Method for producing w-re alloys with grain boundary irradiation damage mitigation properties

W-Re alloys were prepared by combining the sol-gel method with SPS, achieving uniform dispersion and solid solution of Re in the W matrix. This solved the problem of helium ion irradiation damage to W-Re alloys under fusion service conditions, significantly reduced the grain boundary helium bubble number density and swelling rate, and improved the radiation resistance performance.

CN122147117APending Publication Date: 2026-06-05HEFEI INSTITUTE OF PHYSICAL SCIENCE CHINESE ACADEMY OF SCIENCES

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
HEFEI INSTITUTE OF PHYSICAL SCIENCE CHINESE ACADEMY OF SCIENCES
Filing Date
2026-05-09
Publication Date
2026-06-05

AI Technical Summary

Technical Problem

Existing technologies are insufficient to effectively control helium ion irradiation damage in W-Re alloys under fusion service conditions, and the preparation methods suffer from uneven Re dispersion, limited addition amounts, and safety hazards.

Method used

Using ammonium metatungstate, ammonium perrhenate, polyethylene glycol, and citric acid as raw materials, W-Re alloys were prepared by sol-gel method combined with SPS to achieve uniform mixing and solid solution of W and Re, and to prepare W-Re alloys with a Re content of up to 20%.

Benefits of technology

It significantly reduces the grain boundary helium bubble number density and swelling rate, improves the radiation resistance of W-Re alloys, and effectively alleviates grain boundary damage, especially under high-temperature helium ion irradiation.

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Abstract

The application discloses a preparation method of a W-Re alloy with a crystal boundary irradiation damage alleviating characteristic, and belongs to the technical field of alloy materials. The preparation method of the W-Re alloy comprises the following steps: dissolving ammonium metatungstate, ammonium perrhenate and polyethylene glycol in a citric acid aqueous solution, drying and calcining after sol preparation, and obtaining an oxide precursor powder; reducing the oxide precursor powder in an environment containing hydrogen, and then sintering in a vacuum environment to obtain a target product. The application realizes uniform dispersion of W and Re at a molecular level, Re is completely solid-solved in a W matrix and segregation does not occur, compared with pure W under the same irradiation condition, the helium bubble number density and the crystal boundary swelling rate of the W-Re alloy prepared by the application are both reduced, and the crystal boundary irradiation damage is effectively alleviated. The application provides a new technical scheme for the design of the crystal boundary irradiation damage resistance of a nuclear fusion reactor plasma-facing W alloy.
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Description

Technical Field

[0001] This invention belongs to the field of alloy materials technology, specifically relating to a method for preparing a W-Re alloy with grain boundary irradiation damage mitigation properties. Background Technology

[0002] Nuclear fusion energy is one of the most promising clean energy sources for the future. In tokamak fusion devices, plasma-facing materials (PFMs) endure long-term bombardment from high heat fluxes, high-energy particles (deuterium, tritium, and helium), and neutron irradiation, making the working environment extremely harsh. Tungsten (W), due to its high melting point (3410 °C), low sputtering rate, low tritium retention, and good thermal conductivity, has been selected as the preferred plasma-facing material for the first wall and divertor in the International Thermonuclear Experimental Reactor (ITER) and the Demonstration Fusion Reactor (DEMO). During fusion reactor operation, helium ion irradiation damage is one of the core challenges faced by tungsten materials. Helium ions from alpha particles in the fusion reaction and edge plasma form helium bubbles in tungsten, inducing material swelling and hardening, leading to material performance degradation.

[0003] Studies have shown that adding Re to tungsten can improve the density and hardness of tungsten alloys, but there are still some shortcomings: on the one hand, existing studies have not addressed the regulation of helium ion irradiation damage under fusion service conditions; on the other hand, existing methods for preparing W-Re alloys still have problems such as uneven dispersion of Re in W, limited addition amount, and safety hazards in preparation conditions.

