Preparation method of 700 DEG C micro-nano particle reinforced near-alpha high-temperature titanium alloy

By preparing a high-temperature titanium alloy with a dual-state structure of Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si, and employing micro-nano particle strengthening methods and thermomechanical processing technology, the problem of low microstructure stability at high temperatures was solved, achieving a balance between high-temperature strength and plasticity, making it suitable for aerospace and other fields.

CN117535556BActive Publication Date: 2026-04-21TAIYUAN UNIVERSITY OF TECHNOLOGY
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
TAIYUAN UNIVERSITY OF TECHNOLOGY
Filing Date
2023-12-05
Publication Date
2026-04-21

AI Technical Summary

Technical Problem

Existing high-temperature near-α titanium alloys have low microstructure stability at high temperatures, making it difficult to maintain microstructure stability while improving high-temperature strength.

Method used

A high-temperature titanium alloy with a dual-state structure, Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si, was prepared by using a micro-nano particle strengthening method through reciprocating extrusion and vacuum aging treatment. This method controls the precipitation and distribution of micro-nano particles, thereby improving the alloy's microstructure stability and high-temperature strength.

Benefits of technology

It achieves high strength, toughness, and structural stability of high-temperature titanium alloys at 700℃, making it suitable for the rapid development needs of aerospace and other fields.

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Abstract

This invention discloses a method for preparing a near-α high-temperature titanium alloy reinforced with micro / nano particles that can withstand 700℃, belonging to the field of titanium alloy material hot working technology. The specific steps are as follows: S1, casting a high-temperature titanium alloy ingot of raw material Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si; S2, in T... s S3. Solution quenching at 20-50℃ above the silicide dissolution temperature; S4. Passive cooling reciprocating extrusion at 10-50℃ below the (α+β) / β phase transformation point to obtain a near-α high-temperature titanium alloy with both high strength and toughness and structural stability; S5. Aging treatment at 650-750℃. This invention solves the problem that current near-α high-temperature titanium alloys cannot simultaneously achieve high thermal strength and structural stability, aiming to provide a high-temperature titanium alloy capable of operating at 700℃.
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Description

Technical Field

[0001] This invention belongs to the field of hot working technology of titanium alloy materials, and particularly relates to a method for preparing a near-α high-temperature titanium alloy reinforced with micro-nano particles that can withstand 700℃. Background Technology

[0002] Near-alpha high-temperature titanium alloys have long been favored by industries such as aerospace and high-end weaponry due to their advantages of being lightweight, high-strength, corrosion-resistant, and heat-resistant. Currently, the long-term heat resistance temperature of traditional near-alpha high-temperature titanium alloys has reached the thermal barrier temperature (600℃). With the rapid development of new aerospace vehicles both domestically and internationally, there is an urgent need to develop new high-temperature titanium alloy materials with even higher heat resistance levels.

[0003] High-temperature strength and microstructure stability are a major contradiction in high-temperature titanium alloys. That is, while improving high-temperature strength, microstructure stability will be reduced (microstructure stability is usually measured by room temperature plasticity after long-term heat exposure). The decrease in microstructure stability is closely related to the precipitation of silicides under high-temperature long-term service or aging conditions: (1) silicides themselves reduce plasticity; (2) silicides enhance the precipitation of ordered Ti3Al phase (α2).

[0004] If the dynamic precipitation of near-α high-temperature titanium alloy silicides and α2 and the synergistic regulation of matrix structure can be achieved based on thermoplastic deformation, it is expected that the high-temperature strength can be improved without losing its structural stability. Summary of the Invention

[0005] To address the issue of low microstructural stability in existing high-temperature near-alpha titanium alloys, this invention develops a method for preparing a near-alpha high-temperature titanium alloy reinforced with micro / nano particles that can withstand temperatures up to 700℃. This method can produce high-temperature titanium alloys that combine high strength and toughness with stable microstructure, and is suitable for large-scale industrial production.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] A near-α high-temperature titanium alloy reinforced with micro / nano particles to withstand 700℃ has a dual-state microstructure, with an equiaxed α phase volume fraction of 10-30%, a precipitated phase (TiZr)6Si3 with a size of 0.05-1μm, and a precipitated phase Ti3Al with a size of 0.1-5nm.

