Preparation method of tantalum-titanium alloy bar with high tantalum content

By mixing tantalum-titanium powders with matching particle size, degassing treatment, and controlling specific process parameters, the problem of non-uniform composition of tantalum-titanium alloy ingots was solved, and high tantalum-content tantalum-titanium alloy rods were prepared, which are suitable for aerospace, nuclear power and other fields.

CN121847766APending Publication Date: 2026-04-14NORTHWEST INSTITUTE FOR NONFERROUS METAL RESEARCH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-18
Publication Date
2026-04-14

AI Technical Summary

Technical Problem

In the existing technology, the compositional uniformity of tantalum-titanium alloys is difficult to control. Traditional preparation methods lead to potential problems with the stability and uniformity of the composition of tantalum-titanium alloy ingots, especially at high tantalum contents, where inclusions and segregation are difficult to avoid.

Method used

Using tantalum and titanium powder with matching particle size as raw materials, the process involves mixing in a three-dimensional mixer, degassing, isostatic pressing, and sintering, combined with specific process parameter control, to ensure uniform element distribution and absence of metallurgical inclusions in the tantalum-titanium alloy rods. This includes argon protection and gradient cooling during the mixing process.

Benefits of technology

High tantalum-titanium alloy rods with uniform element distribution and no metallurgical inclusion defects were prepared, meeting the high-temperature mechanical performance requirements of aerospace, nuclear power, and defense weaponry, and achieving stability and high yield in industrial production.

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Abstract

The invention discloses a preparation method of a tantalum-titanium alloy bar with high tantalum content. The method comprises the following steps: 1, selecting tantalum powder and titanium powder as raw materials; 2, uniformly mixing the tantalum powder and the titanium powder; 3, degassing treatment; 4, filling into a sheath and carrying out isostatic compaction; 5, carrying out vertical fusion sintering and gradient cooling; and 6, upsetting and drawing, heat treatment and machining treatment are carried out after scalping treatment, and the tantalum-titanium alloy bar with the high tantalum content is obtained. According to the method, through the working procedures and process control of mixing, degassing, isostatic pressing, vertical sintering, upsetting and drawing and the like of tantalum powder and titanium powder raw materials, the titanium and tantalum mixing degree is improved, and tantalum element refractory metal inclusion and segregation are avoided; the high-tantalum-content tantalum-titanium alloy bar which is uniform in element distribution, free of metallurgical inclusion defects, good in surface quality and capable of reaching the mechanical property standard is prepared, the preparation method is suitable for the industries such as aerospace, nuclear power, national defense weapons, medicine, chemical engineering and metallurgy, the process is simple, and industrial production is easy to achieve.
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Description

Technical Field

[0001] This invention belongs to the field of tantalum-titanium alloy rod preparation technology, specifically relating to a method for preparing tantalum-titanium alloy rods with high tantalum content. Background Technology

[0002] Titanium and its alloys, with their high specific strength, excellent comprehensive mechanical properties, and corrosion resistance, are widely used in many key fields such as aerospace, medical, and chemical industries. Tantalum and tantalum alloys, on the other hand, are highly favored in chemical and medical fields due to their high melting point, outstanding high-temperature strength, and excellent corrosion resistance and biocompatibility. Tantalum-titanium alloys combine the core advantages of both, possessing low density, good room temperature and high-temperature mechanical properties, high corrosion resistance, and excellent biocompatibility. Among them, tantalum-titanium alloys with high tantalum content (30wt%~65wt%) are expected to have superior high-temperature mechanical properties, making them a key core material for the manufacture of advanced defense weapons and equipment, and of significant value in potential applications such as aerospace, energy equipment, and extreme environments.

