Nano beryllium material and preparation method thereof
Nano-beryllium materials were prepared by a segmented sintering degassing method combining cold isostatic pressing and hot isostatic pressing, which solved the problem of insufficient strength and ductility of micron-sized beryllium materials and realized high-strength and high-toughness nano-beryllium materials to meet the application needs of nuclear industry and aerospace.
Patent Information
- Application Number
- CN202511008730.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-22
- Publication Date
- 2025-11-18
AI Technical Summary
Beryllium materials prepared by existing technologies can only reach the micrometer scale, and their strength and ductility are insufficient to meet the development needs of nuclear industry, aerospace and civilian fields.
A combination of cold isostatic pressing and hot isostatic pressing is used to prepare nano-beryllium materials through segmented sintering and degassing. The process includes steps such as vacuuming, sealed cold isostatic pressing, segmented sintering, and hot isostatic pressing. The vacuum level and temperature are controlled to remove gases and impurities and improve the material density.
The prepared beryllium nanomaterials have a tensile strength greater than 700 MPa, an elongation greater than 8%, and an oxygen content of 2–4%, meeting the needs of nuclear industry, aerospace and civilian fields.
Abstract
Description
Technical Field
[0001] This invention belongs to the field of beryllium materials technology, and particularly relates to a nano-beryllium material and its preparation method. Background Technology
[0002] Beryllium is a rare, lightweight metal with excellent nuclear and physical properties, widely used as a functional and structural material in the nuclear industry, aerospace, and civilian sectors. With increasing industrial demands and diversified application scenarios, high strength, high plasticity, and high toughness have become inevitable trends in the development of metallic materials.
[0003] Because of their extremely small size, nanomaterials exhibit novel properties not found in conventional particulate materials, making them suitable for use as functional and structural materials in numerous fields. However, existing technologies can only produce beryllium materials at the micrometer scale. Micrometer-sized beryllium materials have low strength and ductility, failing to meet the development needs of the nuclear industry, aerospace, and civilian applications. Summary of the Invention
[0004] One of the objectives of this invention is to provide a method for preparing nano-beryllium materials. The nano-beryllium materials prepared by this method have high strength and high ductility, which can meet the development needs of nuclear industry, aerospace and civilian fields.
[0005] The second objective of this invention is to provide a nano-beryllium material.
[0006] To achieve one of the above objectives, the present invention employs the following technical solution:
[0007] A method for preparing nano-beryllium materials, the method comprising the following steps:
[0008] Step S1: Load 30-80 nm beryllium powder into a cold isostatic pressing sleeve;
[0009] Step S2: After evacuating the cold isostatic pressing liner, seal the cold isostatic pressing liner and the cold isostatic pressing liner in sequence to obtain beryllium powder blank;
[0010] In step S2, the pressure of the cold isostatic pressing is 280–300 MPa.
[0011] Step S3: After the beryllium powder blank is sintered and degassed in sections, it is sequentially loaded into a hot isostatic pressing (HIP) sleeve, subjected to secondary degaussing, sealed in a HIP sleeve, subjected to HIP, and removed from the HIP sleeve to obtain nano-beryllium material.
[0012] In step S3, the segmented sintering degassing includes:
[0013] In the first stage, the temperature for segmented sintering and degassing is 120–220℃, and the time is 20–30 hours.
[0014] In the second stage, the vacuum degree of the segmented sintering degassing is 7.6 × 10⁻⁶. -5 ~5.0×10 -4 Pa, temperature 610–720℃, time 1.5–3.5 hours.
[0015] Furthermore, in step S2, the vacuum level inside the cold isostatic pressing jacket after evacuation is 26-75 Pa to remove the gas adsorbed by the beryllium powder.
[0016] Furthermore, in step S3, the temperature of the first stage is 140-200°C, and the time is 23-26 hours.
[0017] Furthermore, in step S3, the vacuum level in the second stage is 1.0 × 10⁻⁶. -4 ~4.0×10 -4 PaPa, temperature 640~690℃, time 1.8~2.8 hours.
[0018] Furthermore, in step S3, the specific process of the secondary degassing is as follows:
[0019] In greater than or equal to 2.0 × 10 -3 Under a vacuum of Pa, at a temperature of 510–590 °C, degas for 12–16 hours.
[0020] Furthermore, in step S3, the vacuum degree of the secondary degassing is 8.7 × 10⁻⁶. -4 ~1.8×10 -3 Pa, temperature 530–570℃, time 13–15 hours.
[0021] Furthermore, in step S3, the pressure of the hot isostatic pressing is 90-110 MPa, the temperature is 1000-1050 °C, and the time is 8-12 hours.