[0008] This invention also provides a method for preparing a near-α high-temperature titanium alloy reinforced with micro / nano particles that can withstand temperatures up to 700℃. The method uses a Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si high-temperature titanium alloy as raw material and employs a reciprocating extrusion process. Specifically, it includes the following steps:

[0009] The raw material Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si was solution treated and quenched to obtain a titanium alloy ingot.

[0010] The titanium alloy ingot is subjected to reciprocating extrusion;

[0011] The extruded sample was subjected to vacuum aging treatment to obtain a near-α high-temperature titanium alloy reinforced with micro-nano particles that can withstand 700℃.

[0012] Furthermore, the solution treatment temperature is 10-50°C above the (TiZr)6Si3 dissolution temperature, and the solution treatment time is 1-2 hours, so that all Si is dissolved into the matrix. During quenching, the billet is completely immersed in water for less than 10 seconds.

[0013] Further, the reciprocating extrusion specifically includes the following steps: placing the titanium alloy ingot sample into the right chamber of the cylindrical die channel, fixing the position of the left hydraulic arm, starting the right hydraulic arm, stopping the extrusion when the sample is completely squeezed into the left chamber, and retracting the right hydraulic arm to a set length and fixing it in place, while the left hydraulic arm presses the sample back in the opposite direction according to the above process, stopping the extrusion when the sample is completely squeezed into the right chamber, and repeating this process constitutes one pass; quenching the sample after one extrusion, which constitutes one round of reciprocating extrusion; placing the sample after one round of extrusion into a heating furnace, adjusting the furnace temperature to lower the sample temperature by 5-20°C compared to the previous round, holding it at that temperature for 1 hour, and then continuing to extrude for another pass; thus completing 2-8 rounds of reciprocating extrusion.

[0014] Furthermore, the titanium alloy ingot sample needs to be heat-treated before being placed into the mold, with a heating temperature of 850℃-T. β (Refers to the transition from the α+β biphase region to the β phase), keep warm for 1-2 hours; heat the mold to 950±20℃ and keep warm before use.

[0015] Furthermore, the stepping rate of the hydraulic arm is 1-5 mm / s.

[0016] Furthermore, the vacuum aging treatment involves holding the temperature at 650-750℃ for 5-10 hours.

[0017] Compared with the prior art, the present invention has the following advantages and technical effects:

[0018] The Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si high-temperature titanium alloy prepared by this invention, containing micro / nano (TiZr)6Si3 and nano Ti3Al, is different from traditional solution-treated and aged near-α high-temperature titanium alloys. Its final microstructure is a dual-state microstructure, containing micro / nano dual-scale (TiZr)6Si3 particles and nanoscale Ti3Al particles.

[0019] This invention employs an extrusion method using alloying synergistic rapid deformation technology in the two-phase region to break the original casting structure within the billet, resulting in a more uniform internal structure and properties. Under high-temperature conditions, the precipitated phases within the alloy grains are more dispersed and the coarsening rate is slower, leading to a slower decline in mechanical properties and thus obtaining more stable performance, which is necessary to meet the needs of the rapid development of the aerospace industry. Attached Figure Description

[0020] The accompanying drawings, which form part of this application, are used to provide a further understanding of this application. The illustrative embodiments and descriptions of this application are used to explain this application and do not constitute an undue limitation of this application. In the drawings:

[0021] Figure 1 This is a schematic diagram of a temperature-controlled reciprocating extrusion die, where 1: right hydraulic arm; 2: heating resistance rod; 3: upper extrusion die; 4: extrusion chamber; 5: left hydraulic arm; 6: sample; 7: lower extrusion die;

[0022] Figure 2 Here is a SEM image of the as-cast state of Example 1;

[0023] Figure 3 BSE diagram of the extruded state in Example 1;

[0024] Figure 4 The images shown are TEM and SADP images after extrusion in Example 1.

[0025] Figure 5 The stress-strain diagrams for room temperature tensile engineering before and after extrusion in Example 1 are shown.

[0026] Figure 6 Here is a SEM image of the as-cast state of Example 2;

[0027] Figure 7 BSE diagram of the extruded state in Example 2;

[0028] Figure 8 The images shown are TEM and SADP images after extrusion in Example 2.

[0029] Figure 9 The stress-strain diagrams for room temperature tensile engineering before and after extrusion in Example 2 are shown.

[0030] Figure 10 Stress-strain diagrams for different samples after extrusion and tensile testing at 700℃. Detailed Implementation

[0031] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0032] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Every smaller range between any stated value or intermediate value within a stated range, and any other stated value or intermediate value within said range, is also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.

