Titanium alloy plate for elastic sealing and elastic connection and preparation method thereof
Through multi-stage aging, dynamic rolling and stress gradient leveling methods, the microstructure of titanium alloy sheets is optimized, and the problems of titanium alloy sheets in high elastic properties and deformation recovery are solved, and the preparation of titanium alloy sheets with low elastic modulus and high shear modulus is realized, which is suitable for elastic sealing and flexible connections.
Patent Information
- Application Number
- CN202510766255.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-10
- Publication Date
- 2025-08-12
- Estimated Expiration
- 2045-06-10
AI Technical Summary
The existing titanium alloy materials have high elastic modulus, which is difficult to meet the application fields with strict requirements for high elastic properties and deformation recovery, and traditional preparation processes are difficult to achieve the uniformity of alloy structure and stability of performance.
Using a combination of multi-stage aging, dynamic rolling and stress gradient leveling, the microstructure of titanium alloy sheets is optimized through specific proportional design and multi-step heat treatment to achieve low elastic modulus and high shear modulus.
Titanium alloy sheets with low elastic modulus, high shear modulus and good durability were prepared, suitable for elastic seals and flexible connections, solving the performance requirements of the materials in extreme environments.
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of metal material preparation, and relates to a titanium alloy plate for elastic sealing and elastic connection and a preparation method thereof. Background Art
[0002] In recent years, titanium alloys have been widely used in high-end manufacturing fields such as aerospace, marine engineering, and medical devices due to their excellent mechanical properties, good corrosion resistance, and high specific strength. Against the backdrop of the increasing demand for lightweight, high-strength materials in modern industry, titanium alloys have become the preferred structural material for many applications due to their low density and excellent performance. However, the elastic modulus of conventional titanium alloys is generally high (approximately 110GPa), which significantly limits their further application in applications requiring high elastic properties and deformation recovery, such as critical components such as elastic seals and flexible connectors that require large elastic recovery capabilities.
[0003] The materials used for elastic seals and flexible connectors in the current market are mainly polymers and highly elastic steel. However, these materials have obvious limitations in certain properties:
[0004] 1. Polymer materials - Although they have excellent elasticity, they have poor durability and temperature resistance. They are prone to performance degradation under high temperature, strong corrosion or cyclic stress, and it is difficult to meet the long life requirements in extreme environments.
[0005] 2. Highly elastic steel - Although it has good mechanical strength, its elastic modulus is as high as about 200 GPa, making it difficult to meet sufficient elastic recovery requirements while achieving the necessary strength.
[0006] Therefore, in fields such as aerospace, deep-sea exploration, and biomedical equipment, there is an urgent need for advanced materials that combine low elastic modulus, high elastic recovery, excellent durability, and corrosion resistance. Overcoming the limitations of traditional elastic materials through material design has become a pressing challenge for the high-end equipment manufacturing industry.
[0007] However, existing research and process technologies still have obvious difficulties in the following aspects:
[0008] 1. Balancing performance optimization: How to maintain or improve the mechanical strength of the alloy while reducing the elastic modulus is a core challenge in the current design of β-type titanium alloys.
[0009] 2. Microstructure uniformity - Existing technologies make it difficult to achieve high uniformity of alloy structure in batch production, especially in terms of stress gradient control in the thickness direction and optimization of nanodomain distribution.
[0010] 3. Process complexity and consistency - Traditional preparation process steps are often limited to the optimization of a single performance and lack a multi-stage control mechanism, resulting in instability in the overall performance of the material.
[0011] In response to the above difficulties, the present invention proposes a method for preparing low elastic modulus, high-performance titanium alloy plates by combining multi-stage aging, dynamic rolling and stress gradient leveling. The titanium alloy plates obtained by this method have good mechanical and elastic properties and are suitable for elastic seals and flexible connections. Summary of the Invention
[0012] In response to the problem that the existing technology lacks elastic titanium alloy plates and is difficult to meet the specific needs of elastic sealing and elastic connection, the present invention provides a titanium alloy plate for elastic sealing and elastic connection and a preparation method thereof. By combining a specific ratio design with multi-step heat treatment and deformation treatment, fine control of the material microstructure is achieved, thereby giving the titanium alloy a low elastic modulus and a higher shear modulus.
[0013] To achieve the above object, the present invention adopts the following technical solutions:
[0014] According to one aspect of the present invention, a method for preparing a titanium alloy plate for elastic sealing and elastic connection is provided, the method specifically comprising the following steps:
[0015] Step 1: Prepare titanium, niobium, zirconium, titanium-tin master alloy and titanium dioxide as raw materials, press the raw materials into alloy electrodes, and then perform vacuum melting. After melting three times, forge and blank to obtain a blank; wherein, the pressing force is 1MPa~3MPa, and the blanking temperature is 800℃~1100℃;
[0016] Step 2: subject the blank to the first aging treatment at room temperature for 3 to 7 days;
[0017] Step 3: The aging-treated billet is subjected to the first rolling, and then cooled to 100°C~200°C to obtain a primary rolled product;
[0018] Step 4: Level the cooled product for the first time, and then cool it to room temperature to obtain a leveled product; wherein the leveling temperature is the temperature after cooling in step 3; the leveling times are 1 to 3 times, and the cooling rate after leveling is 5°C / min to 30°C / min;
[0019] Step 5: subject the once-leveled product to a second aging treatment at a temperature of 70°C for 3 days to obtain a second-aged product;
[0020] Step 6: The secondary aged product is rolled for the second time, and then cooled to 200°C~300°C at a set speed. After holding for 1 hour, the cooling speed is kept constant and further cooled to 20°C~30°C to obtain a secondary rolled product.