[0003] However, titanium and tantalum have significantly different physical properties. Tantalum's melting point (2996℃) is much higher than titanium's (1668℃). As the tantalum content increases, the difficulty of alloying increases dramatically, and the compositional uniformity becomes difficult to control. Currently, the traditional method for preparing tantalum alloy ingots in industrial production is electron beam melting. However, electron beam melting for preparing tantalum-titanium alloys has certain drawbacks. Due to the large difference in melting points between Ti and Ta, and the fact that Ti's saturated vapor pressure is much higher than Ta's during melting, the volatilization of Ti during electron beam melting is difficult to control, resulting in potential problems with the compositional stability and uniformity of tantalum-titanium ingots. Therefore, it is urgent to explore an efficient and stable process route for preparing homogenized tantalum-titanium alloys. Summary of the Invention

[0004] The technical problem to be solved by this invention is to provide a method for preparing high-tantalum-content tantalum-titanium alloy rods, addressing the shortcomings of the prior art. This method uses tantalum powder and titanium powder as raw materials, and through processes such as mixing, degassing, isostatic pressing, sintering, and upsetting, along with process control, improves the homogeneity of titanium and tantalum mixing and avoids refractory metal inclusions and segregation of tantalum. This results in high-tantalum-content tantalum-titanium alloy rods with uniform element distribution, no metallurgical inclusion defects, good surface quality, and satisfactory mechanical properties. This solves the problems of uneven mixing of tantalum and titanium and the difficulty in homogenizing the materials due to the large difference in melting point and density between tantalum and titanium.

[0005] To solve the above-mentioned technical problems, the technical solution adopted by the present invention is: a method for preparing high tantalum content tantalum-titanium alloy rods, characterized in that the method includes the following steps: Step 1: Select tantalum powder and titanium powder with matching particle size distribution as raw materials; Step 2: Mix the tantalum powder and titanium powder selected in Step 1 in a certain proportion to obtain a mixed powder. Step 3: Place the mixed powder from Step 2 into a degassing device, evacuate and heat it to degas the powder, so that the gaseous impurities in the mixed powder will volatilize and be discharged. Step 4: The mixed powder after degassing in Step 3 is loaded into a rubber mold sleeve and isostatically pressed under high pressure to densify the powder and obtain a pressed blank. Step 5: Place the pressed billet from Step 4 into a vacuum sintering furnace, pass DC current through it for vertical melting sintering, and after sintering, use gradient cooling. First, pass inert gas for rapid cooling, and then allow it to cool naturally to room temperature to obtain a high tantalum content tantalum-titanium alloy billet. Step 6: After peeling, the high tantalum content tantalum-titanium alloy billet from Step 5 is subjected to 2-3 heat upsetting, heat treatment, and machining to obtain high tantalum content tantalum-titanium alloy bars; the tantalum content in the high tantalum content tantalum-titanium alloy bars is more than 30% by mass.

[0006] The method for preparing a high-tantalum-content tantalum-titanium alloy rod described above is characterized in that the loose bulk density of both the tantalum powder and titanium powder in step one is 2.0 g / cm³. 3 ~3.5g / cm 3 Furthermore, the particle size of the titanium powder is 63µm~75µm, and the particle size of the tantalum powder is 50µm~63µm. Considering the significant difference in density between tantalum and titanium, this invention selects tantalum powder with a relatively small particle size and titanium powder with a relatively large particle size as raw materials. After mixing, it can ensure that the tantalum powder and titanium powder are completely melted and homogenized at a relatively low temperature and power, avoiding the formation of inclusions due to the incomplete melting of high-melting-point tantalum and the loss of low-melting-point titanium due to volatilization at excessively high temperatures. This ensures that inclusions and component segregation are not easily generated during the vertical melting sintering process.

[0007] The above-mentioned method for preparing a high tantalum content tantalum-titanium alloy rod is characterized in that the uniform mixing process in step two is as follows: tantalum powder and titanium powder are placed in a three-dimensional mixer for mixing, and argon gas is maintained throughout the mixing process, with a 1-hour break after every 2 hours of mixing, for a total mixing time of 8 hours.

[0008] This invention employs a three-dimensional mixer to mix tantalum powder and titanium powder. The three-dimensional mixer features a three-dimensional composite motion of rotation and revolution of the mixing drum, creating a triple mixing effect of convection, diffusion, and shearing, which effectively counteracts the tantalum (16.65 g / cm³) concentration. 3 ) and titanium (4.51g / cm 3The significant density difference between the powder and ingots avoids stratification and mixing dead zones, ensuring excellent control of mixing uniformity (CV value). This provides homogeneous raw materials for subsequent vertical melting sintering, significantly reducing ingot composition segregation. Simultaneously, the mixing process involves no forced stirring components, minimizing mechanical damage. Furthermore, the use of an argon inert gas protection device effectively controls the increase in gas content in the powder. The mixed powder exhibits stable bulk density and flowability, allowing for seamless transition between isostatic pressing and vertical melting sintering processes, significantly reducing production defects such as porosity and inclusions. In addition, this invention employs an intermittent mixing method, avoiding excessively long mixing times and powder overheating, which could lead to an increase in the gaseous element content in the mixed powder.