[0033] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.

[0034] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be obvious to those skilled in the art. This application specification and embodiments are merely exemplary.

[0035] The terms “include,” “including,” “have,” “contain,” etc., used in this article are all open-ended terms, meaning that they include but are not limited to.

[0036] Unless otherwise specified, "room temperature" in this invention refers to 25±2℃.

[0037] All raw materials used in the following embodiments of the present invention are commercially available.

[0038] Existing near-alpha titanium alloys exhibit low microstructural stability at high temperatures. If dynamic precipitation of silicides and α2 phases, along with synergistic control of the matrix microstructure, can be achieved through thermoplastic deformation, it is hoped that high-temperature strength can be improved without sacrificing microstructural stability. Therefore, this invention increases dislocation density through rapid deformation and optimizes the synergistic control of Zr and Al content to induce silicide and α2 phase precipitation. Simultaneously, to mitigate the adverse effects of continuous GBα phases and achieve a good balance between strength and plasticity in titanium alloys, this invention uses a matrix with a bimodal microstructure as the raw material. A bimodal microstructure is defined as the microstructure obtained through hot deformation using mechanical heat treatment in the two-phase region. This invention employs a bimodal microstructure with an equiaxed α phase volume fraction of 10-30%, which exhibits good matching of strength, plasticity, creep, and fatigue properties.

[0039] Reciprocating extrusion (CEC) is a novel grain refinement method. While belonging to the thermomechanical processing category, it differs from traditional methods. Combining extrusion and upsetting, it overcomes the drawbacks of traditional extrusion and rolling methods, such as pronounced fiber orientation and anisotropy within the material. It readily yields equiaxed grain structures while refining, dispersing, and uniformly distributing the grains. Furthermore, it induces the precipitation of dual-scale silicides in the matrix, significantly improving alloy properties. Following extrusion and subsequent aging heat treatment, nanoscale α2 precipitates can be formed in the α matrix.

[0040] This invention employs an extrusion method using alloying-assisted rapid deformation technology in the two-phase region to break down the original casting structure within the billet, resulting in a more uniform internal structure and properties. Under high-temperature conditions, the precipitated phases within the alloy grains are more dispersed and the coarsening rate is slower, leading to a slower decline in mechanical properties and thus a more stable performance, meeting the needs of the rapidly developing aerospace industry. In other words, this invention solves the current problem of the inability to simultaneously achieve high thermal strength and structural stability in near-α high-temperature titanium alloys, aiming to provide a high-temperature titanium alloy capable of operating at 700℃. The specific steps are: S1, preparing a Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si high-temperature titanium alloy ingot through vacuum induction magnetic levitation melting; S2, in T… s S3. Solution quenching at 20-50℃ above the (silicide dissolution temperature); S4. Passive cooling reciprocating extrusion at 10-50℃ below the (α+β) / β phase transformation point to obtain a near-α high-temperature titanium alloy with both high strength and toughness and structural stability; S5. Aging treatment at 650-750℃.

[0041] The technical solution adopted in this invention is: a method for controllable precipitation of nano-silicides and α2 phase in near-α high-temperature titanium alloys through reciprocating extrusion molding technology. The preparation method includes the following steps:

[0042] Step 1) Solution treatment and quenching of the original ingot: The cylindrical billet of Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si is subjected to solution treatment and quenching in a T... s Solution treatment at 20-50℃ above the dissolution temperature of silicide (TiZr)6Si3, holding for 1-2 hours, allows all Si to dissolve into the matrix. Subsequently, water cooling to room temperature improves the alloy's strength while controlling the precipitation and growth of silicides in the matrix.

[0043] Step 2) Passive cooling and reciprocating extrusion:

[0044] 1) Assemble the upper and lower mold halves, apply lubricant evenly inside the mold cavity, and install the mold onto the horizontal hydraulic press;

[0045] 2) Heat the titanium alloy cylindrical ingot to 850℃-T β (α+β / β transition temperature, " / " means "to", indicating the transition from the α+β bistate tissue region to the β transition temperature) Keep warm for 1-2 hours;

[0046] 3) Adjust the parameters of the horizontal extruder and the temperature-controlled reciprocating extrusion die device, and heat the extrusion die to 950±20℃ and keep it at that temperature;

[0047] 4) Place the heated titanium alloy cylindrical ingot into the right cavity of the cylindrical die channel and fix the position of the left hydraulic arm.