[0004] Chinese patent CN107790738B discloses a method for preparing W-Re powder by combustion synthesis combined with hydrogen reduction using ammonium metatungstate, ammonium rheniumate, fuel, and ammonium nitrate as raw materials. This method mainly addresses the issues of powder preparation efficiency and sintering activity. However, the ammonium nitrate used in the process is a flammable and explosive hazardous chemical, and its participation in combustion synthesis poses safety hazards during experimental implementation and scale-up, as it is prone to explosion. Furthermore, the focus is on powder preparation efficiency, without addressing irradiation damage performance.

[0005] Chinese patent CN118957334B discloses a method for preparing a W-Re alloy precursor and a high-density, high-hardness W-Re alloy, using rhenium powder as the Re source, primarily to improve the alloy's density and hardness. The amount of rhenium powder added is limited to 1-10%, and a comparative example shows that when the rhenium powder content is increased to 15%, the preparation fails due to incomplete dissolution, indicating a limitation of this method in preparing higher Re contents. This restricts the preparation of high Re content alloys, and radiation resistance was also not investigated.

[0006] In summary, existing technologies mainly focus on the preparation of W-Re alloy powder, homogenization of precursors, and improvement of density and hardness. There is still a lack of a preparation method for W-Re alloys that is suitable for fusion service conditions, takes into account the design of high Re content, and can alleviate grain boundary irradiation damage. Summary of the Invention

[0007] To address the problem of grain boundary damage accumulation in W alloys under high-temperature helium ion irradiation conditions in existing technologies, this invention provides a method for preparing W-Re alloys with grain boundary irradiation damage mitigation properties. This invention uses ammonium perrhenate, ammonium metatungstate, polyethylene glycol, and citric acid as raw materials, which can ensure uniform mixing of W and Re at the atomic scale in a safe experimental environment. W-Re alloys with a Re content of up to 20% have been successfully prepared, demonstrating a wider range of composition control and better preparation capabilities for high Re content.

[0008] To achieve the above objectives, the technical solution adopted by the present invention is as follows: A method for preparing a W-Re alloy with grain boundary irradiation damage mitigation properties includes the following steps: Ammonium metatungstate, ammonium perrhenate, and polyethylene glycol are dissolved in an aqueous citric acid solution, and the solution is heated and stirred at 60-90 °C to obtain a homogeneous sol. Preferably, the aqueous citric acid solution is obtained by dissolving citric acid in water. The stirring speed is 200-600 r / min, and the stirring time is 3-7 h. The sol is dried and then calcined in air to obtain an oxide precursor powder; preferably, the drying temperature is 90-160 °C and the drying time is 12-24 h. The calcination temperature is 500-800 °C and the calcination time is 6-12 h.

[0009] The oxide precursor powder is reduced in a hydrogen-containing environment to obtain W-Re alloy powder; preferably, the reduction temperature is 700-900 ℃ and the reduction time is 4-6 h.

[0010] W-Re alloy powder is sintered under vacuum to obtain W-Re alloy. Preferably, the sintering is spark plasma sintering (SPS); the sintering temperature is 1600-1800 °C and the pressure is 20-30 MPa.

[0011] As a further optimization of the present invention, the molar ratio of ammonium metatungstate to citric acid is 2:25-50. Within this range, it is beneficial to ensure sufficient complexation and uniform dispersion of tungsten and rhenium components in the precursor system. When the amount of citric acid is too low, the complexation and dispersion effects are insufficient, which can easily lead to decreased sol stability, local precipitation or agglomeration, and reduce the uniformity of W and Re element distribution in the subsequently obtained powder, which is not conducive to obtaining a W-Re alloy with a uniform microstructure. When the amount of citric acid is too high, the organic component content of the system is too high, which can easily cause an increase in sol viscosity, make the gelation and thermal decomposition processes difficult to control, and may lead to increased powder porosity, agglomeration, or an increased risk of residual carbon. Therefore, the above molar ratio range can take into account both the complexation and dispersion effect of the precursor and the controllability of subsequent heat treatment, which is beneficial to obtaining a W-Re alloy material with uniform composition, low impurities, and stable microstructure.

