A gap-reinforced titanium-based composite material with room-temperature high plasticity and high-temperature high strength and a preparation method thereof

Abstract

The present application relates to a kind of room temperature strong plasticity and high temperature strength matching gap reinforced titanium matrix composite and its preparation method, belong to titanium matrix composite technical field.To solve the problem that the method for introducing gap element into titanium matrix composite is difficult to realize uniform distribution of gap element, first, gap element additive powder, reinforcing phase reactant powder and titanium alloy matrix powder are mixed ball milling to obtain raw material powder, the raw material powder is made into raw material bar by hot pressing sintering or hot isostatic pressing, and the raw material bar is made into gap element reinforced titanium matrix composite powder by plasma rotating electrode atomization powder preparation;Finally, the titanium matrix composite powder obtained is hot pressed sintering or hot isostatic pressing to obtain gap reinforced titanium matrix composite.The present application introduces gap element in situ in titanium matrix composite powder, realizes the accurate control of the content and distribution of gap element, and the obtained series of titanium matrix composite has good strength and plasticity matching at room temperature, and the high temperature strength is also greatly improved.

Description

Technical Field

[0001] This invention belongs to the field of titanium-based composite material technology, and particularly relates to a gap-reinforced titanium-based composite material with room temperature strength and high temperature strength matching, and its preparation method. Background Technology

[0002] Titanium-based composites, as an advanced class of structural materials, exhibit broad application prospects in aerospace, automotive manufacturing, medical devices, and energy fields due to their high specific strength, high specific stiffness, excellent high-temperature performance, and good corrosion resistance. Titanium-based composites mainly consist of high-performance reinforcing phases, such as ceramic particles and fibers, combined with a titanium alloy matrix. The introduction of reinforcing phases aims to improve the mechanical properties of the material, including strength, hardness, and wear resistance. While the introduction of reinforcing phases can improve the high-temperature strength of the material, it may also lead to a decrease in room-temperature plasticity. Balancing high-temperature strength and room-temperature plasticity is a challenging problem in the design of titanium-based composites.

[0003] Besides the reinforcing phase, interstitial elements in titanium-based composites also significantly affect the material's properties. Interstitial elements typically refer to atoms or ions that can fill the interstitial spaces within the crystal lattice of a metal or alloy. Appropriate amounts of interstitial elements can increase the resistance to dislocation movement by inducing lattice distortion, thereby improving the yield strength and tensile strength of the material. However, excessive amounts of interstitial elements can lead to excessive lattice distortion, increasing the difficulty of dislocation movement, reducing the toughness of the titanium-based composite, and making it more prone to fracture during plastic deformation. Therefore, rationally controlling the content and distribution of interstitial elements is crucial to the performance of titanium-based composites.

[0004] For reinforcing phases, micro / nano design can reduce plasticity loss and even increase material plasticity while ensuring strength improvement. However, the content and distribution of interstitial elements in alloys are often minute and difficult to control precisely; even small changes in content can have a significant impact on material properties. Therefore, strict process control is required to achieve precise control of interstitial elements.

[0005] Traditional methods for introducing interstitial elements into titanium alloys and titanium-based composites mostly involve decomposing oxides, nitrides, and carbides through melting, or dispersing them through ball milling and high-temperature sintering. However, titanium-based composites prepared by ball milling combined with high-temperature sintering often exhibit large-scale inhomogeneity and are prone to microstructural coarsening. This is particularly true in titanium-based composites containing nano-reinforcing phases, where the rapid growth of the reinforcing phase can lead to performance degradation, making it difficult to ensure the uniformity of large-sized components and to balance room-temperature strength and high-temperature strength. Furthermore, due to the strong atomic bonds between oxides, nitrides, and carbides, repeated melting or prolonged high-temperature sintering is often required to ensure complete decomposition and uniform diffusion. These stringent requirements place stringent demands on the preparation process of titanium-based composites, limiting their large-scale application and development. Summary of the Invention

[0006] To address the problem that existing methods for introducing interstitial elements into titanium matrix composites are difficult to achieve uniform distribution of interstitial elements, resulting in a mismatch between room temperature strength and plasticity and high temperature strength, and that the preparation methods are inefficient, this invention provides an interstitial reinforced titanium matrix composite material with room temperature strength and plasticity matching high temperature strength, and its preparation method.