[0009] The above-mentioned method for preparing a high tantalum content tantalum-titanium alloy rod is characterized in that the degassing process in step three is as follows: the temperature is raised from room temperature to 600°C for 60 minutes, held for 60 minutes, then raised from 600°C to 830°C for 90 minutes, held for 180 minutes, and then cooled to 40°C before being removed from the furnace.

[0010] This invention removes adsorbed moisture, air, and volatile impurities from the mixed powder through degassing treatment, effectively reducing the porosity of the billet prepared in the subsequent vertical melting sintering process, reducing the gas content to avoid brittle inclusions, while improving the powder flowability and compaction density of the compact, ensuring the safety and stability of the subsequent vertical melting sintering process, and ultimately ensuring that the purity, density, and mechanical properties of the tantalum-titanium alloy rod meet the requirements.

[0011] The method for preparing a high-tantalum-content tantalum-titanium alloy rod described above is characterized in that the isostatic pressing pressure in step four is 150 MPa to 220 MPa, and the holding time is 15 min. This invention, by controlling the isostatic pressing pressure and holding time, improves the density of the compact, effectively eliminates gaps and agglomeration between powder particles, and imparts sufficient green strength to the compact, preventing breakage and deformation during subsequent handling and melting. Simultaneously, the uniform density distribution lays the foundation for the diffusion and fusion of tantalum and titanium atoms during melting, reducing the risk of component segregation.

[0012] The method for preparing a high tantalum content tantalum-titanium alloy rod described above is characterized in that the vacuum degree used in the vertical melting sintering step five is 1.0 × 10⁻⁶. -2 Pa ~ 1.0 × 10 -3The sintering temperature is 2000℃~2600℃, and the holding time is 2h~3h. This invention uses direct current for vertical melting sintering. The sintering is achieved by utilizing the large amount of heat generated by the resistance of the blank during pressing, while avoiding the uneven heating caused by intermittent alternating current, ensuring continuous and stable heat distribution within the blank, thus resulting in a more uniform grain structure. Furthermore, after sintering, this invention employs a gradient cooling method. First, inert gas is introduced for rapid cooling to prevent excessive grain growth and uneven grain structure caused by prolonged exposure to high temperatures. Then, natural cooling to room temperature gradually reduces internal stress, preventing cracking or deformation, resulting in a high-tantalum-content tantalum-titanium alloy blank and improving production efficiency.

[0013] The above-mentioned method for preparing a high tantalum content tantalum-titanium alloy bar is characterized in that, in step six, the high tantalum content tantalum-titanium alloy billet is subjected to a peeling process to remove surface pores and surface oxide scale, and then subjected to 2-3 heat upsetting and drawing. During the 2-3 heat upsetting and drawing process, a grinding wheel is used to remove the surface oxide scale of the billet. After air cooling, a forging billet is obtained. The forging billet is subjected to atmospheric annealing heat treatment in an electric heating furnace. After air cooling, it is machined to the target size using a lathe to obtain a high tantalum content tantalum-titanium alloy bar. The high tantalum content tantalum-titanium alloy bar has a room temperature yield strength of 500MPa~700MPa, a tensile strength of 700MPa~900MPa, an elongation of more than 20%, a reduction of area of ​​more than 40%, and a grain size rating of 6 or higher.

[0014] Compared with the prior art, the present invention has the following advantages: 1. This invention uses tantalum powder and titanium powder as raw materials. By controlling the particle size of the raw material powder and processing it through mixing and degassing, combined with the control of sintering and process parameters, the degree of uniformity of titanium and tantalum is improved. Degassing is used to avoid lumps, slag, or breakage during the sintering process, as well as the inclusion and segregation of refractory metals. A high tantalum-content tantalum-titanium alloy billet with uniform distribution of elements, no metallurgical inclusion defects, and good surface quality is prepared to meet the requirements of subsequent production.

