A tungsten-rhenium alloy stir head material for friction stir welding and a method of manufacturing the same

Abstract

The application relates to the technical field of tungsten-rhenium alloy, and discloses a tungsten-rhenium alloy stir head material for friction stir welding, which is characterized in that the tungsten-rhenium alloy stir head material is prepared by reducing and sintering tungsten-rhenium precursors, the tungsten-rhenium precursors are prepared by using ammonium metatungstate, ammonium rhenate and oxalic acid as raw materials, and the application further discloses a preparation method of the tungsten-rhenium alloy stir head material, which comprises the following steps: S1, tungsten-rhenium precursor preparation: after ammonium metatungstate, ammonium rhenate and oxalic acid are dissolved, stirred and heated to react, spray drying is carried out to obtain tungsten-rhenium precursor powder; and S2, tungsten-rhenium precursor powder reduction: tungsten-rhenium precursor powder is heated and reduced in a hydrogen environment to obtain tungsten-rhenium alloy powder. The preparation process is simple, fast, low in cost and convenient for batch industrial production; the prepared single-phase tungsten-rhenium alloy is high in hardness and density and uniform in composition; the relative density of the tungsten-rhenium alloy after sintering reaches 99.6%, the microhardness value is 585+ / -5 Hv, and the grain size is 1-2 mu m.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of tungsten-rhenium alloy, and particularly relates to a tungsten-rhenium alloy material for a friction stir welding tool and a preparation method thereof. BACKGROUND

[0002] Friction stir welding (FSW) is a novel solid-phase joining technology, which is gradually widely applied due to its advantages of energy saving and environmental protection, low heat input, small deformation of welded parts, high welding precision, high welding quality and the like. A tool is the most critical part in the process of friction stir welding and is also the most likely to fail. The tool is mainly composed of a clamping handle, a shoulder and a stirring needle. The stirring needle is deeply inserted into the welded material and is subjected to strong friction and wear and high-temperature cyclic stress. Therefore, the stirring needle material is required to have high-temperature resistance, excellent creep resistance, high hardness, good thermal fatigue resistance and certain plasticity and toughness. Development of a stirring needle material with excellent performance can greatly expand the application range of FSW.

[0003] Metal tungsten has a very high elastic modulus (407 Gpa at room temperature) and a high melting point (3380 DEG C), so it can be used as an ideal high-strength heat-resistant material for a friction stir welding tool. Pure tungsten has a high ductile-brittle transition temperature (> 500 DEG C), so it is prone to brittle fracture below 500 DEG C and fails. Meanwhile, pure tungsten will recrystallize above 1200 DEG C and cause high-temperature brittleness, so its practical application is often limited. Rhenium and tungsten are adjacent in the periodic table of elements, have similar physical and chemical properties and atomic structures, can form a tungsten-rhenium alloy with good solid solubility and cause a "rhenium effect" to produce solid solution softening. High-content rhenium improves the hardness and strength of tungsten and significantly improves the plasticity and toughness of tungsten, so the tungsten-rhenium alloy can be used as an ideal stirring needle material for a friction stir welding tool.

[0004] At present, most of the tungsten-rhenium alloy powders are prepared by mechanical alloying. However, the tungsten-rhenium alloy solid solution prepared by mechanical alloying needs a long-time ball milling treatment by external stress and is easy to introduce impurities. Meanwhile, the tungsten-rhenium alloy powder after ball milling has a large residual stress, so that the grains grow rapidly in the subsequent sintering process. In addition, high-energy ball milling is a high-energy and time-consuming powder preparation process, which is difficult to be mass-produced industrially. Compared with the above, the tungsten-rhenium alloy powder prepared by a wet chemical method has uniform composition distribution, is simple, fast, low in cost and suitable for mass industrial production.

