5 Ti in Example 2 of the present application 35 Zr 30 Nb 25 V 10 -1O-90CR, Ti 35 Zr 30 Nb 25 V 10 Tensile stress-strain curves of 1.5O-90CR alloy samples

[0029] Figure 6 Ti in Example 3 of the present application 35 Zr 30 Nb 25 V 10 Tensile stress-strain curves of 1.5O-90CR alloy samples after tempering at 700℃, 800℃ for 30min, respectively

[0030] Figure 7 Ti in Example 3 of the present application 35 Zr 30 Nb 25 V 10Tensile stress-strain curves of 1.5O-90CR alloy samples after tempering at 500℃ for 30 min, respectively.

[0031] Figure 8 Ti 35 Zr 30 Nb 25 V 10 Tensile stress-strain curves of 1.5O-90CR alloy samples after tempering at 1050℃ for 30 min, respectively.

[0032] Figure 9 Ti 93 Tensile stress-strain curves of 1.5O-90CR alloy samples after tempering at 500℃ for 30 min, respectively. DETAILED DESCRIPTION

[0033] The application will be described in further detail below with reference to the drawings. It is necessary to point out here that the following detailed description is only used to further illustrate the application and cannot be understood as limiting the scope of protection of the application. Those skilled in the art can make some non-essential improvements and adjustments to the application according to the above application content.

[0034] Example 1

[0035] The preparation method of the oxygen-doped TiZr-based single-phase refractory high-entropy alloy in the embodiment includes the following steps:

[0036] Step one: according to the atomic ratio shown in the table, 0 at.%, 1 at.% and 3 at.% oxygen were respectively doped, and the samples were respectively marked as Ti 35 Zr 30 Nb 25 V 10 , Ti 35 Zr 30 Nb 25 V 10 , Ti 35 Zr 30 Nb 25 V 10 -1O and Ti 35 Zr 30 Nb 25 V 10 -3O samples, oxygen was doped in the form of TiO2, and different oxygen doping amounts were determined according to the addition amount of TiO2, then the content of the four metal elements Ti, Zr, Nb and V was slightly adjusted according to the addition amount of TiO2, and the total mass of the raw materials of each sample was about 70g, and the purity of Ti, Zr, Nb and V particles was ≥99.95%.

[0037] Step two: The weighed raw materials of each group of samples were melted in an argon atmosphere by a high-vacuum arc melting furnace. The vacuum degree of the furnace cavity was first extracted to 6x10 -3 Pa, and then argon was filled to-0.05 MPa. Each time, the melting was carried out at a current of 330 A for 8 min, and each group of samples was melted for at least five times.

[0038] Step three: The Ti 35 Zr 30 Nb 25 V 10 sample obtained by melting was cut into a 10 mm x 10 mm x 2 mm square by wire cutting, and was ground to 2000 mesh using sandpaper. XRD testing was performed at a speed of 0.033o / s, and the measurement angle was 20o-90o. 35 Zr 30 Nb 25 V 10 -1O sample and the Ti 35 Zr 30 Nb 25 V 10 -3O sample was cut into a 10 mm x 10 mm x 2 mm square by wire cutting, and was ground to 2000 mesh using sandpaper. XRD testing was performed at a speed of 0.033o / s, and the measurement angle was 20o-90o.

[0039] Step four: The Ti 35 Zr 30 Nb 25 V 10 -1O sample was divided into three parts by wire cutting. One part was not treated, and the other two parts were first cut into flat cuboids, and then were respectively deformed by cold rolling at room temperature for 2 times and 4 times, so that the total thinning amount of the samples was 20% and 60%, respectively. The two groups of samples deformed by cold rolling at room temperature were respectively recorded as Ti 35 Zr 30 Nb 25 V 10 -1O-20CR, Ti 35 Zr 30 Nb 25 V 10 -1O-60CR.

[0040] The Ti 35 Zr 30 Nb 25 V 10 sample obtained by melting in step two, Ti 35 Zr 30 Nb 25 V 10 -1O sample and the Ti 35 Zr 30 Nb 25 V 10 -3O sample, and the Ti 35 Zr30 Nb 25 V 10 -1O-20CR, Ti 35 Zr 30 Nb 25 V 10 -1O-60CR, were prepared by wire cutting standard tensile samples and polished to 2000 grit using sandpaper, then tensile properties were tested, tensile tests were performed on an Instron-5967 tensile machine at a strain rate of 1 x 10 -3 s -1 -1, with the tensile direction along the rolling direction.