[0015] 2. This invention limits the particle size of tantalum powder and titanium powder based on their different densities, and combines them with a specific powder mixing process, which is conducive to the uniform mixing of titanium and tantalum. This ensures that tantalum and titanium melt synchronously during the vertical melting and sintering process, promotes a more uniform distribution of titanium and tantalum elements in the billet, and avoids inclusions and component segregation during the melting process.

[0016] 3. This invention continuously introduces inert gas during the mixing process and uses intermittent mixing to prevent overheating, ensuring that the content of gaseous elements in the mixed powder does not increase. At the same time, the degassing treatment removes adsorbed moisture, air, and volatile impurities from the mixed powder, effectively reducing the porosity of the billet obtained in the subsequent vertical melting sintering process, reducing the gas content to avoid brittle inclusions, and improving the powder flowability and compaction density of the compact, ensuring the safety and stability of the subsequent vertical melting sintering process, and ultimately ensuring that the purity, density, and mechanical properties of the high tantalum content tantalum-titanium alloy rod meet the requirements.

[0017] 4. This invention prepares high-tantalum-content tantalum-titanium alloy rods through processes such as powder mixing, degassing, isostatic pressing, sintering, and upsetting. This improves the degree of element mixing and uniformity in the high-tantalum-content tantalum-titanium alloy rods and avoids refractory metal inclusions and segregation. The resulting high-tantalum-content tantalum-titanium alloy rods have uniform element distribution, no metallurgical inclusion defects, good surface quality, and meet mechanical property standards. They are suitable for aerospace, nuclear power, defense weaponry, medical, chemical, and metallurgical industries.

[0018] 5. The preparation process of this invention is simple, the design is reasonable and easy to implement, and it is easy to achieve industrial production. It effectively solves the problem of preparing tantalum-titanium ingot billets containing high melting point metal elements in the prior art. Moreover, the obtained tantalum-titanium alloy rods have qualified mechanical properties, a high yield, and no tantalum infusible blocks, realizing the continuous and large-scale production of subsequent products.

[0019] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description

[0020] Figure 1 This is a high-magnification microstructure image of the high tantalum content tantalum-titanium alloy rod prepared in Example 1 of the present invention.

[0021] Figure 2 This is a high-magnification microstructure image of the high tantalum content tantalum-titanium alloy rod prepared in Example 2 of the present invention.

[0022] Figure 3 This is a high-magnification microstructure image of the high tantalum content tantalum-titanium alloy rod prepared in Example 3 of the present invention. Detailed Implementation

[0023] Example 1 This embodiment includes the following steps: Step 1: Select tantalum powder with a particle size of 50µm~58µm and titanium powder with a particle size of 63µm~75µm as raw materials, and the loose bulk density of both tantalum powder and titanium powder is 2.0 g / cm³. 3 ~3.5g / cm 3 ; Step 2: Put the tantalum powder and titanium powder selected in Step 1 into a three-dimensional mixer at a mass ratio of 60:40 and mix them evenly. The mixing process is carried out under argon gas conditions, and the mixing is stopped for 1 hour every 2 hours. The total mixing time is 8 hours to obtain the mixed powder. Step 3: Place the mixed powder from Step 2 into a degassing device, vacuum and heat it for degassing treatment: raise the temperature from room temperature to 600℃ in 60 minutes, hold it at that temperature for 60 minutes, then raise the temperature from 600℃ to 830℃ in 90 minutes, hold it at that temperature for 180 minutes, and then cool it down to 40℃ to remove it from the furnace, so that the gaseous impurities in the mixed powder can be volatilized and discharged. Step 4: The mixed powder after degassing in Step 3 is loaded into a rubber mold sleeve and isostatically pressed under high pressure (150 MPa, 15 min) to densify the powder and obtain a compact. Step 5: Place the pressed blank from Step 4 into a vacuum sintering furnace and apply direct current for vertical melting sintering. The vacuum level used is 1.0 × 10⁻⁶. -2 Pa ~ 1.0 × 10 -3 Pa, the sintering temperature is 2000℃~2600℃, the holding time is 3h, and after sintering, a gradient cooling method is adopted. First, argon gas is introduced for rapid cooling, and then it is naturally cooled to room temperature to obtain a high tantalum content tantalum-titanium alloy billet with a diameter of φ90mm±5mm and a length of 500mm. Step Six: The high tantalum content tantalum-titanium alloy billet from Step Five is peeled to remove surface pores and oxide scale, and then subjected to three-heat upsetting. During the three-heat upsetting process, the oxide scale on the surface of the billet is removed by grinding with a grinding wheel. After air cooling, a forging billet is obtained. The forging billet is then subjected to atmospheric annealing heat treatment in an electric heating furnace at a temperature of 840℃ for 120 minutes. After air cooling, it is machined to the target size on a lathe to obtain a high tantalum content tantalum-titanium alloy bar with a diameter of φ50mm±1mm. The high tantalum content tantalum-titanium alloy bar has a room temperature yield strength of 520MPa, a tensile strength of 890MPa, an elongation of 32.5%, a reduction of area of ​​71%, and a grain size rating of 6.5.