[0021] Step 7: The secondary rolled product is subjected to a third rolling, and then cooled to 50°C to 100°C to obtain a tertiary rolled product;
[0022] Step 8: The tertiary rolled product is leveled for the second time. The leveling temperature is the temperature reached at the end of cooling in step 7. The leveling times are 1 to 3 times. The product is then cooled to room temperature at a cooling rate of 5°C / min to 30°C / min to obtain a secondary leveled product.
[0023] Step 9: The secondary leveled product is aged at room temperature for 1 day to perform a first tissue control treatment to obtain a primary tissue control product;
[0024] Step 10: Annealing the primary tissue control product, cooling it to 100°C to 300°C after annealing to obtain an annealed product;
[0025] Step 11: The annealed product is leveled for the third time. The leveling temperature is the temperature reached at the end of step 10. The leveling times are 1 to 3 times. The product is then cooled to room temperature at a cooling rate of 5°C / min to 30°C / min to obtain a three-leveled product.
[0026] Step 12: Pre-stretch the tertiary leveling product to obtain a secondary tissue control product;
[0027] Step 13: performing creep orthopedic treatment on the secondary tissue-regulated product to obtain a final tissue-regulated product;
[0028] Step 14: The final tissue-regulated product is sequentially sanded, polished, and cut to obtain a titanium alloy plate for elastic sealing and elastic connection.
[0029] The alloy electrode composition satisfies the following composition by mass percentage: Nb: 23.5% to 26%, Zr: 3% to 6%, Sn: 6% to 10%, O: 0.05% to 0.5%, and the balance is Ti.
[0030] In step 3, the first rolling conditions are: starting rolling temperature of 500°C to 800°C, rolling deformation of 30% to 90%, 3 to 5 rolling passes; and cooling rate of 5°C / min to 30°C / min.
[0031] In step 6, the second rolling conditions are: starting rolling temperature of 400°C to 900°C, rolling deformation of 30% to 90%, 3 to 5 rolling passes; and cooling rate of 5°C / min to 30°C / min.
[0032] In step 7, the third rolling conditions are: starting rolling temperature is 200°C to 300°C, rolling deformation is 30% to 50%, and rolling passes are 3 to 5 times.
[0033] In step 10, during the annealing process, the annealing temperature is 600° C. to 900° C., the annealing time is 1 hour to 4 hours, and the cooling rate is 5° C. / min to 30° C. / min.
[0034] In step 12, the pre-stretching direction is the second rolling direction, and the pre-stretching deformation is 1% to 3%.
[0035] In step 13, the creep correction temperature is 600° C. to 700° C., and the correction time is 5 min to 360 min.
[0036] A titanium alloy plate for elastic sealing and elastic connection is produced by the method. The titanium alloy plate for elastic sealing and elastic connection has a thickness of 1.5 mm to 10 mm, is composed of titanium, niobium, zirconium, tin, and oxygen, has an elastic modulus of 70 GPa to 90 GPa, a shear modulus of 26 GPa to 40 GPa, and a Poisson's ratio of 0.10 to 0.40.
[0037] The present invention proposes a method for preparing high-performance titanium alloy plates through multi-stage leveling treatment and optimized tissue control process, which solves the difficulties in preparing elastic titanium alloy plates and further improves the consistency and mechanical properties of the material.
[0038] Technical benefits: Compared with traditional elastic materials and existing β-type titanium alloy preparation methods, the present invention has unique advantages in the systematic design of organizational regulation, process sequence and performance optimization, providing a new technical path to meet the demand for materials with elasticity, strength and stability in extreme environments.
[0039] This invention addresses the limitations of existing titanium alloy sheet preparation methods by precisely designing the combined sequence and interaction principles of aging, rolling, and leveling steps to achieve comprehensive optimization of microstructure and mechanical properties. Compared to foil, this invention faces greater technical challenges in the comprehensive control of material thickness, uniformity, and mechanical properties, requiring global optimization of the processing technology to achieve a balance between high strength, superelasticity, and excellent flatness in the sheet. Specifically, based on the theory of multi-stage dynamic microstructure regulation, this invention combines the point defect recombination effect of room temperature aging with the nonlinear lattice distortion model of dynamic rolling for the first time. Through the stress gradient reconstruction theory of multiple leveling steps, it gradually releases internal stress, refines the grain structure, and constructs a periodic nanodomain structure. Compared to certain processing steps that may exist independently in the prior art, this invention clearly stipulates that only by strictly following the step sequence of this invention can the unique thermodynamic and kinetic effects of each stage be synergistic, thereby ensuring the alloy sheet's superelasticity, high strength, and excellent flatness. It is particularly important to emphasize that each stage of the invention relies on specific physicochemical mechanisms that will completely fail if the step sequence is disrupted. For example, the first room temperature aging treatment optimizes the initial structure by reorganizing point defects, while the subsequent dynamic rolling forms a long-range ordered structure by inducing grain boundary migration; if the order of aging and rolling is reversed, it will lead to disorder of nanodomains and uncontrollable performance. At the same time, the leveling step further improves the flatness of the material through stress field reconstruction and interface nucleation effect. This effect requires the stress gradient distribution of the previous stage to be achieved. Therefore, the innovation of the present invention is not only reflected in the combination of processing steps, but also in the deep physical principles behind the multi-stage processing process and its inseparable internal connection. Through this strict step control and unique theoretical design, the present invention effectively solves the technical bottlenecks of titanium alloy plates in the prior art in mechanical properties, microstructure uniformity and processing stability, and has extremely high innovation and industrial application value. Compared with the prior art, any step in the method of the present invention cannot achieve the effect described in the present invention when applied alone or adjusted in sequence. Therefore, it has significant technological advancement and the necessity of patent protection.