[0012] As a further optimization of the present invention, the amount of polyethylene glycol added is 10-21% of the mass of ammonium metatungstate. Polyethylene glycol is mainly used as a dispersant stabilizer and an organic network aid. It can work with citric acid to improve the stability of the precursor sol and the uniformity of the gel network, reduce the risk of local enrichment of W and Re components and powder agglomeration during drying and calcination, and facilitate the subsequent acquisition of W-Re alloy powder with uniform composition and good sintering performance.

[0013] The W-Re alloy prepared by the above method comprises 80-97 wt.% W and 3-20 wt.% Re by mass percentage, with the sum of the mass percentages of W and Re being 100 wt.%. Re is completely dissolved in the W matrix to form a single solid solution without segregation. At 500 keV He... 2+ Under irradiation conditions of 800 °C and a peak damage dose of approximately 5.07 dpa, the helium bubble number density in the grain boundary region of the alloy does not exceed 2.3 × 10⁻⁶. 23 m -3 The grain boundary swelling rate does not exceed 1.7%, which is lower than the corresponding value of pure W under the same irradiation conditions (2.7 × 10⁻⁶). 23 m -3 (and 1.9%). Furthermore, when the mass fraction of Re is 20 wt.%, under the above irradiation conditions, the helium bubble number density in the grain boundary region decreases to 1.7 × 10⁻⁶. 23 m -3 The grain boundary swelling rate was reduced to 1.3%, which is 37% and 31% lower than that of pure W, respectively. The W-Re alloy prepared by this invention has great application prospects in the field of plasma-oriented materials for nuclear fusion reactors.

[0014] This invention proposes a novel radiation-resistant design concept from the perspective of controlling the spatial distribution of defects. Specifically, by introducing an appropriate amount of Re, the strong interactions between Re atoms and helium clusters, vacancies, and interstitial atoms can dominate the spatial redistribution of irradiation defects between grain boundaries and the grain interior. Specifically, Re tends to interact with helium clusters and point defects within the grain, altering the diffusion behavior and aggregation tendency of these defects, causing irradiation damage to gradually shift spatially from grain boundaries (vulnerable sites) to the grain interior. This significantly reduces the helium bubble number density and swelling rate at grain boundary locations, effectively mitigating the risk of grain boundary embrittlement.

[0015] The beneficial effects of this invention are as follows: (1) The ammonium metatungstate and ammonium perrhenate used in this invention have good water solubility and can form a uniform and stable precursor solution in the citric acid system, which is beneficial to achieving uniform mixing of W and Re elements. At the same time, the ammonium ions can decompose and be discharged in the form of gaseous products during the subsequent calcination process, without forming residual impurities in the W-Re alloy powder.

[0016] (2) This invention uses a sol-gel method combined with SPS to prepare W-Re alloys. The uniform dispersion of W and Re at the molecular level is achieved through citric acid complexation, and Re is completely dissolved in the W matrix without segregation under the combined action of polyethylene glycol. The preparation process is simple and the parameter range is well-defined. Its working principle is as follows: Citric acid acts as a complexing agent and gelling agent, playing a stabilizing role. Its molecule contains multiple carboxyl and hydroxyl groups, enabling it to form a uniform and stable complex dispersion system with tungsten and rhenium precursor species, and can also work with polyethylene glycol to promote the formation of a uniform organic precursor network. This structure is beneficial for improving the mixing uniformity of W and Re components and reducing the risk of local enrichment and segregation of Re during subsequent calcination, reduction, and sintering processes.

[0017] (3) This invention evaluates the radiation resistance characteristics of W-Re alloys using quantitative grain boundary irradiation damage indices (helium bubble number density and swelling rate in the grain boundary region), and mitigates the degree of grain boundary damage during high-temperature helium ion irradiation by controlling the defects generated by irradiation through Re. Specifically, the helium bubble number density at the pure W grain boundary is increased from 2.7 × 10⁻⁶. 23 m -3 Reduced to 1.7 × 10⁻⁶ for W-20Re 23 m -3 (Reduced by 37%), decreasing the grain boundary swelling rate from 1.9% to 1.3% (a reduction of 31%). This fills a gap in the field of mitigating grain boundary damage in W alloys.