[0048] 5) Start the right hydraulic arm and control the hydraulic arm stepping speed to 1-5 mm / s. The right hydraulic arm applies pressure to the sample to make it pass through the necking channel. When the sample contacts the left arm, continue to squeeze to upset the sample in the left sample chamber. Stop squeezing when the sample is completely squeezed into the left chamber, and the right hydraulic arm retracts to the set length and stays still.

[0049] 6) The left hydraulic arm presses the sample back in the opposite direction of the above process, and stops pressing when the sample is completely squeezed into the right chamber. This process is repeated to complete one pass.

[0050] 7) The alloy in one extrusion pass is quenched to shorten the cooling time, thereby inhibiting the growth of micron and nano-sized silicides precipitated during the extrusion process, thus controlling the grain size and volume fraction of silicides; this constitutes one round of reciprocating extrusion.

[0051] 8) Place the sample after one extrusion pass into the heating furnace, adjust the furnace temperature to cool the sample by 5-20°C compared to the previous pass, hold for 1 hour, and then continue extruding for another pass. Repeat this process to complete 2-8 rounds of reciprocating extrusion.

[0052] Step 3) Aging heat treatment: In order to ensure the precipitation and orderly transformation of the nano-scale α2 phase without coarsening, thereby avoiding the reduction of the alloy's plasticity, the extruded specimens were subjected to vacuum aging treatment at 650-750℃ for 5-10 hours.

[0053] Testing revealed that the final microstructure after extrusion aging was a bimodal structure, with an equiaxed α phase volume fraction of 10-30%; the size of the precipitated phase (TiZr)6Si3 was 0.05-1 μm; and the size of the Ti3Al precipitated phase was 0.1-5 nm. The resulting high-temperature titanium alloy exhibited a tensile strength of 1100-1300 MPa, a yield strength of 1000-1200 MPa, and an elongation of not less than 8%. At 700℃, the tensile strength of the high-temperature titanium alloy was 500-700 MPa, and the yield strength was 400-600 MPa.

[0054] The vacuum induction levitation melting method for Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si cylindrical billets can be obtained using conventional methods in this field, and will not be elaborated further below.

[0055] The following embodiments are further illustrations of the technical solution of the present invention.

[0056] The solution temperature T of the Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si alloy β It is 980℃.

[0057] The raw material Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si used in the following embodiments of the present invention can be obtained by conventional vacuum induction levitation melting method in the art. The preparation method of this raw material is not the focus of the present invention and will not be described in detail.

[0058] Example 1

[0059] Step 1) Solution treatment and quenching of the original ingot: The obtained Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si cylindrical billet was solution treated by holding it at 1200℃ for 2 hours, and then water-cooled to room temperature.

[0060] Step 2) Passive cooling and reciprocating extrusion ( Figure 1 (Schematic diagram of a temperature-controlled reciprocating extrusion die):

[0061] 1) Assemble the upper and lower mold halves, apply lubricant evenly inside the mold cavity, and install the mold onto the horizontal hydraulic press;

[0062] 2) Heat the titanium alloy cylindrical ingot to 970℃ and hold for 1 hour;

[0063] 3) Adjust the pressure value of the horizontal extruder, set the stepping speed of the pressure arm to 2 mm / s, and heat the temperature-controlled reciprocating extrusion die to 970℃ and keep it at that temperature.

[0064] 4) Withdraw the right hydraulic arm, place the heated titanium alloy cylindrical ingot into the right cavity of the cylindrical die channel, and fix the position of the left hydraulic arm.

[0065] 5) Start the right hydraulic arm, so that the right hydraulic arm contacts the sample and applies pressure to squeeze the sample through the necking channel. When the sample contacts the left hydraulic arm, it is resisted and upset. Stop squeezing when the sample is completely squeezed into the left chamber, and the right hydraulic arm retracts to the set length and stays still.

[0066] 6) The left hydraulic arm presses the sample back in the opposite direction of the above process, and stops pressing when the sample is completely squeezed into the right chamber. This process is repeated to complete one pass.

[0067] 7) Quench the alloy after one extrusion (just enough to cool it down), and repeat this process for one round of extrusion.