[0007] The technical solution of the present invention:

[0008] A method for preparing a gap-reinforced titanium-based composite material with room-temperature high plasticity and high-temperature strength, comprising the following steps:

[0009] Step 1: Prepare the raw material powder:

[0010] Oxygen, nitrogen, or carbon elements are used as interstitial elements, and TiB, La2O3, or Y2O3 are used as reinforcing phases. The interstitial element additive powder, reinforcing phase reactant powder, and titanium alloy matrix powder are weighed according to the designed interstitial element content and reinforcing phase content. The interstitial element additive powder, reinforcing phase reactant powder, and titanium alloy matrix powder are mixed and ball-milled to obtain raw material powder.

[0011] Step 2: Preparation of interstitial element-reinforced titanium-based composite powder:

[0012] The raw material powder obtained by ball milling is hot-pressed and sintered or hot isostatically pressed to obtain raw material rods, which are then powdered by plasma rotating electrode atomization to obtain interstitial element reinforced titanium-based composite powder.

[0013] Step 3: Preparation of interstitial reinforced titanium-based composite materials:

[0014] The obtained interstitial element-reinforced titanium-based composite powder is subjected to hot pressing sintering or hot isostatic pressing to obtain interstitial-reinforced titanium-based composite materials.

[0015] Furthermore, the particle size of the interstitial element additive powder mentioned in step one is 50nm, 100nm, 1μm, 2μm, 3μm or 5μm. When the interstitial element is oxygen, the corresponding additive powder is TiO2 powder; when the interstitial element is nitrogen, the corresponding additive powder is TiN powder; and when the interstitial element is carbon, the corresponding additive powder is graphite powder.

[0016] The particle size of the reinforcing phase reactant powder mentioned in step one is 50nm, 100nm, 1μm, 2μm, 3μm or 5μm. When the reinforcing phase is TiB, the reinforcing phase reactant powder is TiB2, ZrB2 or BN powder. When the reinforcing phase is La2O3, the reinforcing phase reactant powder is La2O3 or LaB6 powder. When the reinforcing phase is Y2O3, the reinforcing phase reactant powder is Y2O3 powder.

[0017] The particle size distribution range of the titanium alloy matrix powder is 1-75μm, 1-53μm, 75-150μm, 53-180μm, 150-250μm, 1-150μm, 1-180μm or 1-250μm, and the titanium alloy matrix powder is Ti, TC4, TA15, Ti65, Ti60, Ti55 or TC11 powder.

[0018] Furthermore, the ball milling speed in step one is 100-400 r / min, the mass ratio of material to steel balls during ball milling is 1:1-7, the diameter of the steel balls is 6 mm or 10 mm, the ball milling time is 2-8 h, and the ball milling rotation mode is forward rotation, reverse rotation, or alternating forward and reverse rotation.

[0019] Furthermore, in step two, the hot pressing sintering involves placing the raw material powder obtained in step one into a mold for sintering at a temperature of 1200–1400°C, a pressure of 10–40 MPa, and a sintering time of 1.5–2.5 h; the hot isostatic pressing involves placing the raw material powder obtained in step one into a titanium sheath, at a temperature of 1200–1400°C, a pressure of 100–200 MPa, and a sintering time of 1.5–2.5 h.

[0020] Furthermore, the processing diameter of the raw material bar in step two is 25mm, 50mm, or 75mm.

[0021] Furthermore, in step two, the feed rate of the plasma rotating electrode atomization powder production is 0.5–3 mm / s, the arc current is 1500–3000 A, and the rod rotation speed is 10000–30000 r / min.

[0022] Furthermore, the particle size distribution range of the interstitial element-reinforced titanium-based composite powder obtained by atomization in step two is 1–75 μm, 1–53 μm, 75–150 μm, 53–180 μm, 150–250 μm, 1–150 μm, 1–180 μm, or 1–250 μm.

[0023] Furthermore, in step three, the hot pressing sintering involves placing the interstitial element-reinforced titanium-based composite powder obtained in step two into a mold for sintering at a temperature of 950–1100°C, a pressure of 20–80 MPa, and a sintering time of 1–10 h; the hot isostatic pressing involves placing the interstitial element-reinforced titanium-based composite powder obtained in step two into a titanium sheath, at a temperature of 900–1100°C, a pressure of 100–200 MPa, and a sintering time of 1–10 h.