[0040] It is particularly important to emphasize that the technical solutions of the present invention differ fundamentally in the application requirements of sheet materials and foil materials. The core difficulty in sheet material processing lies in controlling the microstructural uniformity and internal residual stress distribution in the thickness direction, which requires precise control of the three-dimensional stress field through multiple rolling and leveling steps in a specific sequence. Foil preparation, on the other hand, focuses more on suppressing local microcracks and controlling warpage of extremely thin materials under dynamic deformation. To address this difference, the present invention innovatively introduces the following key steps and principles:
[0041] Multi-stage dynamic rolling after room temperature aging - Through dynamic lattice control in multiple temperature zones, the internal grain distribution of thicker plates is optimized to ensure uniform internal stress.
[0042] The gradual stress release mechanism of multiple leveling - the stress gradient reconstruction theory based on the thickness direction during the plate leveling process effectively avoids the local internal stress accumulation phenomenon caused by the large plate thickness.
[0043] Construction of periodic distribution of nanodomains - by precisely controlling the rolling and cooling rates, a regular arrangement of niobium-rich and niobium-poor regions within the plate is achieved, thereby establishing the plate's unique superelasticity and high-strength compatibility properties in the thickness direction. DETAILED DESCRIPTION
[0044] In order to enable those skilled in the art to better understand the present invention, the technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without making creative efforts should fall within the scope of protection of the present invention.
[0045] Example 1:
[0046] In this embodiment, a titanium alloy plate for elastic sealing and elastic connection and a preparation method thereof are provided, and the following steps are performed in sequence:
[0047] (1) Prepare high-purity raw materials of pure titanium, pure niobium, pure zirconium, titanium-tin master alloy and titanium dioxide, so that the weight percentage of the alloy components satisfies Nb: 24%, Zr: 5%, Sn: 7.5%, O: 0.5%, and the balance is Ti; press the raw materials into alloy electrodes with a pressing force of 3 MPa; vacuum melt for 3 times; then forge and open the blank at a blanking temperature of 1000°C.
[0048] (2) The first aging treatment is at room temperature and lasts for 3 days.
[0049] (3) For the first rolling, the starting rolling temperature was 800 °C, the rolling deformation was 30%, the rolling passes were 3, and then the steel was cooled to 100 °C at a cooling rate of 30 °C / min.
[0050] (4) The first leveling temperature is the temperature reached at the end of cooling in step 3. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 30°C / min.
[0051] (5) The second aging treatment is carried out at a temperature of 70°C and a aging time of 3 days.
[0052] (6) The second rolling process starts at a rolling temperature of 600 °C, with a rolling deformation of 30% and three rolling passes. The steel is then cooled to 200 °C at a cooling rate of 30 °C / min, kept at this temperature for 1 h, and further cooled to 20 °C at a cooling rate of 30 °C / min.
[0053] (7) The third rolling process starts at a rolling temperature of 200°C, with a rolling deformation of 30% and 5 rolling passes, followed by cooling to 100°C.
[0054] (8) The second leveling temperature is the temperature reached at the end of cooling in step 7. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 30 °C / min.
[0055] (9) The first tissue conditioning treatment is room temperature aging for 1 day.
[0056] (10) Annealing treatment: annealing temperature 700℃, annealing time 2h, cooling to 100℃ after annealing, cooling rate 30℃ / min.
[0057] (11) The third leveling is performed. The leveling temperature is the temperature reached at the end of cooling in step 10. The leveling is performed twice, and then cooled to room temperature at a cooling rate of 30°C / min.
[0058] (12) The second tissue control treatment is to perform pre-stretching treatment, the pre-stretching direction is the second rolling direction, and the pre-stretching deformation is 1%.
[0059] (13) The final tissue control treatment is creep correction treatment, the correction temperature is 600℃, and the correction time is 5min.
[0060] (14) Sanding, grinding, and cutting are performed to obtain titanium alloy plates for elastic sealing and elastic connection.
[0061] The method was used to produce a 10mm thick titanium alloy sheet for elastic sealing and elastic connection, with good flatness and a periodic nanodomain structure. The sheet exhibited a high strength of 1030 MPa, a recoverable strain of 2%, an elastic modulus of 70 GPa, a shear modulus of 28 GPa, and a Poisson's ratio of 0.25.
[0062] Example 2:
[0063] In this embodiment, a titanium alloy plate for elastic sealing and elastic connection and a preparation method thereof are provided, and the following steps are performed in sequence:
[0064] (1) Prepare high-purity raw materials of pure titanium, pure niobium, pure zirconium, titanium-tin master alloy and titanium dioxide, so that the weight percentage of the alloy components satisfies Nb: 24%, Zr: 5%, Sn: 7.5%, O: 0.5%, and the balance is Ti; press the raw materials into alloy electrodes with a pressing force of 3 MPa; vacuum melt for 3 times; then forge and open the blank at a blanking temperature of 1000°C.
[0065] (2) The first aging treatment is at room temperature and lasts for 3 days.
[0066] (3) For the first rolling, the starting rolling temperature was 700 °C, the rolling deformation was 30%, the rolling passes were 3, and then the steel was cooled to 100 °C at a cooling rate of 30 °C / min.
[0067] (4) The first leveling temperature is the temperature reached at the end of cooling in step 3. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 30°C / min.
[0068] (5) The second aging treatment is carried out at a temperature of 70°C and a aging time of 3 days.
[0069] (6) The second rolling process starts at a rolling temperature of 800 °C, with a rolling deformation of 70% and three rolling passes. The steel is then cooled to 200 °C at a cooling rate of 30 °C / min, kept at this temperature for 1 h, and further cooled to 20 °C at a cooling rate of 30 °C / min.
[0070] (7) The third rolling process starts at a rolling temperature of 300°C, with a rolling deformation of 30% and three rolling passes, followed by cooling to 100°C.