[0041] The results are shown in Table 1, where: Figures 1-4

[0042] Figure 1 Ti 35 Zr 30 Nb 25 V 10 , Ti 35 Zr 30 Nb 25 V 10 -1O and Ti 35 Zr 30 Nb 25 V 10 -3O samples, as can be seen from the figures, the addition of oxygen does not cause a phase structure transition, the alloys all maintain a single-phase body-centered cubic structure.

[0043] Figure 2 Ti 35 Zr 30 Nb 25 V 10 room temperature tensile curves, as can be seen from the figures, the Ti 35 Zr 30 Nb 25 V 10 alloy samples have a tensile strength of about 850 MPa.

[0044] Figure 3 Ti 35 Zr 30 Nb 25 V 10 -1O alloy samples with 1 at.% oxygen added, as well as Ti 35 Zr 30 Nb 25 V 10 -1O-20CR, Ti 35 Zr 30 Nb 25 V 10 ​- Room temperature tensile curve of 1O-60CR alloy sample. From the figure, it can be seen that after adding 1 at.% oxygen, Ti 35 Zr 30 Nb 25 V 10 - The tensile strength of 1O alloy sample reaches 982 MPa, while the plasticity does not decrease;

[0045] After different rolling deformations, Ti 35 Zr 30 Nb 25 V 10 - 1O-20CR and Ti 35 Zr 30 Nb 25 V 10 - 1O-60CR alloy samples have tensile strengths of 1240 MPa and 1430 MPa, respectively. Even with small deformation, the strength is significantly improved, and Ti 35 Zr 30 Nb 25 V 10 - 1O-20CR alloy sample has an elongation of 15%. Ti 35 Zr 30 Nb 25 V 10 - 1O-60CR alloy sample has an elongation of 12%. It can be seen that after oxygen doping combined with cold rolling deformation, the strength of the alloy is greatly improved while still maintaining an elongation of more than 10%.

[0046] Figure 4 For Ti 35 Zr 30 Nb 25 V 10 - Room temperature tensile curve of 3O sample, the sample produces brittle fracture, from which it can be seen that the content of doped oxygen should not be too high, and the range should be 1 at.%-2 at.%.

[0047] Example 2

[0048] The oxygen-doped TiZr-based single-phase refractory high-entropy alloy in this embodiment has a preparation method comprising the following steps:

[0049] Step one: 1O sample of Ti 35 Zr 30 Nb 25 V 10 - 1O sample doped with 1.5 at.% oxygen, and Ti 35 Zr 30 Nb 25 V 10-1.5O samples were prepared by line cutting into flat cuboids, then through 6 times of cold rolling deformation at room temperature to make the total thinning of the sample 90%, the sample after cold rolling deformation at room temperature was recorded as Ti

[0050] Step two: the weighed raw materials were melted in an argon atmosphere by a high vacuum arc melting furnace, the vacuum degree of the furnace cavity was first extracted to 6x10 -3 Pa, then argon was filled to -0.05MPa. Each time was melted for 8min under a current of 330A, and each sample was melted for at least five times.

[0051] Step three: the Ti 35 Zr 30 Nb 25 V 10- 1O sample and Ti 35 Zr 30 Nb 25 V 10 -1.5O samples were respectively cut into flat cuboids by line cutting, then through 6 times of cold rolling deformation at room temperature to make the total thinning of the sample 90%, the sample after cold rolling deformation at room temperature was recorded as Ti 35 Zr 30 Nb 25 V 10 -1O-90CR and Ti 35 Zr 30 Nb 25 V 10 -1.5O-90CR.

[0052] Ti 35 Zr 30 Nb 25 V 10 -1O-90CR, Ti 35 Zr 30 Nb 25 V 10 -1.5O-90CR were respectively prepared into standard tensile samples by line cutting, sanded to 2000 mesh, then tensile property test was carried out, the tensile test was carried out on an Instron-5967 tensile machine at a strain rate of 1x10 -3 s -1 , and the tensile direction was along the rolling direction.