[0005] The conventional tungsten-rhenium alloy preparation is to use mold pressing forming and then high-temperature sintering, and the sintering method is to carry out high-temperature pressureless sintering in a protective atmosphere, so that the sintering method cannot obtain high-density tungsten-rhenium alloy, and the tungsten-rhenium alloy diffuses rapidly at high temperature, leading to coarse grains of the tungsten-rhenium alloy, so that the tungsten-rhenium alloy obtained by mold pressing sintering has poor hardness, strength and other performances and poor solid solution effect of the tungsten-rhenium alloy; the tungsten-rhenium precursor powder with uniform composition is prepared by using a wet chemical method and adding oxalic acid as a process control agent, the tungsten-rhenium alloy powder with good solid solubility is obtained by reducing the precursor powder by hydrogen, and finally a high-hardness, high-density single-phase tungsten-rhenium alloy with uniform composition is prepared by using a spark plasma sintering technology. SUMMARY

[0006] To solve the technical problem that the conventional tungsten-rhenium alloy preparation is to use mold pressing forming and then high-temperature sintering, and the sintering method is to carry out high-temperature pressureless sintering in a protective atmosphere, so that the sintering method cannot obtain high-density tungsten-rhenium alloy, and the tungsten-rhenium alloy diffuses rapidly at high temperature, leading to coarse grains of the tungsten-rhenium alloy, so that the tungsten-rhenium alloy obtained by mold pressing sintering has poor hardness, strength and other performances and poor solid solution effect of the tungsten-rhenium alloy, the present application provides a tungsten-rhenium alloy stir head material for friction stir welding and a preparation method thereof.

[0007] The present application adopts the following technical scheme: a tungsten-rhenium alloy stir head material for friction stir welding is prepared by reduction and sintering of tungsten-rhenium precursor, and the tungsten-rhenium precursor is prepared by using ammonium metatungstate, ammonium rhenate and oxalic acid as raw materials.

[0008] A preparation method of a tungsten-rhenium alloy stir head material for friction stir welding comprises the following steps:

[0009] S1 tungsten-rhenium precursor preparation:

[0010] After ammonium metatungstate, ammonium rhenate and oxalic acid are dissolved, stirred and heated for reaction, spray drying is carried out to obtain tungsten-rhenium precursor powder;

[0011] S2 reduction of tungsten-rhenium precursor powder:

[0012] The tungsten-rhenium precursor powder is heated and reduced in a hydrogen environment to obtain tungsten-rhenium alloy powder;

[0013] S3 sintering of tungsten-rhenium alloy powder:

[0014] The tungsten-rhenium alloy powder is pressed in a mold and then vacuum sintered, and after cooling and demolding, the tungsten-rhenium alloy material is obtained.

[0015] As a further improvement of the above scheme, the purity of the ammonium metatungstate is ≥ 99.95%, the purity of the ammonium rhenate is ≥ 99.9%, and the purity of the oxalic acid is pure.

[0016] As a further improvement of the above scheme, the adding amount of ammonium tungstate, ammonium rhenate and oxalic acid is 26.46-39.52%, 20.45-28.49% of the mass of ammonium tungstate respectively.

[0017] As a further improvement of the above scheme, in the step S1, the ammonium tungstate, ammonium rhenate and oxalic acid are dissolved in deionized water respectively, and stirred sufficiently until the solution is clear and free of precipitates.

[0018] As a further improvement of the above scheme, in the step S1, the stirring and heating reaction condition is that the heating is carried out in a magnetic stirrer, the temperature is raised to 100-120℃, after the temperature is stable, the reaction is carried out for 3-5h, and the precursor solution is obtained after the solute is completely reacted, wherein the solid content of the precursor solution is 25%-32%.

[0019] As a further improvement of the above scheme, in the step S1, the spray drying condition is that the inlet air temperature is 200-230℃, the outlet air temperature is 100-120℃, the rotation speed of the atomizer is 300-350r / min, and the feeding rate is 1-2L / h.