[0071] (8) The second leveling temperature is the temperature reached at the end of step 7, the leveling is performed once, and then cooled to room temperature at a cooling rate of 30 °C / min.
[0072] (9) The first tissue conditioning treatment is room temperature aging for 1 day.
[0073] (10) Annealing treatment: annealing temperature 900℃, annealing time 2h, cooling to 100℃ after annealing, cooling rate 30℃ / min.
[0074] (11) The third leveling is performed. The leveling temperature is the temperature reached at the end of cooling in step 10. The leveling is performed twice, and then cooled to room temperature at a cooling rate of 30°C / min.
[0075] (12) The second tissue control treatment is to perform pre-stretching treatment, the pre-stretching direction is the second rolling direction, and the pre-stretching deformation is 1%.
[0076] (13) The final tissue control treatment is creep correction treatment, the correction temperature is 700℃, and the correction time is 360min.
[0077] (14) Sanding, grinding, and cutting are performed to obtain titanium alloy plates for elastic sealing and elastic connection.
[0078] The method is used to produce a titanium alloy plate for elastic sealing and elastic connection, which has a thickness of 6.5 mm, good flatness, and a periodic nanodomain structure. The plate has a high strength of 1050 MPa, a recoverable strain of 2.2%, an elastic modulus of 73 GPa, a shear modulus of 26 GPa, and a Poisson's ratio of 0.40.
[0079] Example 3:
[0080] In this embodiment, a titanium alloy plate for elastic sealing and elastic connection and a preparation method thereof are provided, and the following steps are performed in sequence:
[0081] (1) Prepare high-purity raw materials of pure titanium, pure niobium, pure zirconium, titanium-tin master alloy and titanium dioxide, so that the weight percentage of the alloy components satisfies Nb: 24%, Zr: 5%, Sn: 7.5%, O: 0.5%, and the balance is Ti; press the raw materials into alloy electrodes with a pressing force of 3 MPa; vacuum melt for 3 times; then forge and open the blank at a blanking temperature of 1000°C.
[0082] (2) The first aging treatment is at room temperature and lasts for 3 days.
[0083] (3) For the first rolling, the starting rolling temperature was 800 °C, the rolling deformation was 50%, the rolling passes were 5, and then the steel was cooled to 100 °C at a cooling rate of 30 °C / min.
[0084] (4) The first leveling temperature is the temperature reached at the end of cooling in step 3. The leveling is repeated once, and then cooled to room temperature at a cooling rate of 30°C / min.
[0085] (5) The second aging treatment is carried out at a temperature of 70°C and a aging time of 3 days.
[0086] (6) The second rolling process starts at a rolling temperature of 400 °C, with a rolling deformation of 50% and five rolling passes. The steel is then cooled to 200 °C at a cooling rate of 30 °C / min, kept at this temperature for 1 h, and then cooled to 20 °C at a cooling rate of 30 °C / min.
[0087] (7) The third rolling process starts at a rolling temperature of 200°C, with a rolling deformation of 50% and 5 rolling passes, followed by cooling to 50°C.
[0088] (8) The second leveling temperature is the temperature reached at the end of cooling in step 7. The leveling is repeated 3 times, and then cooled to room temperature at a cooling rate of 30 °C / min.
[0089] (9) The first tissue conditioning treatment is room temperature aging for 1 day.
[0090] (10) Annealing treatment: annealing temperature 700℃, annealing time 1h, cooling to 100℃ after annealing, cooling rate 30℃ / min.
[0091] (11) The third leveling is performed. The leveling temperature is the temperature reached at the end of cooling in step 10. The leveling is performed 3 times, and then cooled to room temperature at a cooling rate of 30°C / min.
[0092] (12) The second tissue control treatment is to perform pre-stretching treatment, the pre-stretching direction is the second rolling direction, and the pre-stretching deformation is 1%.
[0093] (13) The final tissue control treatment is creep correction treatment, the correction temperature is 600℃, and the correction time is 360min.
[0094] (14) Sanding, grinding, and cutting are performed to obtain titanium alloy plates for elastic sealing and elastic connection.
[0095] The method is used to produce a titanium alloy plate for elastic sealing and elastic connection, which has a thickness of 5 mm, good flatness, and a periodic nanodomain structure. The plate has a high strength of 1150 MPa, a recoverable strain of 2.8%, an elastic modulus of 80 GPa, a shear modulus of 33 GPa, and a Poisson's ratio of 0.21.
[0096] Example 4:
[0097] In this embodiment, a titanium alloy plate for elastic sealing and elastic connection and a preparation method thereof are provided, and the following steps are performed in sequence:
[0098] (1) Prepare high-purity raw materials of pure titanium, pure niobium, pure zirconium, titanium-tin master alloy and titanium dioxide, so that the weight percentage of the alloy components satisfies Nb: 24%, Zr: 5%, Sn: 7.5%, O: 0.5%, and the balance is Ti; press the raw materials into alloy electrodes with a pressing force of 3 MPa; vacuum melt for 3 times; then forge and open the blank at a blanking temperature of 1000°C.
[0099] (2) The first aging treatment is at room temperature and the aging time is 7 days.
[0100] (3) For the first rolling, the starting rolling temperature was 500 °C, the rolling deformation was 30%, the rolling passes were 3, and then the steel was cooled to 200 °C at a cooling rate of 10 °C / min.
[0101] (4) The first leveling temperature is the temperature reached at the end of cooling in step 3. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 10°C / min.
[0102] (5) The second aging treatment is carried out at a temperature of 70°C and a aging time of 3 days.