[0024] The high tantalum content tantalum-titanium alloy billet prepared in step five of this embodiment was flattened and peeled on a lathe, and then sawn in the middle. Samples were taken from the upper, middle and lower parts of the obtained billet to test the chemical composition. The results showed that the tantalum mass content of the upper, middle and lower parts of the high tantalum content tantalum-titanium alloy billet prepared in this embodiment was 60.5%, 60.2% and 61.0% respectively, the absolute value of the composition fluctuation deviation was less than 1%, and the uniformity of each alloy composition was good.

[0025] Figure 1 This is a high-magnification microstructure image of the high-tantalum-content tantalum-titanium alloy rod prepared in this embodiment. Figure 1It can be seen that the microstructure of the tantalum-titanium alloy rod is a single equiaxed β phase, and the structure is uniform.

[0026] Example 2 This embodiment includes the following steps: Step 1: Select tantalum powder with a particle size of 50µm~58µm and titanium powder with a particle size of 63µm~75µm as raw materials, and the loose bulk density of both tantalum powder and titanium powder is 2.0 g / cm³. 3 ~3.5g / cm 3 ; Step 2: Put the tantalum powder and titanium powder selected in Step 1 into a three-dimensional mixer at a mass ratio of 48:52 and mix them evenly. The mixing process is carried out under argon gas conditions, and the mixing is stopped for 1 hour every 2 hours. The total mixing time is 8 hours to obtain the mixed powder. Step 3: Place the mixed powder from Step 2 into a degassing device, vacuum and heat it for degassing treatment: raise the temperature from room temperature to 600℃ in 60 minutes, hold it at that temperature for 60 minutes, then raise the temperature from 600℃ to 830℃ in 90 minutes, hold it at that temperature for 180 minutes, and then cool it down to 40℃ to remove it from the furnace, so that the gaseous impurities in the mixed powder can be volatilized and discharged. Step 4: The mixed powder after degassing in Step 3 is loaded into a rubber mold sleeve and isostatically pressed under high pressure (190 MPa, 15 min) to densify the powder and obtain a compact. Step 5: Place the pressed blank from Step 4 into a vacuum sintering furnace and apply direct current for vertical melting sintering. The vacuum level used is 1.0 × 10⁻⁶. -2 Pa ~ 1.0 × 10 -3 Pa, the sintering temperature is 2000℃~2600℃, the holding time is 2.5h, and after sintering, a gradient cooling method is adopted. First, argon gas is introduced for rapid cooling, and then it is naturally cooled to room temperature to obtain a high tantalum content tantalum-titanium alloy billet with a diameter of φ90mm±5mm. Step Six: The high tantalum content tantalum-titanium alloy billet from Step Five is peeled to remove surface pores and oxide scale, and then subjected to three-heat upsetting. During the three-heat upsetting process, the oxide scale on the surface of the billet is removed by grinding with a grinding wheel. After air cooling, a forging billet is obtained. The forging billet is then subjected to atmospheric annealing heat treatment in an electric heating furnace at a temperature of 840℃ for 120 minutes. After air cooling, it is machined to the target size on a lathe to obtain a high tantalum content tantalum-titanium alloy bar with a diameter of φ50mm±1mm. The high tantalum content tantalum-titanium alloy bar has a room temperature yield strength of 605MPa, a tensile strength of 865MPa, an elongation of 32%, a reduction of area of ​​69.5%, and a grain size rating of 7.