[0018] (4) This invention provides a basis for the design of anti-grain boundary irradiation damage composition of W-Re alloy for plasma-oriented fusion reactors. By adjusting the Re content, the degree of grain boundary damage can be directionally controlled, which has clear engineering application value. Attached Figure Description

[0019] Figure 1 Figure 1 shows the distribution and size of helium bubbles at the grain boundaries of pure W after irradiation; where: (a) Figure 2 shows the distribution of helium bubbles at the grain boundaries of pure W after irradiation, and (b) Figure 3 shows its size. Figure 2 The graph shows the helium bubble number density and grain boundary swelling rate at the grain boundary of pure W after irradiation. Figure 3 The following are EDS images of the W-3Re alloy matrix before irradiation; where: (a), (b), and (c) are the EDS images of the W-3Re alloy matrix before irradiation, and the distribution diagrams of W and Re, respectively; Figure 4 Figure 1 shows the distribution and size of helium bubbles at the grain boundary of W-3Re after irradiation; where: (a) Figure 2 shows the distribution of helium bubbles at the grain boundary of W-3Re after irradiation, and (b) Figure 3 shows its size. Figure 5 The graph shows the helium bubble number density and grain boundary swelling rate of W-3Re at the grain boundary after irradiation. Figure 6 The following are EDS diagrams of the W-10Re alloy matrix before irradiation; where: (a), (b), and (c) are EDS diagrams of the W-10Re alloy matrix before irradiation, and distribution diagrams of W and Re, respectively; Figure 7 Figure 1 shows the distribution and size of helium bubbles at the grain boundary of W-10Re after irradiation; (a) shows the distribution of helium bubbles at the grain boundary of W-10Re after irradiation, and (b) shows its size. Figure 8 The graph shows the helium bubble number density and grain boundary swelling rate of W-10Re at the grain boundary after irradiation. Figure 9 The XRD pattern of the reduced W-20Re alloy; Figure 10 The images show the EDS (Electro-Derivatives Analysis) of the W-20Re alloy matrix before irradiation; where (a), (b), and (c) are the EDS of the W-20Re alloy matrix before irradiation, and the distribution diagrams of W and Re, respectively. Figure 11 Figure 1 shows the distribution and size of helium bubbles at the grain boundary of W-20Re after irradiation; where: (a) is the distribution of helium bubbles at the grain boundary of W-20Re after irradiation, and (b) is its size diagram; Figure 12The graph shows the helium bubble number density and grain boundary swelling rate of W-20Re at the grain boundary after irradiation. Detailed Implementation

[0020] To facilitate understanding of the present invention, a more comprehensive description will be given below with reference to specific embodiments. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a more thorough and complete understanding of the disclosure of the present invention.

[0021] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The polyethylene glycol used in the following examples has a molecular weight of 2000.

[0022] Comparative Example 1 This embodiment discloses a method for preparing a pure W alloy block as a reference for irradiation experiments. The preparation method specifically includes the following steps: S1. Add 50 g of citric acid to deionized water and stir until completely dissolved. Then add 13.73 g of ammonium metatungstate and 2 g of polyethylene glycol. Place the solution in a 90 ℃ water bath and stir at 200 r / min for 7 h until a uniform sol is formed. S2. The sol obtained in step S1 is dried at 160 °C for 12 h, and then calcined in air at 800 °C for 6 h to obtain oxide powder; S3. The oxide powder obtained in step S2 is reduced at 900 °C for 4 h in a hydrogen atmosphere to obtain pure W powder; S4. The pure W powder obtained in step S3 is sintered under vacuum using SPS at a temperature of 1800 ℃, a pressure of 20 MPa, and a holding time of 8 min to obtain pure W bulk material. S5. The pure W block prepared in step S4 is polished with silicon carbide sandpaper of 80 mesh, 400 mesh, 800 mesh, 2000 mesh and 3000 mesh in sequence. Then, the tungsten alloy surface is mechanically polished with diamond suspension to make the pure W surface appear mirror-like. S6. Electrolyze the pure W after mechanical polishing in step S5 using a 5% sodium hydroxide solution at an electrolysis voltage of 10 V. S7. Place the pure W processed in step S6 at 500 keV He 2+ The patient was irradiated at a temperature of 800 °C, with a peak irradiation damage dose of 5.07 dpa.