[0024] The present invention provides a method for preparing interstitial reinforced titanium-based composite materials with room-temperature strength and high-temperature strength that are matched, wherein the interstitial element content is 0.01-1 wt% and the reinforcing phase content is 0.1-6 vol.%.

[0025] Furthermore, when the interstitial element is oxygen, the oxygen content is 0.15–0.25 wt%; when the interstitial element is nitrogen, the nitrogen content is 0.075–0.15 wt%; and when the interstitial element is carbon, the carbon content is 0.03–0.2 wt%.

[0026] The beneficial effects of this invention are:

[0027] This invention simplifies the preparation process of interstitial element-reinforced titanium-based composite materials and expands the process window by providing a method for in-situ introduction of interstitial elements into titanium-based composite powder. This method ensures that interstitial element atoms are uniformly dispersed within the powder. Combined with powder metallurgy processes, it enables precise control over the content and distribution of interstitial elements, effectively avoiding performance degradation caused by element segregation. This significantly improves the controllability and stability of the performance of titanium-based composite materials. The resulting series of titanium-based composite materials exhibit good strength-plasticity matching at room temperature and a significant improvement in high-temperature strength. Attached Figure Description

[0028] Figure 1 A micrograph of the titanium-based composite powder reinforced with oxygen as the interstitial element in Example 1;

[0029] Figure 2 Micrographs of cross-sectional microstructures of reinforced titanium-based composite powder with oxygen as the interstitial element in Examples 1-3, magnified at different magnifications;

[0030] Figure 3 This is an oxygen element scan image of the cross-sectional microstructure of the reinforced titanium-based composite powder with oxygen as the interstitial element in Example 1.

[0031] Figure 4 The image shows the microstructure of the titanium-based composite material with oxygen as the interstitial element in Example 3. The left image is a SEM image, and the right image is an IPF image.

[0032] Figure 5 The table shows a comparison of the room temperature properties of titanium-based composite materials with oxygen as the interstitial element in Examples 1-3.

[0033] Figure 6 The high-temperature performance comparison charts for titanium-based composite materials with oxygen as the interstitial element in Examples 1-3 are shown.

[0034] Figure 7 These are micrographs of the cross-sectional microstructure of the reinforced titanium-based composite powder with nitrogen as the interstitial element in Examples 4-5;

[0035] Figure 8 The image shows the microstructure of the titanium-based composite material with nitrogen as the interstitial element in Example 5. The left image is a SEM image, and the right image is an IPF image.

[0036] Figure 9 The table shows a comparison of the room temperature properties of titanium-based composite materials with nitrogen as the interstitial element in Examples 4-5.

[0037] Figure 10 The high-temperature performance comparison charts for titanium-based composite materials with nitrogen as the interstitial element in Examples 4-5 are shown.

[0038] Figure 11 The table shows a comparison of the room temperature properties of titanium-based composite materials with carbon as the interstitial element in Examples 6-7.

[0039] Figure 12 The image shows the metallographic structure of the titanium-based composite material containing O in Comparative Example 1. Detailed Implementation

[0040] The technical solution of the present invention will be further described below with reference to embodiments, but it is not limited thereto. Any modifications or equivalent substitutions to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention should be covered within the protection scope of the present invention. In the following embodiments, the process equipment or apparatus not specifically specified are all conventional equipment or apparatus in the art. Unless otherwise specified, the raw materials used in the embodiments of the present invention are all commercially available; unless otherwise specified, the technical means used in the embodiments of the present invention are all conventional means well known to those skilled in the art.

[0041] Example 1

[0042] This embodiment provides a titanium-based composite material with oxygen as the interstitial element and its preparation method.

[0043] In this embodiment, the interstitial element is oxygen, and the corresponding additive powder is TiO2 powder with a particle size of 50 nm. The reinforcing phase is TiB, and the reinforcing phase reactant powder is TiB2 powder with a particle size of 5 μm. The titanium alloy matrix is ​​TA15 powder with a particle size distribution range of 75-150 μm. In this embodiment, the volume fraction of the reinforcing phase TiB is designed to be 1 vol.%, and the mass fraction of the interstitial element O is 0.15 wt%, denoted as 1TiB+0.15O / TA15 or 1 vol.%TiB+0.15 wt%O+TA15.