[0020] As a further improvement of the above scheme, in the step S2, the powder reduction condition is that the tungsten-rhenium precursor powder is laid flat in a boat, the boat is placed in a hydrogen reduction furnace, then hydrogen is introduced, wherein the purity of the hydrogen is ≥99.999%, the flow rate of the hydrogen is 2m 3 / h, no other gas is allowed in the furnace cavity except hydrogen, then the temperature is raised to 1000-1100℃ at a rate of 8-12℃ / min, the temperature is kept for 2-4h, then the temperature is lowered to 480-520℃ at a rate of 8-12℃ / min, and then the furnace is cooled to room temperature.

[0021] As a further improvement of the above scheme, in the step S3, the mold pressing condition is that the graphite mold loaded with the tungsten-rhenium alloy powder is placed in the cavity of the spark plasma sintering furnace, a unilateral axial pressure of 3-10MPa is applied to the mold punch, and the cavity is vacuumed to 12-18Pa.

[0022] As a further improvement of the above scheme, the sintering condition is that after the sintering starts, a current of 350-420A is pre-loaded to the sample, and a current of 8-12min is loaded to expel the adsorbed gas in the powder and the mold; then the pressure is uniformly increased to 0-10MPa, when the gas pressure in the cavity is reduced to 28-35Pa again, the current is continuously loaded for sintering, the continuous loading condition is that the current is increased at a rate of 80-120A / min until the highest sintering temperature is reached, then the temperature is raised at a rate of 130-180℃ / min, while the pressure is uniformly increased to 45-55MPa, immediately after the temperature reaches 1400-1800℃, the heating is stopped and the furnace is cooled to room temperature, and finally the sample is removed.

[0023] Compared with the prior art, the application has the beneficial effects that:

[0024] The application utilizes a wet chemical method and changes the precursor solution environment by adding oxalic acid as a process control agent to prepare a spherical tungsten-rhenium precursor powder with uniform composition distribution, changes the long-time ball milling treatment of the tungsten-rhenium alloy solid solution by relying on external stress in the traditional mechanical alloying, and the disadvantages that impurities are easily introduced, and the tungsten-rhenium alloy powder has a large residual stress after ball milling, which causes the grains to grow rapidly in the subsequent sintering process, and the preparation is simple, fast, low in cost, and convenient for batch industrial production.

[0025] The application obtains a spherical shell-shaped tungsten-rhenium alloy powder with good solid solubility through hydrogen reduction, finally changes the pressure change and the heating rate in the discharge plasma sintering process, so that the gas adsorbed under the discharge shock wave and the high-speed flow of electrons and ions in the electric field in the opposite direction and the oxidation film on the surface of the powder is broken to a certain extent in the early sintering stage, so that the powder is fully purified and activated, the discharge site and the joule heating site in the powder are quickly moved in the middle and late sintering stage, and the sintering of the powder is promoted to be uniform, the prepared single-phase tungsten-rhenium alloy is a single-phase tungsten-rhenium alloy with uniform composition, high hardness and high density, the relative density of the tungsten-rhenium alloy after sintering is 99.6%, the microhardness value is 585±5Hv, and the grain size is 1-2μm. BRIEF DESCRIPTION OF DRAWINGS

[0026] Figure 1 The X-ray diffraction spectrum of the tungsten-rhenium alloy precursor obtained in Example 3;

[0027] Figure 2 The scanning electron microscope image of the tungsten-rhenium alloy powder obtained in Example 3;

[0028] Figure 3 The X-ray diffraction spectrum of the tungsten-rhenium alloy obtained after sintering in Example 3;

[0029] Figure 4 The scanning electron microscope image of the surface of the tungsten-rhenium alloy obtained after sintering in Example 3;

[0030] Figure 5 The scanning electron microscope image of the fracture of the tungsten-rhenium alloy obtained after sintering in Example 3. DETAILED DESCRIPTION

[0031] In the following, the application will be further described in conjunction with the drawings and specific embodiments, and it should be noted that the following described embodiments or technical features can be combined in any manner to form new embodiments without conflict.