[0103] (6) The second rolling process starts at a rolling temperature of 600 °C, with a rolling deformation of 70% and three rolling passes. The steel is then cooled to 300 °C at a cooling rate of 10 °C / min, kept at this temperature for 1 h, and further cooled to 20 °C at a cooling rate of 10 °C / min.
[0104] (7) The third rolling process starts at a rolling temperature of 200°C, with a rolling deformation of 50% and 5 rolling passes, followed by cooling to 50°C.
[0105] (8) The second leveling temperature is the temperature reached at the end of cooling in step 7. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 10 °C / min.
[0106] (9) The first tissue conditioning treatment is room temperature aging for 1 day.
[0107] (10) Annealing treatment: annealing temperature 700℃, annealing time 2h, cooling to 100℃ after annealing, cooling rate 10℃ / min.
[0108] (11) The third leveling is performed. The leveling temperature is the temperature reached at the end of cooling in step 10. The leveling is performed twice, and then cooled to room temperature at a cooling rate of 10°C / min.
[0109] (12) The second tissue control treatment is to perform pre-stretching treatment, the pre-stretching direction is the second rolling direction, and the pre-stretching deformation is 2%.
[0110] (13) The final tissue control treatment is creep correction treatment, the correction temperature is 600℃, and the correction time is 360min.
[0111] (14) Sanding, grinding, and cutting are performed to obtain titanium alloy plates for elastic sealing and elastic connection.
[0112] The method is used to produce a titanium alloy plate for elastic sealing and elastic connection, which has a thickness of 6 mm, good flatness, and a periodic nanodomain structure. The plate has a high strength of 1100 MPa, a recoverable strain of 2.4%, an elastic modulus of 78 GPa, a shear modulus of 30 GPa, and a Poisson's ratio of 0.30.
[0113] Example 5:
[0114] In this embodiment, a titanium alloy plate for elastic sealing and elastic connection and a preparation method thereof are provided, and the following steps are performed in sequence:
[0115] (1) Prepare high-purity raw materials of pure titanium, pure niobium, pure zirconium, titanium-tin master alloy and titanium dioxide, so that the weight percentage of the alloy components satisfies Nb: 24%, Zr: 5%, Sn: 7.5%, O: 0.5%, and the balance is Ti; press the raw materials into alloy electrodes with a pressing force of 3 MPa; vacuum melt for 3 times; then forge and open the blank at a blanking temperature of 1000°C.
[0116] (2) The first aging treatment is at room temperature and lasts for 3 days.
[0117] (3) For the first rolling, the starting rolling temperature was 800 °C, the rolling deformation was 50%, the rolling passes were 5, and then the steel was cooled to 200 °C at a cooling rate of 5 °C / min.
[0118] (4) The first leveling temperature is the temperature reached at the end of cooling in step 3. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 5°C / min.
[0119] (5) The second aging treatment is carried out at a temperature of 70°C and a aging time of 3 days.
[0120] (6) The second rolling process starts at a rolling temperature of 600 °C, with a rolling deformation of 50% and five rolling passes. The steel is then cooled to 300 °C at a cooling rate of 5 °C / min, kept at this temperature for 1 h, and further cooled to 30 °C at a cooling rate of 5 °C / min.
[0121] (7) The third rolling process starts at a rolling temperature of 200°C, with a rolling deformation of 50% and 5 rolling passes, followed by cooling to 50°C.
[0122] (8) The second leveling is performed at the temperature reached at the end of step 7. The leveling is repeated 3 times, and then cooled to room temperature at a cooling rate of 10°C / min.
[0123] (9) The first tissue conditioning treatment is room temperature aging for 1 day.
[0124] (10) Annealing treatment: annealing temperature 600℃, annealing time 4h, cooling to 300℃ after annealing, cooling rate 10℃ / min.
[0125] (11) The third leveling is performed. The leveling temperature is the temperature reached at the end of cooling in step 10. The leveling is performed 3 times, and then cooled to room temperature at a cooling rate of 10°C / min.
[0126] (12) The second tissue control treatment is to perform pre-stretching treatment, the pre-stretching direction is the second rolling direction, and the pre-stretching deformation is 1%.
[0127] (13) The final tissue control treatment is creep correction treatment, the correction temperature is 600℃, and the correction time is 180min.
[0128] (14) Sanding, grinding, and cutting are performed to obtain titanium alloy plates for elastic sealing and elastic connection.
[0129] The method is used to prepare a titanium alloy plate for elastic sealing and elastic connection, which has a thickness of 5 mm, good flatness, and a periodic nanodomain structure. The plate has a high strength of 1180 MPa, a recoverable strain of 1.8%, an elastic modulus of 85 GPa, a shear modulus of 38 GPa, and a Poisson's ratio of 0.12.
[0130] Example 6:
[0131] In this embodiment, a titanium alloy plate for elastic sealing and elastic connection and a preparation method thereof are provided, and the following steps are performed in sequence:
[0132] (1) Prepare high-purity raw materials of pure titanium, pure niobium, pure zirconium, titanium-tin master alloy and titanium dioxide, so that the weight percentage of the alloy components satisfies Nb: 24%, Zr: 5%, Sn: 7.5%, O: 0.5%, and the balance is Ti; press the raw materials into alloy electrodes with a pressing force of 3 MPa; vacuum melt for 3 times; then forge and open the blank at a blanking temperature of 1000°C.
[0133] (2) The first aging treatment is at room temperature and lasts for 3 days.
[0134] (3) For the first rolling, the starting rolling temperature was 800 °C, the rolling deformation was 70%, the rolling passes were 3, and then the steel was cooled to 100 °C at a cooling rate of 20 °C / min.
[0135] (4) The first leveling temperature is the temperature reached at the end of cooling in step 3. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 20°C / min.
[0136] (5) The second aging treatment is carried out at a temperature of 70°C and a aging time of 3 days.