[0027] The high tantalum content tantalum-titanium alloy billet prepared in step five of this embodiment was flattened and peeled on a lathe, and then sawn in the middle. Samples were taken from the upper, middle and lower parts of the obtained billet to test the chemical composition. The results showed that the tantalum mass content of the upper, middle and lower parts of the high tantalum content tantalum-titanium alloy billet prepared in this embodiment was 47.9%, 48.8% and 48.77% respectively, the absolute value of the composition fluctuation deviation was less than 1%, and the uniformity of each alloy composition was good.

[0028] Figure 2 This is a high-magnification microstructure image of the high-tantalum-content tantalum-titanium alloy rod prepared in this embodiment. Figure 2 It can be seen that the microstructure of the tantalum-titanium alloy rod is a single equiaxed β phase, and the structure is uniform.

[0029] Example 3 This embodiment includes the following steps: Step 1: Select tantalum powder with a particle size of 50µm~58µm and titanium powder with a particle size of 63µm~75µm as raw materials, and the loose bulk density of both tantalum powder and titanium powder is 2.0 g / cm³. 3 ~3.5g / cm 3 ; Step 2: Put the tantalum powder and titanium powder selected in Step 1 into a three-dimensional mixer at a mass ratio of 55:45 and mix them evenly. The mixing process is carried out under argon gas conditions, and the mixing is stopped for 1 hour every 2 hours. The total mixing time is 8 hours to obtain the mixed powder. Step 3: Place the mixed powder from Step 2 into a degassing device, vacuum and heat it for degassing treatment: raise the temperature from room temperature to 600℃ in 60 minutes, hold it at that temperature for 60 minutes, then raise the temperature from 600℃ to 830℃ in 90 minutes, hold it at that temperature for 180 minutes, and then cool it down to 40℃ to remove it from the furnace, so that the gaseous impurities in the mixed powder can be volatilized and discharged. Step 4: The mixed powder after degassing in Step 3 is loaded into a rubber mold sleeve and isostatically pressed under high pressure (220 MPa, 15 min) to densify the powder and obtain a compact. Step 5: Place the pressed blank from Step 4 into a vacuum sintering furnace and apply direct current for vertical melting sintering. The vacuum level used is 1.0 × 10⁻⁶. -2 Pa ~ 1.0 × 10 -3 Pa, the sintering temperature is 2000℃~2600℃, the holding time is 2h, and after sintering, the gradient cooling method is adopted. First, argon gas is introduced for rapid cooling, and then it is naturally cooled to room temperature to obtain a high tantalum content tantalum-titanium alloy billet with a diameter of φ90mm±5mm. Step Six: The high tantalum content tantalum-titanium alloy billet from Step Five is peeled to remove surface pores and oxide scale, and then subjected to three-heat upsetting. During the three-heat upsetting process, the oxide scale on the surface of the billet is removed by grinding with a grinding wheel. After air cooling, a forging billet is obtained. The forging billet is then subjected to atmospheric annealing heat treatment in an electric heating furnace at a temperature of 840℃ for 120 minutes. After air cooling, it is machined to the target size on a lathe to obtain a high tantalum content tantalum-titanium alloy bar with a diameter of φ50mm±1mm. The room temperature yield strength of the high tantalum content tantalum-titanium alloy bar is 690MPa, the tensile strength is 720MPa, the elongation is 29%, the reduction of area is 69%, and the grain size rating is 6.5.

[0030] The high tantalum content tantalum-titanium alloy billet prepared in step five of this embodiment was flattened and peeled on a lathe, and then sawn in the middle. Samples were taken from the upper, middle and lower parts of the obtained billet to test the chemical composition. The results showed that the tantalum mass content of the upper, middle and lower parts of the high tantalum content tantalum-titanium alloy billet prepared in this embodiment was 54.7%, 55.01% and 55.42% respectively, the absolute value of the composition fluctuation deviation was less than 1%, and the uniformity of each alloy composition was good.