[0032] Example 1

[0033] A tungsten-rhenium alloy and a preparation method thereof, comprising the following steps:

[0034] Step 1: tungsten-rhenium precursor

[0035] Ammonium metatungstate (AMT, Aladdin, purity ≥ 99.95%), ammonium rhenate (NH4ReO4, purity ≥ 99.9%), and oxalic acid (C2H2O4·2H2O, analytical pure) are respectively dissolved in deionized water, and stirred thoroughly until the solution is clear and free of precipitates; the solution is placed in a magnetic stirrer for heating, and the temperature is raised to 100-120°C; after the temperature is stabilized, the solution is allowed to react for 3-5h, and the solute is completely reacted to obtain a tungsten-rhenium precursor solution, and the solid content of the precursor solution is 25%-32%; then a spray drying device is used to prepare a precursor powder, and the spray drying parameters are set as follows: the inlet air temperature is 200-230°C, the outlet air temperature is 100-120°C, the atomizer rotation speed is 300-350r / min, and the feeding rate is 1-2L / h; after the spray drying is completed, the powder in the collection tank is collected to obtain the tungsten-rhenium precursor powder;

[0036] In step 1, the addition amounts of ammonium rhenate and oxalic acid are 35.79% and 26.49% of the mass of ammonium metatungstate, respectively;

[0037] Step 2: powder reduction

[0038] The tungsten-rhenium precursor is laid flat in a boat, which is then placed in a hydrogen reduction furnace, and then hydrogen gas (hydrogen purity ≥ 99.999%, hydrogen flow rate is 2m3 / h) is introduced to ensure that there is no other gas in the tube furnace cavity except hydrogen; then the temperature is raised to 1000-1100°C at a rate of 8-12°C / min, and the temperature is maintained for 2-4h; then the temperature is lowered to 480-520°C at a rate of 8-12°C / min, and then the furnace is cooled to room temperature, thereby obtaining a tungsten-rhenium alloy powder;

[0039] Step 3: sintering process

[0040] A graphite mold loaded with the tungsten-rhenium alloy powder is placed in a discharge plasma sintering furnace cavity, a one-sided axial pressure of 10MPa is applied to the mold punch, and the furnace cavity is vacuumed to 15Pa; after the sintering starts, a current of 400A is pre-loaded on the sample for 10min to remove the adsorbed gas in the powder and the mold; when the gas pressure in the furnace cavity is reduced to 30Pa again, the sintering is continued by loading a current, and the continued loading conditions are as follows: the current is increased at a rate of 100 A / min until the highest sintering temperature is reached, and then the temperature is raised at a rate of 150°C / min while being uniformly pressurized to 50MPa; immediately after the temperature reaches 1600°C, the heating is stopped and the furnace is cooled to room temperature, and after the sample is removed, a tungsten-rhenium alloy block is obtained.

[0041] Example 2

[0042] A tungsten-rhenium alloy and a preparation method thereof, comprising the following steps:

[0043] Step 1: tungsten-rhenium precursor

[0044] Ammonium metatungstate (AMT, Aladdin, purity ≥ 99.95%), ammonium rhenate (NH4ReO4, purity ≥ 99.9%), and oxalic acid (C2H2O4·2H2O, analytical pure) are respectively dissolved in deionized water, and stirred thoroughly until the solution is clear and free of precipitates; the solution is placed in a magnetic stirrer for heating, and the temperature is raised to 100-120°C; after the temperature is stabilized, the solution is allowed to react for 3-5h; after the solute is completely reacted, a tungsten-rhenium precursor solution is obtained, and the solid content of the precursor solution is 25%-32%; then, a precursor powder is prepared by using a spray drying device; the spray drying parameters are set as follows: the inlet air temperature is 200-230°C, the outlet air temperature is 100-120°C, the rotation speed of the atomizer is 300-350r / min, and the feeding rate is 1-2L / h; after the spray drying is completed, the powder in the collection tank is collected, and a tungsten-rhenium precursor powder is obtained;

[0045] In step 1, the addition amounts of ammonium rhenate and oxalic acid are 35.79% and 26.49% of the mass of ammonium metatungstate, respectively.