[0137] (6) The second rolling process starts at a rolling temperature of 700 °C, with a rolling deformation of 70% and three rolling passes. The steel is then cooled to 200 °C at a cooling rate of 20 °C / min, kept at this temperature for 1 h, and further cooled to 20 °C at a cooling rate of 20 °C / min.
[0138] (7) The third rolling process starts at a rolling temperature of 200°C, with a rolling deformation of 30% and three rolling passes, followed by cooling to 50°C.
[0139] (8) The second leveling is performed at the temperature reached at the end of step 7. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 5°C / min.
[0140] (9) The first tissue conditioning treatment is room temperature aging for 1 day.
[0141] (10) Annealing treatment: annealing temperature 700℃, annealing time 2h, cooling to 100℃ after annealing, cooling rate 5℃ / min.
[0142] (11) The third leveling is performed. The leveling temperature is the temperature reached at the end of cooling in step 10. The leveling is performed twice, and then cooled to room temperature at a cooling rate of 20°C / min.
[0143] (12) The second tissue control treatment is to perform pre-stretching treatment, the pre-stretching direction is the second rolling direction, and the pre-stretching deformation is 1.5%.
[0144] (13) The final tissue control treatment is creep correction treatment, the correction temperature is 700℃, and the correction time is 360min.
[0145] (14) Sanding, grinding, and cutting are performed to obtain titanium alloy plates for elastic sealing and elastic connection.
[0146] The method is used to produce a titanium alloy plate for elastic sealing and elastic connection, which has a thickness of 3 mm, good flatness, and a periodic nanodomain structure. The plate has a high strength of 1200 MPa, a recoverable strain of 2.1%, an elastic modulus of 88 GPa, a shear modulus of 40 GPa, and a Poisson's ratio of 0.10.
[0147] Example 7:
[0148] In this embodiment, a titanium alloy plate for elastic sealing and elastic connection and a preparation method thereof are provided, and the following steps are performed in sequence:
[0149] (1) Prepare high-purity raw materials of pure titanium, pure niobium, pure zirconium, titanium-tin master alloy and titanium dioxide, so that the weight percentage of the alloy components satisfies Nb: 24%, Zr: 5%, Sn: 7.5%, O: 0.5%, and the balance is Ti; press the raw materials into alloy electrodes with a pressing force of 3 MPa; vacuum melt for 3 times; then forge and open the blank at a blanking temperature of 1000°C.
[0150] (2) The first aging treatment is at room temperature and lasts for 3 days.
[0151] (3) For the first rolling, the starting rolling temperature was 800 °C, the rolling deformation was 90%, the rolling passes were 5, and then the steel was cooled to 100 °C at a cooling rate of 5 °C / min.
[0152] (4) The first leveling temperature is the temperature reached at the end of cooling in step 3. The leveling is repeated 3 times, and then cooled to room temperature at a cooling rate of 5°C / min.
[0153] (5) The second aging treatment is carried out at a temperature of 70°C and a aging time of 3 days.
[0154] (6) The second rolling process starts at a rolling temperature of 900 °C, with a rolling deformation of 90% and five rolling passes. The steel is then cooled to 200 °C at a cooling rate of 5 °C / min, kept at this temperature for 1 h, and further cooled to 30 °C at a cooling rate of 5 °C / min.
[0155] (7) The third rolling process starts at a rolling temperature of 300°C, with a rolling deformation of 30% and three rolling passes, followed by cooling to 100°C.
[0156] (8) The second leveling temperature is the temperature reached at the end of step 7. The leveling is repeated 3 times, and then cooled to room temperature at a cooling rate of 5 °C / min.
[0157] (9) The first tissue conditioning treatment is room temperature aging for 1 day.
[0158] (10) Annealing treatment: annealing temperature 900℃, annealing time 4h, cooling to 300℃ after annealing, cooling rate 5℃ / min.
[0159] (11) The third leveling is performed. The leveling temperature is the temperature reached at the end of cooling in step 10. The leveling is performed once, and then cooled to room temperature at a cooling rate of 5°C / min.
[0160] (12) The second tissue control treatment is to perform pre-stretching treatment, the pre-stretching direction is the second rolling direction, and the pre-stretching deformation is 3%.
[0161] (13) The final tissue control treatment is creep correction treatment, the correction temperature is 600℃, and the correction time is 360min.
[0162] (14) Sanding, grinding, and cutting are performed to obtain titanium alloy plates for elastic sealing and elastic connection.
[0163] The method is used to prepare a titanium alloy plate for elastic sealing and elastic connection, which has a thickness of 1.5 mm, good flatness, and a periodic nanodomain structure. The plate has a high strength of 1250 MPa, a recoverable strain of 2.5%, an elastic modulus of 90 GPa, a shear modulus of 34 GPa, and a Poisson's ratio of 0.32.
[0164] Example 8:
[0165] In this embodiment, a titanium alloy plate for elastic sealing and elastic connection and a preparation method thereof are provided, and the following steps are performed in sequence:
[0166] (1) Prepare high-purity raw materials of pure titanium, pure niobium, pure zirconium, titanium-tin master alloy and titanium dioxide, so that the weight percentage of the alloy components satisfies Nb: 26%, Zr: 6%, Sn: 10%, O: 0.5%, and the balance is Ti; press the raw materials into alloy electrodes with a pressing force of 1 MPa; vacuum melt for 3 times; then forge and open the blank at a blanking temperature of 1100°C.
[0167] (2) The first aging treatment is at room temperature and lasts for 3 days.
[0168] (3) For the first rolling, the starting rolling temperature was 800 °C, the rolling deformation was 30%, the rolling passes were 3, and then the steel was cooled to 100 °C at a cooling rate of 30 °C / min.