[0022] To achieve the second objective mentioned above, the present invention employs the following technical solution:
[0023] A nano-beryllium material, wherein the nano-beryllium material is prepared using the preparation method described above.
[0024] Furthermore, the grain size of the beryllium nanomaterial is 20–70 nanometers.
[0025] Furthermore, the nano-beryllium material has a tensile strength greater than or equal to 700 MPa, an elongation greater than or equal to 8%, and an oxygen content of 2–4%.
[0026] In summary, the solution proposed in this invention has the following technical effects:
[0027] Compared with micron-scale beryllium materials, the nanoscale beryllium materials of this invention have significantly improved strength and ductility, achieving a breakthrough in beryllium material preparation from the micron-scale to the nanoscale. The nanoscale beryllium materials of this invention have a tensile strength greater than or equal to 700 MPa, an elongation greater than or equal to 8%, and an oxygen content of 2-4%, meeting the development needs of nuclear industry, aerospace and civilian fields. Detailed Implementation
[0028] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0029] This embodiment provides a method for preparing nano-beryllium materials, which includes the following steps:
[0030] Step S1: Load 30-80 nm beryllium powder into a cold isostatic pressing sleeve.
[0031] Step S2: After evacuating the cold isostatic pressing (COP) liner, seal the COP liner and the COP liner in sequence to obtain the beryllium powder blank.
[0032] In order to remove the gas adsorbed by the beryllium powder, eliminate the porosity of the beryllium powder particles, promote the formation of nano-beryllium materials, and improve the yield strength of nano-beryllium materials, this embodiment evacuates the cold isostatic pressing cladding, so that the vacuum degree inside the cold isostatic pressing cladding after evacuation is 26-75 Pa.
[0033] The nano-beryllium powder has a fine particle size, a large specific surface area, and poor particle flowability. In order to ensure the forming rate of the nano-beryllium material, this embodiment uses cold isostatic pressing for pressing, and the pressure of cold isostatic pressing is 280-300 MPa.
[0034] Step S3: After the beryllium powder blank is sintered and degassed in sections, it is sequentially loaded into a hot isostatic pressing (HIP) sleeve, subjected to secondary degaussing, sealed in a HIP sleeve, subjected to HIP, and removed from the HIP sleeve to obtain nano-beryllium material.
[0035] The segmented sintering degassing in this embodiment includes:
[0036] In the first stage, the temperature for segmented sintering and degassing is 120–220°C, preferably 140–200°C, and the time is 20–30 hours, preferably 23–26 hours. This can effectively remove the water vapor adsorbed by the beryllium powder blank and inhibit the formation of beryllium compounds.
[0037] In the second stage, the vacuum degree of the segmented sintering degassing is 7.6 × 10⁻⁶. -5~5.0×10 -4 Pa, preferably 1.0 × 10 -4 ~4.0×10 -4 Pa, temperature of 610-720℃, preferably 640-690℃, time of 1.5-3.5 hours, preferably 1.8-2.8 hours, to gradually eliminate the gaps between beryllium particles, increase the density of beryllium powder blank, so that the beryllium material achieves preliminary densification and has a certain strength.
[0038] To remove metallic impurities from beryllium materials and hydrogen and oxygen compounds from beryllium powder blanks, this embodiment employs secondary degassing. The specific process of secondary degassing is as follows:
[0039] In greater than or equal to 2.0 × 10 -3 Under a vacuum of Pa, at a temperature of 510–590 °C, degas for 12–16 hours.
[0040] To remove impurity oxides, ensure degassing cleanliness, and reduce the oxidation degree of beryllium materials, the gaps and pores between beryllium powder particles continue to shrink, increasing the material density. Simultaneously, this weakens the adverse effects of beryllium oxide on material properties. In this embodiment, the preferred vacuum degree for secondary degassing is 8.7 × 10⁻⁶. -4 ~1.8×10 -3 Pa, the preferred temperature is 530-570℃, and the preferred time is 13-15 hours.
[0041] In this embodiment, the hot isostatic pressing pressure is 90-110 MPa, the temperature is 1000-1050°C, and the time is 8-12 hours.
[0042] The strength and ductility of the nanoscale beryllium material in this embodiment are significantly improved, achieving a breakthrough in beryllium material preparation from the micrometer to the nanometer scale. The tensile strength of the nanoscale beryllium material in this embodiment is greater than or equal to 700 MPa, the elongation is greater than or equal to 8%, and the oxygen content is 2-4%, meeting the development needs of nuclear industry, aerospace and civilian fields.