[0023] The irradiated pure W in this embodiment was characterized to obtain the following results: Figure 1 The distribution of helium bubbles at the grain boundary sites of pure W after irradiation (as shown in Figure a) and the size diagram (as shown in Figure b) are as follows. Figure 2 The diagram shows the helium bubble number density and grain boundary swelling rate at the grain boundary of pure W after irradiation.

[0024] from Figure 1 As can be seen in Figure (a), pure W exhibits a relatively dense distribution of helium bubbles at the grain boundaries after helium ion irradiation; from Figure 1 Figure (b) shows that the average size of helium bubbles at the grain boundary of pure W after helium ion irradiation is 5.1 nm.

[0025] from Figure 2 As can be seen, the number density of helium bubbles on the grain boundaries of pure W after helium ion irradiation is 2.7 × 10⁻⁶. 23 m -3 The corresponding swelling rate was 1.9%.

[0026] Example 1 This embodiment proposes a W-3Re alloy with grain boundary irradiation damage mitigation properties and its preparation method, specifically including the following steps: S1. Add 40 g of citric acid to deionized water and stir until completely dissolved. Then add 13.32 g of ammonium metatungstate, 0.43 g of ammonium perrhenate and 1.5 g of polyethylene glycol in sequence. Place the solution in a 60 ℃ water bath and stir at 600 r / min for 3 h until a uniform sol is formed. S2. The sol obtained in step S1 is dried at 90 °C for 24 h, and then calcined in air at 500 °C for 12 h to obtain nano-oxide powder; S3. The oxide powder obtained in step S2 is reduced at 700 °C for 6 h in a hydrogen atmosphere to obtain W-3Re alloy powder; S4. The W-3Re alloy powder obtained in step S3 is subjected to SPS sintering in a vacuum environment at a temperature of 1600 ℃, a pressure of 30 MPa, and a holding time of 8 min to obtain W-3Re alloy bulk. S5. The W-3Re alloy block prepared in step S4 is polished with silicon carbide sandpaper of 80 mesh, 400 mesh, 800 mesh, 2000 mesh and 3000 mesh in sequence. Then, the tungsten alloy surface is mechanically polished with diamond suspension to make the tungsten alloy surface appear as a mirror. S6. Electrolyze the mechanically polished W-3Re tungsten alloy from step S5 using a 5% sodium hydroxide solution at an electrolysis voltage of 10 V. S7. Place the W-3Re alloy treated in step S6 at 500 keV He 2+ The irradiation was carried out at a temperature of 800℃, and the peak irradiation damage dose was 5.07 dpa.

[0027] The W-3Re alloy before and after irradiation in this embodiment were characterized to obtain the following results: Figure 3 The EDS diagram of the W-3Re alloy matrix before irradiation is shown below. Figure 4 The distribution of helium bubbles at grain boundary sites of W-3Re after irradiation (as shown in Figure a) and the size diagram (as shown in Figure b) are shown below. Figure 5 The diagram shows the helium bubble number density and grain boundary swelling rate of W-3Re at the grain boundary after irradiation.

[0028] Figure 3 Figures (a), (b), and (c) show the EDS diagrams of the W-3Re alloy matrix before irradiation, as well as the distribution diagrams of W and Re, respectively. It can be seen that in the prepared W-3Re alloy, Re is uniformly distributed in the W matrix without segregation, and solid solution of Re in W is achieved.

[0029] from Figure 4 As can be seen, the average size of helium bubbles at the grain boundary of the W-3Re alloy after helium ion irradiation is 5.2 nm.