[0053] The results are shown in Table 1, Table 2 and Table 3. Figure 5 Table 1: Tensile properties of Ti 35 Zr 30 Nb 25 V 10 -1O and Ti 35 Zr 30 Nb 25 V 10-1.5O sample after 90% cold rolling deformation, Ti 35 Zr 30 Nb 25 V 10 -1O-90CR sample reaches 1595 MPa, Ti 35 Zr 30 Nb 25 V 10 -1.5O-90CR sample reaches 1750 MPa, which is 88% and 106% higher than the original sample, respectively, and has an elongation of 12% and 10%, respectively. By increasing the doping oxygen content and increasing the cold rolling deformation, a refractory high-entropy alloy with ultra-high strength is successfully prepared.

[0054] Example 3

[0055] The oxygen-doped TiZr-based single-phase refractory high-entropy alloy in this embodiment has a preparation method comprising the following steps:

[0056] Step one: Ti 35 Zr 30 Nb 25 V 10 -1.5O sample is prepared by weighing the raw materials with a total mass of about 70g, and the purity of Ti, Zr, Nb and V particles is ≥99.95%.

[0057] Step two: the weighed raw materials are melted in an argon atmosphere by a high vacuum arc melting furnace. First, the vacuum degree of the furnace cavity is extracted to 6x10 -3 Pa, and then argon is filled to-0.05MPa. Each time is melted for 8min at a current of 330A, and the sample is melted for at least five times.

[0058] Step three: the Ti 35 Zr 30 Nb 25 V 10 -1.5O sample is cut into a flat cuboid by wire cutting, and the total thinning amount of the sample is 90% by cold rolling deformation at room temperature for 6 times. Then, it is divided into four parts by wire cutting.

[0059] Step four: one of the samples obtained in step three is quenched after being kept at 500℃ for 30min, one is quenched after being kept at 700℃ for 30min, one is quenched after being kept at 800℃ for 30min, and the other is quenched after being kept at 1050℃ for 30min. The heat treatment process is carried out in an argon atmosphere tube furnace.

[0060] The sample obtained by the intermediate temperature tempering treatment in step four was prepared into a standard tensile sample by wire cutting, sanded to 2000 mesh, and then tensile property test was carried out. The tensile test was carried out on an Instron-5967 tensile machine at a strain rate of 1×10 -3 s -1 The tensile direction was along the rolling direction.

[0061] The results are shown in Table 1, wherein: Figures 6-8

[0062] Figure 6 Ti 35 Zr 30 Nb 25 V 10 The room temperature tensile curves of the sample after 90% rolling deformation and intermediate temperature tempering at 700℃ and 800℃, respectively. The tensile strength of the sample tempered at 700℃ reaches 1400MPa, with an elongation of 14%; the tensile strength of the sample tempered at 800℃ reaches 1350MPa, with an elongation of 22%, which has a more excellent combination of strength and plasticity than most refractory high-entropy alloys. In contrast, Figure 7 The sample tempered at 500℃ in Example 3 produces brittle fracture, and low-temperature tempering can cause brittleness of the alloy, which is not conducive to the improvement of mechanical properties. Figure 8 The strength of the sample tempered at 1050℃ in Example 4 is greatly reduced, and high-temperature tempering can cause a significant reduction in strengthening effect.

[0063] Comparative Example 1

[0064] The preparation method of the oxygen-doped TiZr-based single-phase refractory high-entropy alloy in the present comparative example comprises the following steps:

[0065] Step one: raw material proportioning of (NbTiZr) 93 Al5O2sample, and the Ti, Zr, Nb and Al particles have a purity of ≥99.95%.

[0066] Step two: the weighed raw materials are melted in an argon atmosphere by a high-vacuum arc melting furnace. First, the furnace cavity is vacuumed to 6×10 -3 Pa, and then argon is filled to-0.05MPa. Each time, the melting is carried out at a current of 330A for 8min, and each sample is melted for at least five times.