[0044] The specific steps for preparing the titanium-based composite material with oxygen as the interstitial element in this embodiment are as follows:

[0045] Step 1: Prepare the raw material powder:

[0046] According to the designed interstitial element content and reinforcing phase content, weigh 3 kg of TA15 powder, 17.6470 g of TiB2 powder, and 7.5065 g of TiO2 powder. Place all the weighed powders into a ball mill jar, seal it, and purge it with high-purity argon gas. Then, ball milling is performed at a speed of 220 r / min. The mass ratio of material to steel balls is 1:5, the diameter of the steel balls is 10 mm, the ball milling time is 4 h, and the ball milling mode is forward rotation to obtain raw material powder.

[0047] Step 2: Preparation of interstitial element-reinforced titanium-based composite powder:

[0048] The raw material powder obtained from ball milling in step one was placed in a mold for hot pressing and sintering at a temperature of 1200℃, a pressure of 20MPa, and a sintering time of 2 hours to obtain cylindrical raw material rods. The oxide layer on the surface of the raw material rods was removed using a lathe, and the rods were machined to a fixed size to meet a diameter of 75mm. One end of the rod was machined to obtain a thread that mates with the powder maker. The machined raw material rods were cleaned and assembled onto a plasma rotating electrode atomizing powder maker. Once the atomization chamber was filled with high-purity argon gas, atomization powder production began. The feed rate was 1.1mm / s, the arc current was 2600A, and the rod rotation speed was 20000r / min. The resulting powder was first cleaned of impurities and then screened to obtain powder with a particle size distribution range of 75–150μm, resulting in interstitial element-reinforced titanium-based composite powder. Its surface morphology is as follows: Figure 1 As shown, the resulting interstitial element-reinforced titanium-based composite powder particles are mostly regular spherical in shape with smooth surfaces.

[0049] Step 3: Preparation of interstitial reinforced titanium-based composite materials:

[0050] The interstitial element-reinforced titanium-based composite powder obtained in step two was placed in a mold for hot pressing and sintering at a temperature of 1000℃, a pressure of 60MPa, and a sintering time of 6h. After removing the mold, the interstitial element-reinforced titanium-based composite material was obtained.

[0051] Example 2

[0052] This embodiment provides a titanium-based composite material with oxygen as the interstitial element and its preparation method.

[0053] In this embodiment, the interstitial element is oxygen, and the corresponding additive powder is TiO2 powder with a particle size of 50 nm. The reinforcing phase is TiB, and the reinforcing phase reactant powder is TiB2 powder with a particle size of 5 μm. The titanium alloy matrix is ​​TA15 powder with a particle size distribution range of 75-150 μm. In this embodiment, the volume fraction of the reinforcing phase TiB is designed to be 1 vol.%, and the mass fraction of the interstitial element O is 0.2 wt%, denoted as 1TiB+0.2O / TA15 or 1 vol.%TiB+0.20 wt%O+TA15.

[0054] The specific steps for preparing the titanium-based composite material with oxygen as the interstitial element in this embodiment are as follows:

[0055] Step 1: Prepare the raw material powder:

[0056] According to the designed interstitial element content and reinforcing phase content, weigh 3 kg of TA15 powder, 17.6470 g of TiB2 powder, and 11.2739 g of TiO2 powder. Place all the weighed powders into a ball mill jar, seal it, and purge it with high-purity argon gas. Then, ball milling is performed at a speed of 220 r / min. The mass ratio of material to steel balls is 1:5, the diameter of the steel balls is 10 mm, the ball milling time is 4 h, and the ball milling mode is forward rotation to obtain the raw material powder.

[0057] Step 2: Preparation of interstitial element-reinforced titanium-based composite powder:

[0058] The raw material powder obtained from ball milling in step one was placed in a mold for hot pressing and sintering at a temperature of 1200℃, a pressure of 20MPa, and a sintering time of 2 hours to obtain cylindrical raw material rods. The oxide layer on the surface of the raw material rods was removed using a lathe, and the rods were machined to a fixed size to meet a diameter of 75mm. One end of the rods was machined to obtain threads that would mate with the powder maker. The machined raw material rods were cleaned and assembled onto a plasma rotating electrode atomizing powder maker. Once the atomization chamber was filled with high-purity argon gas, atomization powder making began. The feed rate was 1.1mm / s, the arc current was 2600A, and the rod rotation speed was 20000r / min. The resulting powder was first cleaned of impurities and then screened to obtain powder with a particle size distribution range of 75–150μm, yielding interstitial element-reinforced titanium-based composite powder.