[0043] Another embodiment provides a beryllium nanomaterial prepared using the preparation method described in the above embodiments. The beryllium nanomaterial has a grain size of 20–70 nanometers, a tensile strength greater than or equal to 700 MPa, an elongation greater than or equal to 8%, and an oxygen content of 2–4%.
[0044] The technical solution of this application is illustrated below with specific embodiments:
[0045] Example 1:
[0046] Step S1: Load 50 nm beryllium powder into a cold isostatic pressing sleeve.
[0047] Step S2: After evacuating the cold isostatic pressing package to a vacuum of 62 Pa, seal the cold isostatic pressing package, load it into a cold isostatic press, and use a pressure of 300 MPa to cold isostatically press beryllium powder blanks.
[0048] Step S3: Sinter the beryllium powder blank at 120°C for 20 hours, then at 3.5×10 -4 Under a vacuum of Pa, the temperature was raised to 710℃, and after sintering for 3.5 hours, it was placed into a hot isostatic pressing (HIP) sleeve, and then pressed at 8.7 × 10⁻⁶. -4 Under a vacuum of 100 MPa and a temperature of 590 °C, after degassing for 16 hours, the hot isostatic pressing (HIP) jacket is sealed, and the material is subjected to HIP for 8 hours at a pressure of 100 MPa and a temperature of 1000 °C. Finally, the HIP jacket is removed to obtain 40 nm beryllium nanomaterials.
[0049] The nano-beryllium material in this embodiment has a tensile strength of 723.7 MPa, an elongation of 8.6%, and an oxygen content of 3%.
[0050] Example 2:
[0051] Step S1: Load 80 nm beryllium powder into a cold isostatic pressing sleeve.
[0052] Step S2: After evacuating the cold isostatic pressing package to a vacuum of 75 Pa, seal the cold isostatic pressing package, load it into a cold isostatic press, and use a pressure of 295 MPa to cold isostatically press beryllium powder blanks.
[0053] Step S3: Sinter the beryllium powder blank at 140°C for 23 hours, then at 4.0×10 -4 Under a vacuum of Pa, the temperature was raised to 640℃, and after sintering for 2.8 hours, it was placed into a hot isostatic pressing (HIP) sleeve, and then pressed at 1.8 × 10⁻⁶. -3 Under a vacuum of 100 MPa and at a temperature of 570 °C, after degassing for 15 hours, the hot isostatic pressing (HIP) jacket is sealed, and the material is subjected to HIP for 12 hours at a pressure of 110 MPa and a temperature of 1010 °C. Finally, the HIP jacket is removed to obtain 70 nm beryllium nanomaterials.
[0054] The nano-beryllium material in this embodiment has a tensile strength of 737.5 MPa, an elongation of 9.3%, and an oxygen content of 4%.
[0055] Example 3:
[0056] Step S1: Load 30 nm beryllium powder into a cold isostatic pressing sleeve.
[0057] Step S2: After evacuating the cold isostatic pressing package to a vacuum of 26 Pa, seal the cold isostatic pressing package, load it into a cold isostatic press, and use a pressure of 280 MPa to cold isostatically press beryllium powder into a blank.
[0058] Step S3: Sinter the beryllium powder blank at 200°C for 26 hours, then at 7.6 × 10⁻⁶ °C. -5 Under a vacuum of Pa, the temperature was raised to 610℃, and after sintering for 1.5 hours, it was placed into a hot isostatic pressing (HIP) sleeve, and then pressed at 2.0 × 10⁻⁶ Pa. -3 Under a vacuum of 100 MPa and at a temperature of 530 °C, after degassing for 13 hours, the hot isostatic pressing (HIP) jacket is sealed, and the material is subjected to HIP for 10 hours at a pressure of 90 MPa and a temperature of 1020 °C. Finally, the HIP jacket is removed to obtain 20 nm beryllium nanomaterials.
[0059] The nano-beryllium material in this embodiment has a tensile strength of 753.1 MPa, an elongation of 8.1%, and an oxygen content of 2%.
[0060] Example 4:
[0061] Step S1: Load 60 nm beryllium powder into a cold isostatic pressing sleeve.
[0062] Step S2: After evacuating the cold isostatic pressing package to a vacuum of 40 Pa, seal the cold isostatic pressing package, load it into a cold isostatic press, and use a pressure of 270 MPa to cold isostatically press beryllium powder into a blank.
[0063] Step S3: Sinter the beryllium powder blank at 220°C for 30 hours, then at 5.0×10⁻⁶... -4 Under a vacuum of Pa, the temperature was raised to 720℃, and after sintering for 1.8 hours, it was placed into a hot isostatic pressing (HIP) sleeve, and then pressed at 1.4 × 10⁻⁶ Pa. -3 Under a vacuum of 100 MPa and at a temperature of 510 °C, after degassing for 12 hours, the hot isostatic pressing (HIP) jacket is sealed, and the material is subjected to HIP for 9 hours at a pressure of 100 MPa and a temperature of 1050 °C. Finally, the HIP jacket is removed to obtain 45 nm beryllium nanomaterials.