[0067] Step three: the (NbTiZr) 93 Al5O2sample prepared in step two is cut into two parts by wire cutting. One part is cut into a flat cuboid, and then the sample is cold-rolled at room temperature for 6 times to make the total thinning amount of the sample reach 90%. The sample after room temperature cold rolling is denoted as (NbTiZr) 93 ​Al5O2-90CR.

[0068] (NbTiZr) 93 Al5O2 and (NbTiZr) 93 Standard tensile samples of Al5O2-90CR were prepared by wire cutting, ground to 2000 grit with sandpaper, and then subjected to tensile property testing on an Instron-5967 tensile testing machine at a speed of 1×10⁻⁶. -3 s -1 The strain rate is adjusted, and the stretching direction is along the rolling direction.

[0069] The results are as follows Figure 9 As shown, (NbTiZr) 93 The tensile strength of Al₅O₂ reaches 1140 MPa, while the strength of NbTiZr is typically around 700 MPa. This demonstrates that replacing V with Al and doping with oxygen can achieve a similarly good strengthening effect. After 90% cold deformation, the strength reaches 1500 MPa, significantly exceeding the strength limit of NbTiZr. This also shows that the invention is not limited to Nb, Ti, V, and Zr, and has good effects on all TiZr-based high-entropy alloys.

[0070] The embodiments described above are merely examples of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention.

Claims

1. An oxygen-doped TiZr-based single-phase refractory high-entropy alloy, characterized in that, The oxygen-doped TiZr-based single-phase refractory high-entropy alloy comprises Ti, Zr, Nb, V and O elements, wherein the sum of the atomic contents of Ti, Zr, Nb and V elements is equal to 100%, and the atomic contents of Ti, Zr, Nb and V elements satisfy Ti≥Zr>Nb>V; The atomic contents of Ti, Zr, Nb and V elements are 25 at.%-40 at.% for Ti, 25 at.%-40 at.% for Zr, 15 at.%-30 at.% for Nb and 5 at.%-15 at.% for V; The O element is doped in the form of TiO2, and the atomic content of the doped O element in the alloy is 1 at.%-2 at.%; The oxygen-doped TiZr-based single-phase refractory high-entropy alloy is obtained by first smelting raw materials containing Ti, Zr, Nb, V and O elements to obtain an alloy ingot, and then performing large plastic deformation treatment and medium-temperature tempering treatment on the alloy ingot; The strength of the oxygen-doped TiZr-based single-phase refractory high-entropy alloy reaches 1.4-1.8 GPa while still maintaining a room temperature plasticity of >10%.

2. A method of preparing the oxygen-doped TiZr-based single-phase refractory high-entropy alloy according to claim 1, characterized in that, The method comprises the following steps: Step one: design the atomic contents of Ti, Zr, Nb and V elements in the alloy and the atomic content of the doped O element, and then weigh the raw materials according to the designed atomic contents of the chemical elements; Step two: smelt the raw materials weighed in step one to obtain an oxygen-doped TiZr-based single-phase refractory high-entropy alloy ingot; Step three: perform large plastic deformation treatment on the oxygen-doped TiZr-based single-phase refractory high-entropy alloy ingot obtained in step two; Step four: perform medium-temperature tempering treatment on the oxygen-doped TiZr-based single-phase refractory high-entropy alloy ingot obtained in step three.

3. The method of claim 2, wherein the method comprises the steps of: preparing a TiZr-based single-phase refractory high-entropy alloy; and doping the TiZr-based single-phase refractory high-entropy alloy with oxygen. In step three, the oxygen-doped TiZr-based single-phase refractory high-entropy alloy ingot is first cut into a cuboid shape by wire cutting to obtain a rectangular alloy sample, and then the rectangular alloy sample is subjected to a small amount of multiple cold rolling deformation treatment at room temperature, with each deformation amount being not higher than 20%.

4. The method of claim 3, wherein the method is characterized by: In step three, the total thinning amount of the sample after cold rolling deformation is 20%-90% of the thickness of the original sample.

5. The method for preparing an oxygen-doped TiZr-based single-phase refractory high-entropy alloy according to claim 2, characterized in that, In step four, the temperature range of the medium-temperature tempering treatment is 600-800℃, and the time is 10-30 min.

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