[0068] 8) Withdraw the hydraulic arm, take out the extruded sample, put the sample into the heating furnace, adjust the temperature of the heating furnace and the reciprocating extrusion die to 965℃, keep it at the temperature for 1 hour, and then continue to extrude one more pass.

[0069] 9) Repeat this process, each time cooling the sample by 5°C and holding it at that temperature for 1 hour before extrusion;

[0070] 10) After each extrusion, the alloy sample is quenched to complete three rounds of reciprocating extrusion.

[0071] Step 3) Aging heat treatment: The extruded specimen is subjected to vacuum aging treatment at 700℃ and held for 5 hours.

[0072] Figure 2 Here is a SEM image of the as-cast state of Example 1; Figure 3 BSE diagram of the extruded state in Example 1; Figure 4 The images shown are TEM and SADP images after extrusion in Example 1. Figure 5 The stress-strain diagrams for room temperature tensile engineering before and after extrusion in Example 1 are shown. Figure 10 The stress-strain diagram is shown for the tensile test at 700℃ after extrusion in Example 1.

[0073] It can be seen that the final microstructure after extrusion aging is a bimodal microstructure, with an equiaxed α phase volume fraction of 25%; the size of the precipitated phase (TiZr)6Si3 is 0.68±0.08 μm; and the size of the Ti3Al precipitated phase is 0.42±0.03 nm. The prepared high-temperature titanium alloy has a tensile strength of 1219.8 MPa, a yield strength of 1140.2 MPa, and an elongation of 12.43% at room temperature. At 700℃, the tensile strength is 567.842 MPa, and the yield strength is 514.33 MPa.

[0074] Example 2

[0075] Step 1) Solution treatment and quenching of the original ingot: The cylindrical billet of Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si was kept at 1200℃ for 2 hours, and then water-cooled to room temperature.

[0076] Step 2) Passive cooling and reciprocating extrusion ( Figure 1 (Schematic diagram of a temperature-controlled reciprocating extrusion die):

[0077] 1) Assemble the upper and lower mold halves, apply lubricant evenly inside the mold cavity, and install the mold onto the horizontal hydraulic press;

[0078] 2) Heat the titanium alloy cylindrical ingot to 965℃ and hold for 1 hour;

[0079] 3) Adjust the pressure value of the horizontal extruder, set the stepping speed of the pressure arm to 2 mm / s, and heat the temperature-controlled reciprocating extrusion die to 965℃ and keep it at that temperature.

[0080] 4) Withdraw the right hydraulic arm, place the heated titanium alloy cylindrical ingot into the right cavity of the cylindrical die channel, and fix the position of the left hydraulic arm.

[0081] 5) Start the right hydraulic arm, so that the right hydraulic arm contacts the sample and applies pressure to squeeze the sample through the necking channel. When the sample contacts the left hydraulic arm, it is resisted and upset. Stop squeezing when the sample is completely squeezed into the left chamber, and the right hydraulic arm retracts to the set length and stays still.

[0082] 6) The left hydraulic arm presses the sample back in the opposite direction of the above process, and stops pressing when the sample is completely squeezed into the right chamber. This process is repeated to complete one pass.

[0083] 7) The alloy extruded in one pass is quenched, and this constitutes one round of reciprocating extrusion;

[0084] 8) Withdraw the hydraulic arm, take out the extruded sample, put the sample into the heating furnace, adjust the heating furnace and reciprocating extrusion temperature to 955℃, keep it at the temperature for 1 hour, and then continue to extrude one more pass.

[0085] 9) Repeat this process, each time cooling the sample by 10°C and holding it at that temperature for 1 hour before extrusion;

[0086] 10) After each extrusion, the alloy sample is quenched to complete three rounds of reciprocating extrusion.

[0087] Step 3) Aging heat treatment: The extruded specimen is subjected to vacuum aging treatment at 700℃ and held for 8 hours.

[0088] Figure 6 Here is a SEM image of the as-cast state of Example 2; Figure 7 BSE diagram of the extruded state in Example 2; Figure 8 The images shown are TEM and SADP images after extrusion in Example 2. Figure 9 The stress-strain diagrams for room temperature tensile engineering before and after extrusion in Example 2 are shown. Figure 10 The stress-strain diagram is shown for the tensile test at 700℃ after extrusion in Example 2.