[0031] Figure 3 This is a high-magnification microstructure image of the high-tantalum-content tantalum-titanium alloy rod prepared in this embodiment. Figure 3 It can be seen that the microstructure of the tantalum-titanium alloy rod is a single equiaxed β phase, and the structure is uniform.

[0032] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention in any way. Any simple modifications, alterations, and equivalent changes made to the above embodiments based on the inventive essence shall still fall within the protection scope of the present invention.

Claims

1. A method for preparing a high tantalum content tantalum-titanium alloy rod, characterized in that, The method includes the following steps: Step 1: Select tantalum powder and titanium powder with matching particle size distribution as raw materials; Step 2: Mix the tantalum powder and titanium powder selected in Step 1 in a certain proportion to obtain a mixed powder. Step 3: Place the mixed powder from Step 2 into a degassing device, evacuate and heat it to degas the powder, so that the gaseous impurities in the mixed powder will volatilize and be discharged. Step 4: The mixed powder after degassing in Step 3 is loaded into a rubber mold sleeve and isostatically pressed under high pressure to densify the powder and obtain a pressed blank. Step 5: Place the pressed billet from Step 4 into a vacuum sintering furnace, pass DC current through it for vertical melting sintering, and after sintering, use gradient cooling. First, pass inert gas for rapid cooling, and then allow it to cool naturally to room temperature to obtain a high tantalum content tantalum-titanium alloy billet. Step 6: After peeling, the high tantalum content tantalum-titanium alloy billet from Step 5 is subjected to 2-3 heat upsetting, heat treatment, and machining to obtain high tantalum content tantalum-titanium alloy bars; the tantalum content in the high tantalum content tantalum-titanium alloy bars is more than 30% by mass.

2. The method for preparing a high tantalum content tantalum-titanium alloy rod according to claim 1, characterized in that, The loose bulk density of both tantalum powder and titanium powder mentioned in step one is 2.0 g / cm³. 3 ~3.5g / cm 3 Furthermore, the particle size of titanium powder is 63µm~75µm, and the particle size of tantalum powder is 50µm~63µm.

3. The method for preparing a high tantalum content tantalum-titanium alloy rod according to claim 1, characterized in that, The process of uniform mixing in step two is as follows: tantalum powder and titanium powder are placed in a three-dimensional mixer for mixing. Argon gas is maintained throughout the mixing process, and the mixing is stopped for 1 hour every 2 hours, for a total mixing time of 8 hours.

4. The method for preparing a high tantalum content tantalum-titanium alloy rod according to claim 1, characterized in that, The degassing process in step three is as follows: the temperature is raised from room temperature to 600℃ in 60 minutes, held for 60 minutes, then raised from 600℃ to 830℃ in 90 minutes, held for 180 minutes, and then cooled to 40℃ before being removed from the furnace.

5. The method for preparing a high tantalum content tantalum-titanium alloy rod according to claim 1, characterized in that, The isostatic pressing pressure in step four is 150MPa~220MPa, and the holding time is 15min.

6. The method for preparing a high tantalum content tantalum-titanium alloy rod according to claim 1, characterized in that, The vacuum degree used in the vertical melting sintering step five is 1.0 × 10⁻⁶. -2 Pa ~ 1.0 × 10 -3 Pa, sintering temperature is 2000℃~2600℃, holding time is 2h~3h.

7. The method for preparing a high tantalum content tantalum-titanium alloy rod according to claim 1, characterized in that, In step six, the high-tantalum-content tantalum-titanium alloy billet is peeled to remove surface pores and oxide scale, and then subjected to 2-3 heat upsetting and drawing. During the 2-3 heat upsetting and drawing process, a grinding wheel is used to remove the oxide scale from the billet surface. After air cooling, a forging billet is obtained. The forging billet is then subjected to atmospheric annealing heat treatment in an electric heating furnace. After air cooling, it is machined to the target size using a lathe to obtain a high-tantalum-content tantalum-titanium alloy bar. The high-tantalum-content tantalum-titanium alloy bar has a room temperature yield strength of 500MPa~700MPa, a tensile strength of 700MPa~900MPa, an elongation of more than 20%, a reduction of area of ​​more than 40%, and a grain size rating of 6 or higher.