[0169] (4) The first leveling temperature is the temperature reached at the end of cooling in step 3. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 30°C / min.
[0170] (5) The second aging treatment is carried out at a temperature of 70°C and a aging time of 3 days.
[0171] (6) The second rolling process starts at a rolling temperature of 600 °C, with a rolling deformation of 30% and three rolling passes. The steel is then cooled to 200 °C at a cooling rate of 30 °C / min, kept at this temperature for 1 h, and further cooled to 20 °C at a cooling rate of 30 °C / min.
[0172] (7) The third rolling process starts at a rolling temperature of 200°C, with a rolling deformation of 30% and 5 rolling passes, followed by cooling to 100°C.
[0173] (8) The second leveling temperature is the temperature reached at the end of cooling in step 7. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 30 °C / min.
[0174] (9) The first tissue conditioning treatment is room temperature aging for 1 day.
[0175] (10) Annealing treatment: annealing temperature 700℃, annealing time 2h, cooling to 100℃ after annealing, cooling rate 30℃ / min.
[0176] (11) The third leveling is performed. The leveling temperature is the temperature reached at the end of cooling in step 10. The leveling is performed twice, and then cooled to room temperature at a cooling rate of 30°C / min.
[0177] (12) The second tissue control treatment is to perform pre-stretching treatment, the pre-stretching direction is the second rolling direction, and the pre-stretching deformation is 1%.
[0178] (13) The final tissue control treatment is creep correction treatment, the correction temperature is 600℃, and the correction time is 5min.
[0179] (14) Sanding, grinding, and cutting are performed to obtain titanium alloy plates for elastic sealing and elastic connection.
[0180] The method is used to prepare a titanium alloy plate for elastic sealing and elastic connection, which has a thickness of 10 mm, good flatness, and a periodic nanodomain structure. The plate has a high strength of 1010 MPa, a recoverable strain of 1.3%, an elastic modulus of 74 GPa, a shear modulus of 32 GPa, and a Poisson's ratio of 0.16.
[0181] Example 9:
[0182] In this embodiment, a titanium alloy plate for elastic sealing and elastic connection and a preparation method thereof are provided, and the following steps are performed in sequence:
[0183] (1) Prepare high-purity raw materials of pure titanium, pure niobium, pure zirconium, titanium-tin master alloy and titanium dioxide, so that the weight percentage of the alloy components satisfies Nb: 23.5%, Zr: 3%, Sn: 6%, O: 0.05%, and the balance is Ti; press the raw materials into alloy electrodes with a pressing force of 1 MPa; vacuum melt for 3 times; then forge and open the blank at a blanking temperature of 800°C.
[0184] (2) The first aging treatment is at room temperature and the aging time is 7 days.
[0185] (3) For the first rolling, the starting rolling temperature was 500 °C, the rolling deformation was 30%, the rolling passes were 3, and then the steel was cooled to 200 °C at a cooling rate of 10 °C / min.
[0186] (4) The first leveling temperature is the temperature reached at the end of cooling in step 3. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 10°C / min.
[0187] (5) The second aging treatment is carried out at a temperature of 70°C and a aging time of 3 days.
[0188] (6) The second rolling process starts at a rolling temperature of 600 °C, with a rolling deformation of 70% and three rolling passes. The steel is then cooled to 300 °C at a cooling rate of 10 °C / min, kept at this temperature for 1 h, and further cooled to 20 °C at a cooling rate of 10 °C / min.
[0189] (7) The third rolling process starts at a rolling temperature of 200°C, with a rolling deformation of 50% and 5 rolling passes, followed by cooling to 50°C.
[0190] (8) The second leveling temperature is the temperature reached at the end of cooling in step 7. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 10 °C / min.
[0191] (9) The first tissue conditioning treatment is room temperature aging for 1 day.
[0192] (10) Annealing treatment: annealing temperature 700℃, annealing time 2h, cooling to 100℃ after annealing, cooling rate 10℃ / min.
[0193] (11) The third leveling is performed. The leveling temperature is the temperature reached at the end of cooling in step 10. The leveling is performed twice, and then cooled to room temperature at a cooling rate of 10°C / min.
[0194] (12) The second tissue control treatment is to perform pre-stretching treatment, the pre-stretching direction is the second rolling direction, and the pre-stretching deformation is 2%.
[0195] (13) The final tissue control treatment is creep correction treatment, the correction temperature is 600℃, and the correction time is 360min.
[0196] (14) Sanding, grinding, and cutting are performed to obtain titanium alloy plates for elastic sealing and elastic connection.
[0197] The method is used to produce a titanium alloy plate for elastic sealing and elastic connection, which has a thickness of 6 mm, good flatness, and a periodic nanodomain structure. The plate has a high strength of 1120 MPa, a recoverable strain of 1.5%, an elastic modulus of 82 GPa, a shear modulus of 35 GPa, and a Poisson's ratio of 0.17.
[0198] Comparative Example 1:
[0199] This comparative example is similar to Example 1, except that the second and third rolling of steps (6) and (7) are performed in sequence, and then the second aging treatment of step (5) is performed. The strength of the obtained titanium alloy plate is lower than 1000 MPa, the elastic modulus is lower than 70 GPa, and the nanodomain structure is disordered.
[0200] Comparative Example 2:
[0201] This comparative example is similar to Example 1, except that the pre-stretching treatment in step (12) is not performed. The strength of the titanium alloy plate obtained can recover the strain below 1%, and the elastic modulus is higher than 90 GPa.
[0202] Comparative Example 3:
[0203] (1) Prepare high-purity raw materials of pure titanium, pure niobium, pure zirconium, titanium-tin master alloy and titanium dioxide, meeting the requirements of Nb: 24%, Zr: 5%, Sn: 7.5%, O: 0.5%, and the balance is Ti; press the raw materials into alloy electrodes with a pressing force of 3 MPa; vacuum melt for 3 times; then forge and open the blank at a blanking temperature of 1000°C.