[0089] It can be observed that the final microstructure after extrusion aging is a bimodal structure, with an equiaxed α phase volume fraction of 30%; the size of the precipitated phase (TiZr)6Si3 is 0.42±0.05 μm; and the size of the Ti3Al precipitated phase is 0.35±0.03 nm. The prepared high-temperature titanium alloy has a tensile strength of 1201.9 MPa, a yield strength of 1124.2 MPa, and an elongation of 8.12% at room temperature. At 700℃, the tensile strength is 546.87 MPa, and the yield strength is 492.05 MPa.

[0090] Comparative Example 1

[0091] Similar to Example 1, the difference is that step two) is different in that isothermal multi-directional forging is used, and two passes of isothermal die forging are performed at 930°C.

[0092] The results showed that the microstructure obtained after extrusion aging was equiaxed, with a tensile strength of 347.26 MPa and a yield strength of 299.73 MPa at 700℃. The low strength makes it unsuitable for service at 700℃.

[0093] Comparative Example 2

[0094] Same as Example 1, except that solution quenching was not performed in step one).

[0095] The results showed that the microstructure after extrusion aging remained a bimodal structure, but the amount of biscale silicides was significantly reduced. This was because no solution quenching treatment was performed before extrusion, and the Si was not fused into the matrix. The tensile strength at 700℃ was 396.26 MPa, and the yield strength was 349.52 MPa. The low strength makes it unsuitable for service at 700℃.

[0096] Application Example 1

[0097] To evaluate whether the material could serve at 700℃, tensile tests at 700℃ were conducted on Examples 1, 2, Comparative Example 1, and Comparative Example 2. The tensile stress-strain diagrams are shown below. Figure 10 .

[0098] from Figure 10 As can be seen, the high-temperature strength of Examples 1 and 2 is much higher than that of Comparative Examples 1 and 2, and the product prepared by the present invention has good service capability at 700°C.

[0099] The above are merely preferred embodiments of this application, but the scope of protection of this application is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in this application should be included within the scope of protection of this application. Therefore, the scope of protection of this application should be determined by the scope of the claims.

Claims

1. A method for preparing a near-α high-temperature titanium alloy reinforced with micro / nano particles to withstand 700℃, characterized in that, The microstructure of the near-α high-temperature titanium alloy reinforced with micro / nano particles that can withstand 700℃ is a bimodal structure, with an equiaxed α phase volume fraction of 10-30%, a precipitated phase (TiZr)6Si3 with a size of 0.05-1μm, and a precipitated phase Ti3Al with a size of 0.1-5nm. The 700℃-resistant micro / nano particle-reinforced near-α high-temperature titanium alloy is made from Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si high-temperature titanium alloy and formed using a reciprocating extrusion process, specifically including the following steps: The raw material Ti-7Al-2.5Sn-9Zr-1.5Mo-1.8Nb-1.8W-0.6Si is subjected to solution treatment and quenched to obtain a titanium alloy ingot; the solution treatment temperature is 10-50℃ above the (TiZr)6Si3 dissolution temperature, and the solution treatment time is 1-2h. The titanium alloy ingot is subjected to reciprocating extrusion. The reciprocating extrusion specifically includes the following steps: placing the titanium alloy ingot sample into the right chamber of a cylindrical die channel, fixing the position of the left hydraulic arm, starting the right hydraulic arm, stopping the extrusion when the sample is completely extruded into the left chamber, and retracting the right hydraulic arm to a set length and fixing it in place; then, the left hydraulic arm pushes the sample back in the opposite direction, stopping the extrusion when the sample is completely extruded into the right chamber. This reciprocating motion constitutes one pass; quenching the sample after one extrusion pass constitutes one round of reciprocating extrusion; placing the sample after one round of extrusion into a heating furnace, adjusting the furnace temperature to lower the sample temperature by 5-20°C compared to the previous round, holding it at that temperature for 1 hour, and then continuing with another pass; this process is repeated 2-8 times to complete the reciprocating extrusion. The titanium alloy ingot sample needs to be heated before being placed into the die at a temperature of 850°C-T. β Keep warm for 1-2 hours; heat the mold to 950±20℃ and keep warm before use; the stepping speed of the hydraulic arm is 1-5mm / s; The extruded sample was subjected to vacuum aging treatment to obtain a near-α high-temperature titanium alloy reinforced with micro-nano particles that can withstand 700℃; the vacuum aging treatment was carried out at 650-750℃ for 5-10 hours.