[0046] Step 2: powder reduction

[0047] The tungsten-rhenium precursor is laid flat in a boat, which is then placed in a hydrogen reduction furnace; then, hydrogen gas (hydrogen purity ≥ 99.999%, hydrogen flow rate is 2m3 / h) is introduced into the furnace chamber, so that no other gas is present in the furnace chamber except hydrogen; then, the temperature is raised to 1000-1100°C at a rate of 8-12°C / min, and the temperature is maintained for 2-4h; then, the temperature is lowered to 480-520°C at a rate of 8-12°C / min, and the furnace is cooled to room temperature; and finally, a tungsten-rhenium alloy powder is obtained.

[0048] Step 3: sintering process

[0049] A graphite mold loaded with the tungsten-rhenium alloy powder is placed in a discharge plasma sintering furnace chamber; a single-sided axial pressure of 3MPa is applied to the mold punch, and the gas pressure in the furnace chamber is reduced to 15Pa; after the sintering starts, a small amount of current is pre-loaded to the sample; the current intensity pre-loaded to the sample is 400A, and the current is loaded for 10min at low temperature to remove the adsorbed gas in the powder and the mold; the pressure is uniformly increased to 10MPa; when the gas pressure in the furnace chamber is reduced to 30Pa again, the sintering is continued by loading the current; the current is continuously loaded at a rate of 100 A / min until the highest sintering temperature is reached; then, the temperature is raised at a rate of 150°C / min, and the pressure is uniformly increased to 50MPa; when the temperature reaches 1600°C, the heating is immediately stopped, and the furnace is cooled to room temperature; after the sample is removed, a tungsten-rhenium alloy block is obtained.

[0050] Example 3

[0051] A tungsten-rhenium alloy and a preparation method thereof, comprising the following steps:

[0052] Step 1: tungsten-rhenium precursor

[0053] Ammonium metatungstate (AMT, Aladdin, purity ≥ 99.95%), ammonium rhenate (NH4ReO4, purity ≥ 99.9%), and oxalic acid (C2H2O4·2H2O, analytical pure) were respectively dissolved in deionized water, and stirred thoroughly until the solution was clear without precipitate; the solution was heated in a magnetic stirrer, and the temperature was raised to 100-120°C; after the temperature was stable, the solution was reacted for 3-5h; after the solute was completely reacted, a tungsten-rhenium precursor solution was obtained, and the solid content of the precursor solution was 25%-32%; then, a precursor powder was prepared by using a spray drying device; the spray drying parameters were set as follows: the inlet air temperature was 200-230°C, the outlet air temperature was 100-120°C, the atomizer rotating speed was 300-350r / min, and the feeding rate was 1-2L / h; after the spray drying was completed, the powder in the collection tank was collected, and a tungsten-rhenium precursor powder was obtained;

[0054] In step 1, the adding amounts of ammonium rhenate and oxalic acid were 35.79% and 26.49% of the mass of ammonium metatungstate, respectively;

[0055] Step 2: powder reduction

[0056] The tungsten-rhenium precursor was laid flat in a boat, and the boat was placed in a hydrogen reduction furnace; then, hydrogen (hydrogen purity ≥ 99.999%, hydrogen flow rate was 2m3 / h) was introduced, so that there was no other gas in the tube furnace cavity except hydrogen; then, the temperature was raised to 1000-1100°C at a rate of 8-12°C / min, and the temperature was kept for 2-4h; then, the temperature was lowered to 480-520°C at a rate of 8-12°C / min, and the furnace was cooled to room temperature, so that a tungsten-rhenium alloy powder was obtained;