[0059] Step 3: Preparation of interstitial reinforced titanium-based composite materials:

[0060] The interstitial element-reinforced titanium-based composite powder obtained in step two was placed in a mold for hot pressing and sintering at a temperature of 1000℃, a pressure of 60MPa, and a sintering time of 6h. After removing the mold, the interstitial element-reinforced titanium-based composite material was obtained.

[0061] Example 3

[0062] This embodiment provides a titanium-based composite material with oxygen as the interstitial element and its preparation method.

[0063] In this embodiment, the interstitial element is oxygen, and the corresponding additive powder is TiO2 powder with a particle size of 50 nm. The reinforcing phase is TiB, and the reinforcing phase reactant powder is TiB2 powder with a particle size of 5 μm. The titanium alloy matrix is ​​TA15 powder with a particle size distribution range of 75-150 μm. In this embodiment, the volume fraction of the reinforcing phase TiB is designed to be 1 vol.%, and the mass fraction of the interstitial element O is 0.25 wt%, denoted as 1TiB+0.25O / TA15 or 1 vol.%TiB+0.25 wt%O+TA15.

[0064] The specific steps for preparing the titanium-based composite material with oxygen as the interstitial element in this embodiment are as follows:

[0065] Step 1: Prepare the raw material powder:

[0066] According to the designed interstitial element content and reinforcing phase content, weigh 3 kg of TA15 powder, 17.6470 g of TiB2 powder, and 15.0508 g of TiO2 powder. Place all the weighed powders into a ball mill jar, seal it, and purge it with high-purity argon gas. Then, ball milling is performed at a speed of 220 r / min. The mass ratio of material to steel ball during ball milling is 1:5. The diameter of the steel ball is 10 mm. The ball milling time is 4 h. The ball milling mode is forward rotation to obtain the raw material powder.

[0067] Step 2: Preparation of interstitial element-reinforced titanium-based composite powder:

[0068] The raw material powder obtained from ball milling in step one was placed in a mold for hot pressing and sintering at a temperature of 1200℃, a pressure of 20MPa, and a sintering time of 2 hours to obtain cylindrical raw material rods. The oxide layer on the surface of the raw material rods was removed using a lathe, and the rods were machined to a fixed size to meet a diameter of 75mm. One end of the rods was machined to obtain threads that would mate with the powder maker. The machined raw material rods were cleaned and assembled onto a plasma rotating electrode atomizing powder maker. Once the atomization chamber was filled with high-purity argon gas, atomization powder making began. The feed rate was 1.1mm / s, the arc current was 2600A, and the rod rotation speed was 20000r / min. The resulting powder was first cleaned of impurities and then screened to obtain powder with a particle size distribution range of 75–150μm, yielding interstitial element-reinforced titanium-based composite powder.

[0069] Step 3: Preparation of interstitial reinforced titanium-based composite materials:

[0070] The interstitial element-reinforced titanium-based composite powder obtained in step two was placed in a mold for hot pressing and sintering at a temperature of 1000℃, a pressure of 60MPa, and a sintering time of 6h. After removing the mold, the interstitial element-reinforced titanium-based composite material was obtained.

[0071] Figure 2These are magnified micrographs of the cross-sectional microstructure of the titanium-based composite powder reinforced with oxygen as the interstitial element in Examples 1-3, taken at different magnifications. Figure 2 It can be seen that the oxygen-reinforced titanium-based composite powder contains nano-sized TiB, which is beneficial to the strength and plasticity matching of the material. Its structure is uniform and free of defects, which is conducive to sintering and forming. Figure 3 This is an oxygen element scan image of the cross-sectional microstructure of the reinforced titanium-based composite powder with oxygen as the interstitial element in Example 1; from Figure 3 It can be seen that the oxygen element is evenly distributed in the powder.

[0072] Figure 4 The image shows the microstructure of the titanium-based composite material with oxygen as the interstitial element in Example 3. The left image is a SEM image, and the right image is an IPF image. Figure 4 It can be seen that the oxygen-reinforced titanium-based composite material obtained by sintering has a fine and uniform microstructure and no small defects, which is beneficial to the strengthening and plasticization of the material.