[0204] (2) The first aging treatment is at room temperature and lasts for 3 days.
[0205] (3) For the first rolling, the starting rolling temperature was 600 °C, the rolling deformation was 30%, the rolling passes were 3, and then the steel was cooled to 100 °C at a cooling rate of 20 °C / min.
[0206] (4) The first leveling temperature is the temperature reached at the end of cooling in step 3. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 20°C / min.
[0207] (5) Annealing treatment: annealing temperature 700℃, annealing time 2h, cooling to 100℃ after annealing, cooling rate 20℃ / min.
[0208] (6) The second leveling temperature is the temperature reached at the end of cooling in step 5. The leveling is repeated twice, and then cooled to room temperature at a cooling rate of 20 °C / min.
[0209] (7) Tissue control treatment, creep correction treatment, correction temperature 600℃, correction time 360min.
[0210] (8) Perform sanding, grinding and cutting.
[0211] The titanium alloy plate obtained through the above steps has a strength lower than 900 MPa, a recoverable strain lower than 1%, an elastic modulus lower than 70 GPa, and a disordered nanodomain structure.
Claims
1. A method for preparing a titanium alloy plate for elastic sealing and elastic connection, characterized in that: The method specifically consists of the following steps: Step 1: Prepare titanium, niobium, zirconium, titanium-tin master alloy and titanium dioxide as raw materials, press the raw materials into alloy electrodes, and then perform vacuum melting. After melting three times, forge and blank to obtain a blank; wherein, the pressing force is 1MPa~3MPa, and the blanking temperature is 800℃~1100℃; Step 2: subject the blank to the first aging treatment at room temperature for 3 to 7 days; Step 3: The aging-treated billet is subjected to the first rolling, and then cooled to 100°C~200°C to obtain a primary rolled product; Step 4: Level the cooled product for the first time, and then cool it to room temperature to obtain a leveled product; wherein the leveling temperature is the temperature after cooling in step 3; the leveling times are 1 to 3 times, and the cooling rate after leveling is 5°C / min to 30°C / min; Step 5: subject the once-leveled product to a second aging treatment at a temperature of 70°C for 3 days to obtain a second-aged product; Step 6: The secondary aged product is rolled for the second time, and then cooled to 200°C~300°C at a set speed. After holding for 1 hour, the cooling speed is kept constant and further cooled to 20°C~30°C to obtain a secondary rolled product. Step 7: The secondary rolled product is subjected to a third rolling, and then cooled to 50°C to 100°C to obtain a tertiary rolled product; Step 8: The tertiary rolled product is leveled for the second time. The leveling temperature is the temperature reached at the end of cooling in step 7. The leveling times are 1 to 3 times. The product is then cooled to room temperature at a cooling rate of 5°C / min to 30°C / min to obtain a secondary leveled product. Step 9: The secondary leveled product is aged at room temperature for 1 day to perform a first tissue control treatment to obtain a primary tissue control product; Step 10: Annealing the primary tissue control product, cooling it to 100°C to 300°C after annealing to obtain an annealed product; Step 11: The annealed product is leveled for the third time. The leveling temperature is the temperature reached at the end of step 10. The leveling times are 1 to 3 times. The product is then cooled to room temperature at a cooling rate of 5°C / min to 30°C / min to obtain a three-leveled product. Step 12: Pre-stretch the tertiary leveling product to obtain a secondary tissue control product; Step 13: performing creep orthopedic treatment on the secondary tissue-regulated product to obtain a final tissue-regulated product; Step 14: The final tissue-controlled product is sequentially sanded, polished, and cut to obtain a titanium alloy plate for elastic sealing and elastic connection; The alloy electrode composition meets the following requirements in terms of mass percentage: Nb: 23.5% to 26%, Zr: 3% to 6%, Sn: 6% to 10%, O: 0.05% to 0.5%, and the balance is Ti; In step 3, the first rolling conditions are: starting rolling temperature of 500°C to 800°C, rolling deformation of 30% to 90%, 3 to 5 rolling passes; cooling rate of 5°C / min to 30°C / min; In step 6, the second rolling conditions are as follows: starting rolling temperature is 400°C to 900°C, rolling deformation is 30% to 90%, rolling passes are 3 to 5 times; cooling rate is 5°C / min to 30°C / min; In step 7, the third rolling conditions are: starting rolling temperature is 200°C to 300°C, rolling deformation is 30% to 50%, and rolling passes are 3 to 5 times; In step 10, during the annealing process, the annealing temperature is 600° C. to 900° C., the annealing time is 1 hour to 4 hours, and the cooling rate is 5° C. / min to 30° C. / min; In step 13, the creep correction temperature is 600° C. to 700° C., and the correction time is 5 min to 360 min.
2. The method for preparing a titanium alloy plate for elastic sealing and elastic connection according to claim 1, characterized in that: In step 12, the pre-stretching direction is the second rolling direction, and the pre-stretching deformation is 1% to 3%.
3. A titanium alloy plate for elastic sealing and elastic connection prepared by the method according to claim 1 or 2, characterized in that: The titanium alloy plate for elastic sealing and elastic connection has a thickness of 1.5 mm to 10 mm and is composed of titanium, niobium, zirconium, tin and oxygen. Its elastic modulus is 70 GPa to 90 GPa, its shear modulus is 26 GPa to 40 GPa and its Poisson's ratio is 0.10 to 0.40.
Citation Information
Patent Citations
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CN109504876A
High-flexibility and high-strength titanium alloy foil and preparation and application thereof
CN118581352A