[0057] Step 3: sintering process

[0058] A graphite mold loaded with the tungsten-rhenium alloy powder was placed in a discharge plasma sintering furnace cavity, a unilateral axial pressure of 5MPa was applied to the mold punch, and the cavity was vacuumed to 15Pa; after the sintering started, a small amount of current was pre-loaded to the sample, the current intensity pre-loaded to the sample was 400A, and the gas adsorbed by the powder and the mold was removed by low-temperature loading for 10min; the pressure was uniformly increased to 10MPa, and when the cavity pressure was reduced to 30Pa again, the sintering was continued by loading the current, the continuous loading condition was that the current was loaded at a rate of 100 A / min until the highest sintering temperature was reached, and then the temperature was raised at a rate of 150°C / min, while the pressure was uniformly increased to 50MPa; when the temperature reached 1600°C, the heating was immediately stopped, and the furnace was cooled to room temperature; after the sample was taken out, a tungsten-rhenium alloy block was obtained.

[0059] AsFigure 1 The X-ray diffraction pattern of the tungsten-rhenium alloy precursor obtained in Example 3, wherein oxalic acid is added to the ammonium paratungstate, ammonium rhenate precursor solution and fully reacted, and the component-uniform spherical precursor powder is prepared by using the spray drying process, the tungsten-rhenium alloy precursor powder is prepared by using the wet chemical method and adding oxalic acid as a process control agent, the uniformity of the component of the tungsten-rhenium alloy precursor powder is improved, the pre-alloying process of the subsequent powder reduction and the densification process of sintering are promoted;

[0060] As shown in Figure 2 The scanning electron microscope pattern of the tungsten-rhenium alloy powder obtained in Example 3, wherein the component-uniform tungsten-rhenium alloy precursor powder is reduced by hydrogen and further pre-alloyed to obtain the preliminary solid-solution spherical tungsten-rhenium alloy powder;

[0061] As shown in Figure 4 The scanning electron microscope pattern of the surface of the tungsten-rhenium alloy obtained after sintering in Example 3, wherein the sintering process of the tungsten-rhenium alloy powder is optimized, the pressure change and the heating rate in the spark plasma sintering process are improved on the basis of Example 1, the adsorbed gas of the powder under the discharge shock wave generated by the pulse discharge and the high-speed flow of the electrons and ions in the electric field in the opposite direction is dissipated, and the oxide film on the surface of the powder is broken to a certain extent, so that the powder is fully purified and activated, and is more conducive to the subsequent high-temperature sintering to form the dense tungsten-rhenium alloy block;

[0062] Table 1 is the relative density and hardness table of the tungsten-rhenium alloy obtained after sintering in Examples 1, 2 and 3:

[0063]

[0064] The tungsten-rhenium alloy blocks prepared in Examples 1, 2 and 3 are subjected to performance testing and microstructure analysis, it is found that the tungsten-rhenium alloy block with small grain size, high hardness and high density can be sintered by adjusting the sintering pressure in the early stage and the current in the middle and late stages, the relative density of the tungsten-rhenium alloy block is 99.6%, the grain size is about 1-2 μm, and the microhardness is 585±5 Hv; unlike the traditional tungsten-rhenium alloy preparation process, the tungsten-rhenium alloy powder is prepared by using the wet chemical method and adding oxalic acid as a process control agent, and the performance of the tungsten-rhenium alloy is further improved by adjusting the spark plasma sintering parameters.

[0065] The above-mentioned embodiments are only preferred embodiments of the present application, and cannot be used to limit the protection scope of the present application, and any non-essential changes and substitutions made by those skilled in the art on the basis of the present application all belong to the protection scope of the present application.