[0064] The nano-beryllium material in this embodiment has a tensile strength of 733.7 MPa, an elongation of 8.3%, and an oxygen content of 2.3%.
[0065] Example 5:
[0066] Step S1: Load 70 nm beryllium powder into a cold isostatic pressing sleeve.
[0067] Step S2: After evacuating the cold isostatic pressing package to a vacuum of 55 Pa, seal the cold isostatic pressing package, load it into a cold isostatic press, and use a pressure of 290 MPa to cold isostatically press beryllium powder into a blank.
[0068] Step S3: Sinter the beryllium powder blank at 150°C for 22 hours, then at 4.1×10 -4Under a vacuum of Pa, the temperature was raised to 690℃, and after sintering for 1.5 hours, it was placed into a hot isostatic pressing (HIP) sleeve, and then pressed at 6.9 × 10⁻⁶. -4 Under a vacuum of 100 MPa and at a temperature of 520 °C, after degassing for 14 hours, the hot isostatic pressing (HIP) jacket is sealed, and the material is subjected to HIP for 11 hours at a pressure of 100 MPa and a temperature of 1045 °C. Finally, the HIP jacket is removed to obtain 55 nm beryllium nanomaterials.
[0069] The nano-beryllium material in this embodiment has a tensile strength of 729.4 MPa, an elongation of 8.2%, and an oxygen content of 2.5%.
[0070] The above embodiments merely illustrate several implementation methods of this application, 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 this application, and these all fall within the protection scope of this application. Therefore, the protection scope of this patent application should be determined by the appended claims.
Claims
1. A method for preparing nano-beryllium materials, characterized in that, The preparation method includes the following steps: Step S1: Load 30-80 nm beryllium powder into a cold isostatic pressing sleeve; Step S2: After evacuating the cold isostatic pressing liner, seal the cold isostatic pressing liner and the cold isostatic pressing liner in sequence to obtain beryllium powder blank; In step S2, the pressure of the cold isostatic pressing is 280-300 MPa; Step S3: After the beryllium powder blank is sintered and degassed in sections, it is sequentially loaded into a hot isostatic pressing (HIP) sleeve, subjected to secondary degaussing, sealed in a HIP sleeve, subjected to HIP, and removed from the HIP sleeve to obtain nano-beryllium material. In step S3, the segmented sintering degassing includes: In the first stage, the temperature for segmented sintering and degassing is 120–220℃, and the time is 20–30 hours. In the second stage, the vacuum degree of the segmented sintering degassing is 7.6 × 10⁻⁶. -5 ~5.0×10 -4 Pa, temperature 610–720℃, time 1.5–3.5 hours.
2. The preparation method according to claim 1, characterized in that, In step S2, the vacuum level inside the cold isostatic pressing jacket after evacuation is 26–75 Pa.
3. The preparation method according to claim 2, characterized in that, In step S3, the temperature of the first stage is 140-200°C, and the time is 23-26 hours.
4. The preparation method according to claim 3, characterized in that, In step S3, the vacuum level in the second stage is 1.0 × 10⁻⁶. -4 ~4.0×10 -4 Pa, temperature 640–690℃, time 1.8–2.8 hours.
5. The preparation method according to any one of claims 1 to 4, characterized in that, In step S3, the specific process of secondary degassing is as follows: In greater than or equal to 2.0 × 10 -3 Under a vacuum of Pa, at a temperature of 510–590 °C, degas for 12–16 hours.
6. The preparation method according to claim 5, characterized in that, In step S3, the vacuum degree of the secondary degassing is 8.7 × 10⁻⁶. -4 ~1.8×10 -3 Pa, temperature 530–570℃, time 13–15 hours.
7. The preparation method according to claim 6, characterized in that, In step S3, the pressure of the hot isostatic pressing is 90-110 MPa, the temperature is 1000-1050 °C, and the time is 8-12 hours.
8. A nano-beryllium material, characterized in that, The nano-beryllium material is prepared using the preparation method described in any one of claims 1 to 7.
9. The nano-beryllium material according to claim 8, characterized in that, The grain size of the beryllium nanomaterial is 20–70 nanometers.
10. The nano-beryllium material according to claim 9, characterized in that, The nano-beryllium material has a tensile strength greater than or equal to 700 MPa, an elongation greater than or equal to 8%, and an oxygen content of 2-4%.