[0030] from Figure 5 As can be seen, the helium bubble number density at the grain boundaries of the W-3Re alloy after helium ion irradiation is 2.3 × 10⁻⁶. 23 m -3 The corresponding swelling rate was 1.7%.

[0031] Example 2 This embodiment proposes a W-10Re alloy with grain boundary irradiation damage mitigation properties and its preparation method, specifically including the following steps: S1. Add 50 g of citric acid to deionized water and stir until completely dissolved. Then add 12.36 g of ammonium metatungstate, 1.44 g of ammonium perrhenate and 2.5 g of polyethylene glycol in sequence. Place the solution in a 70 ℃ water bath and stir at 500 r / min for 6 h until a uniform sol is formed. S2. The sol obtained in step S1 is dried at 150 °C for 15 h, and then calcined in air at 700 °C for 10 h to obtain nano-oxide powder; S3. The oxide powder obtained in step S2 is reduced at 800 °C for 5 h in a hydrogen atmosphere to obtain W-10Re alloy powder; S4. The W-10Re alloy powder obtained in step S3 is subjected to SPS sintering in a vacuum environment at a temperature of 1700 ℃, a pressure of 30 MPa, and a holding time of 8 min to obtain W-10Re alloy bulk. S5. The W-10Re alloy block prepared in step S4 is polished with silicon carbide sandpaper of 80 mesh, 400 mesh, 800 mesh, 2000 mesh and 3000 mesh in sequence. Then, the tungsten alloy surface is mechanically polished with diamond suspension to make the tungsten alloy surface appear as a mirror. S6. Electrolyze the mechanically polished W-10Re tungsten alloy from step S5 using a 5% sodium hydroxide solution at an electrolysis voltage of 10 V. S7. Place the W-10Re alloy treated in step S6 at 500 keV He 2+ The irradiation was carried out at a temperature of 800℃, and the peak irradiation damage dose was 5.07 dpa.

[0032] The W-10Re alloy before and after irradiation in this embodiment were characterized to obtain the following results: Figure 6 The EDS diagram of the W-10Re alloy matrix before irradiation is shown below. Figure 7 The distribution of helium bubbles at grain boundary locations of W-10Re after irradiation (as shown in Figure a) and the size diagram (as shown in Figure b) are shown below. Figure 8 The diagram shows the helium bubble number density and grain boundary swelling rate of W-10Re at the grain boundary after irradiation.

[0033] Figure 6 Figures (a), (b), and (c) show the EDS diagrams of the W-10Re alloy matrix before irradiation, as well as the distribution diagrams of W and Re, respectively. It can be seen that in the prepared W-10Re alloy, Re is uniformly distributed in the W matrix without segregation, and solid solution of Re in W is achieved.

[0034] from Figure 7 As can be seen, the average size of helium bubbles at the grain boundary of the W-10Re alloy after helium ion irradiation is 5.3 nm.

[0035] from Figure 8 As can be seen, the helium bubble number density at the grain boundaries of the W-10Re alloy after helium ion irradiation is 2.0 × 10⁻⁶. 23 m -3 The corresponding swelling rate was 1.6%.

[0036] Example 3 This embodiment proposes a W-20Re alloy with grain boundary irradiation damage mitigation properties and its preparation method, specifically including the following steps: S1. Add 45 g of citric acid to deionized water and stir until completely dissolved. Then add 10.98 g of ammonium metatungstate, 2.88 g of ammonium perrhenate and 1.1 g of polyethylene glycol in sequence. Place the solution in an 80 ℃ water bath and stir at 300 r / min for 5 h until a uniform sol is formed. S2. The sol obtained in step S1 is dried at 100 °C for 20 h, and then calcined in air at 600 °C for 8 h to obtain nano-oxide powder; S3. The oxide powder obtained in step S2 is reduced at 700 °C for 6 h in a hydrogen atmosphere to obtain W-20Re alloy powder; S4. The W-20Re alloy powder obtained in step S3 is subjected to SPS sintering in a vacuum environment at a temperature of 1800 ℃, a pressure of 30 MPa, and a holding time of 8 min to obtain W-20Re alloy bulk. S5. The W-20Re alloy block prepared in step S4 is polished with silicon carbide sandpaper of 80 mesh, 400 mesh, 800 mesh, 2000 mesh and 3000 mesh in sequence. Then, the tungsten alloy surface is mechanically polished with diamond suspension to make the tungsten alloy surface appear as a mirror. S6. Electrolyze the mechanically polished W-20Re tungsten alloy from step S5 using a 5% sodium hydroxide solution at an electrolysis voltage of 10 V. S7. Place the W-20Re alloy treated in step S6 at 500 keV He 2+ The irradiation was carried out at a temperature of 800℃, and the peak irradiation damage dose was 5.07 dpa.