Claims

1. A method of producing a tungsten-rhenium alloy tool material for friction stir welding, characterized by, The method comprises the following steps: S1: preparation of tungsten-rhenium precursor Dissolve, stir and heat ammonium metatungstate, ammonium rhenate and oxalic acid, and then perform spray drying to obtain tungsten-rhenium precursor powder; S2: reduction of tungsten-rhenium precursor powder Place the tungsten-rhenium precursor powder in a hydrogen environment and heat to reduce to obtain tungsten-rhenium alloy powder; S3: sintering of tungsten-rhenium alloy powder Place the tungsten-rhenium alloy powder in a mold and press, and then perform vacuum sintering, and after cooling and demolding, obtain tungsten-rhenium alloy material; The mold pressing conditions are as follows: the graphite mold loaded with tungsten-rhenium alloy powder is placed in the discharge plasma sintering furnace cavity, a unilateral axial pressure of 5 MPa is applied to the mold punch, and the vacuum in the furnace cavity is extracted to 12-18 Pa; The sintering conditions are as follows: after starting sintering, a current with an intensity of 350-420 A is pre-loaded on the sample for 8-12 minutes to remove the adsorbed gas in the powder and the mold; then, the pressure is uniformly increased to 10 MPa, and when the gas pressure in the furnace cavity is reduced to 28-35 Pa again, the sintering is continued by loading current, the continued loading condition is to increase the current at a rate of 80-120 A / min until the highest sintering temperature, and the temperature is increased at a rate of 130-180 ℃ / min, while uniformly increasing the pressure to 45-55 MPa, and when the temperature reaches 1400-1800 ℃, the heating is immediately stopped and the furnace is cooled to room temperature, and finally the sample is demolded.

2. The method of claim 1, wherein the tungsten-rhenium alloy material for a friction stir welding tool is prepared by the steps of: The purity of the ammonium metatungstate is ≥99.95%, the purity of the ammonium rhenate is ≥99.9%, and the purity of the oxalic acid is analytically pure.

3. The method of claim 1, wherein the tungsten-rhenium alloy material for a friction stir welding tool is prepared by the steps of: In step S1, the ammonium metatungstate, the ammonium rhenate and the oxalic acid are dissolved in deionized water respectively, and fully stirred until the solution is clear and free of precipitates.

4. The method of claim 1, wherein the tungsten-rhenium alloy material for a friction stir welding tool is prepared by the steps of: In step S1, the stirring and heating reaction conditions are as follows: a magnetic stirrer is used for heating, the temperature is increased to 100-120 ℃, and after the temperature is stabilized, the reaction is performed for 3-5 h, and after the solute is completely reacted, a tungsten-rhenium precursor solution is obtained, wherein the solid content of the precursor solution is 25%-32%.

5. The method of claim 1, wherein the tungsten-rhenium alloy material for a friction stir welding tool is prepared by the steps of: The spray drying conditions in step S1 are as follows: the inlet air temperature is 200-230 ℃, the outlet air temperature is 100-120 ℃, the atomizer speed is 300-350 r / min, and the feeding rate is 1-2 L / h.

6. The method of claim 1, wherein the tungsten-rhenium alloy material for a friction stir welding tool is prepared by the steps of: The powder reduction condition in the step S2 is that the tungsten-rhenium precursor powder is laid in a boat, the boat is put into a hydrogen reduction furnace, then hydrogen is introduced, wherein the purity of the hydrogen is ≥99.999%, the hydrogen flow is 2m 3 / h, no other gas is ensured in the furnace cavity except hydrogen, then the temperature is increased to 1000-1100℃ at a rate of 8-12℃ / min, the temperature is kept for 2-4h, then the temperature is decreased to 480-520℃ at a rate of 8-12℃ / min, then the furnace is cooled to room temperature.

7. The method of claim 1-6, wherein the tungsten-rhenium alloy material for friction stir welding tool is prepared by the method, and the tungsten-rhenium alloy material for friction stir welding tool is characterized in that, The addition amounts of the ammonium rhenate and the oxalic acid are 26.46-39.52% and 20.45-28.49% of the mass of the ammonium metatungstate, respectively.

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