[0037] The W-20Re alloy before and after irradiation in this embodiment were characterized to obtain the following results: Figure 9 The XRD pattern of the reduced W-20Re alloy powder is shown below. Figure 10 The matrix EDS diagram of W-20Re alloy before irradiation is shown below. Figure 11 The distribution of helium bubbles at grain boundary locations of W-20Re after irradiation (as shown in Figure a) and the size diagram (as shown in Figure b) are shown below. Figure 12 The diagram shows the helium bubble number density and grain boundary swelling rate of W-20Re at the grain boundary after irradiation.

[0038] from Figure 9 As can be seen from the XRD diffraction peaks of the reduced W-20Re alloy powder, only the diffraction peaks of W are present, and no diffraction peaks of Re or intermetallic compounds are observed, proving that Re has achieved complete solid solution in W.

[0039] Figure 10Figures (a), (b), and (c) show the EDS diagram of the W-20Re alloy matrix before irradiation, and the distribution diagrams of W and Re, respectively. It can be seen that in the prepared W-20Re alloy, Re is uniformly distributed in the W matrix without segregation, and solid solution of Re in W is achieved.

[0040] from Figure 11 As can be seen, the average size of helium bubbles at the grain boundary of the W-20Re alloy after helium ion irradiation is 5.3 nm.

[0041] from Figure 12 As can be seen, the helium bubble number density at the grain boundaries of the W-20Re alloy after helium ion irradiation is 1.7 × 10⁻⁶. 23 m -3 The corresponding swelling rate was 1.3%.

[0042] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0043] The embodiments described above are merely illustrative 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 invention patent. 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 all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.

Claims

1. A method for preparing a W-Re alloy with grain boundary irradiation damage mitigation properties, characterized in that, Includes the following steps: Ammonium metatungstate, ammonium perrhenate, and polyethylene glycol were dissolved in an aqueous citric acid solution, heated, and stirred to obtain a homogeneous sol; the amount of polyethylene glycol added was 10-21% of the mass of ammonium metatungstate. After the sol is dried, it is calcined in air to obtain oxide precursor powder; The oxide precursor powder was reduced in a hydrogen-containing environment to obtain W-Re alloy powder. W-Re alloy powder was sintered in a vacuum environment to obtain W-Re alloy.

2. The preparation method according to claim 1, characterized in that, The W-Re alloy comprises, by mass percentage, 80-97 wt.% W and 3-20 wt.% Re.

3. The preparation method according to claim 1, characterized in that, The molar ratio of ammonium metatungstate to citric acid is 2:25-50.

4. The preparation method according to claim 1, characterized in that, The heating temperature is 60-90 ℃.

5. The preparation method according to claim 1, characterized in that, The stirring speed is 200-600 r / min, and the stirring time is 3-7 h.

6. The preparation method according to claim 1, characterized in that, The drying temperature is 90-160 ℃, and the drying time is 12-24 h.

7. The preparation method according to claim 1, characterized in that, The calcination temperature is 500-800 ℃, and the calcination time is 6-12 h.

8. The preparation method according to claim 1, characterized in that, The reduction temperature is 700-900 ℃, and the reduction time is 4-6 h.

9. The preparation method according to claim 1, characterized in that, The sintering is spark plasma sintering; the sintering temperature is 1600-1800 ℃ and the pressure is 20-30 MPa.