[0073] Figure 5 This is a comparison chart of the room temperature properties of titanium-based composite materials with oxygen as the interstitial element in Examples 1-3. Figure 5 It can be seen that oxygen-reinforced titanium-based composites have good room-temperature strength-plasticity matching.

[0074] The yield strength, ultimate strength, and elongation of titanium-based composite materials with oxygen as the interstitial element in Examples 1-3 are shown in Table 1.

[0075] Table 1

[0076] Test item Yield strength MPa Ultimate strength MPa Elongation % Example 1 973 1053 18.8 Example 2 1017 1098 17.1 Example 3 1049 1121 17.2

[0077] Figure 6 This is a comparison chart of the high-temperature performance of titanium-based composite materials with oxygen as the interstitial element in Examples 1-3; from Figure 6 It can be seen that oxygen-reinforced titanium-based composite materials have good high-temperature strength within the range of 600-700℃.

[0078] Example 4

[0079] This embodiment provides a titanium-based composite material with nitrogen as the interstitial element and its preparation method.

[0080] In this embodiment, the interstitial element is nitrogen, and the corresponding additive powder is TiN powder with a particle size of 1 μm. The reinforcing phase is TiB, and the reinforcing phase reactant powder is TiB2 powder with a particle size of 5 μm. The titanium alloy matrix is ​​TA15 powder with a particle size distribution range of 75-150 μm. In this embodiment, the volume fraction of the reinforcing phase TiB is designed to be 1 vol.%, and the mass fraction of the interstitial element N is 0.075 wt%, denoted as 1TiB+0.075N / TA15 or 1 vol.%TiB+0.075 wt%N+TA15.

[0081] The specific steps for preparing the titanium-based composite material with nitrogen as the interstitial element in this embodiment are as follows:

[0082] Step 1: Prepare the raw material powder:

[0083] According to the designed interstitial element content and reinforcing phase content, weigh 3 kg of TA15 powder, 17.6470 g of TiB2 powder, and 9.9765 g of TiN powder. Place all the weighed powders into a ball mill jar, seal it, and purge it with high-purity argon gas. Then, ball milling is performed at a speed of 220 r / min. The mass ratio of material to steel balls during ball milling is 1:5. The diameter of the steel balls is 10 mm. The ball milling time is 4 h. The ball milling mode is forward rotation to obtain the raw material powder.

[0084] Step 2: Preparation of interstitial element-reinforced titanium-based composite powder:

[0085] The raw material powder obtained from ball milling in step one was placed in a mold for hot pressing and sintering at a temperature of 1300℃, a pressure of 20MPa, and a sintering time of 2 hours to obtain cylindrical raw material rods. The oxide layer on the surface of the raw material rods was removed using a lathe, and the rods were machined to a fixed size to meet a diameter of 75mm. One end of the rods was machined to obtain threads that would mate with the powder maker. The machined raw material rods were cleaned and assembled onto a plasma rotating electrode atomizing powder maker. Once the atomization chamber was filled with high-purity argon gas, atomization powder making began. The feed rate was 1.1mm / s, the arc current was 2600A, and the rod rotation speed was 20000r / min. The resulting powder was first cleaned of impurities and then screened to obtain powder with a particle size distribution range of 75–150μm, yielding interstitial element-reinforced titanium-based composite powder.

[0086] Step 3: Preparation of interstitial reinforced titanium-based composite materials:

[0087] The interstitial element-reinforced titanium-based composite powder obtained in step two was placed in a mold for hot pressing and sintering at a temperature of 1000℃, a pressure of 60MPa, and a sintering time of 6h. After removing the mold, the interstitial element-reinforced titanium-based composite material was obtained.

[0088] Example 5

[0089] This embodiment provides a titanium-based composite material with nitrogen as the interstitial element and its preparation method.

[0090] In this embodiment, the interstitial element is nitrogen, and the corresponding additive powder is TiN powder with a particle size of 1 μm. The reinforcing phase is TiB, and the reinforcing phase reactant powder is TiB2 powder with a particle size of 5 μm. The titanium alloy matrix is ​​TA15 powder with a particle size distribution range of 75-150 μm. In this embodiment, the volume fraction of the reinforcing phase TiB is designed to be 1 vol.%, and the mass fraction of the interstitial element N is 0.15 wt%, denoted as 1TiB+0.15N / TA15 or 1 vol.%TiB+0.15 wt%N+TA15.

[0091] The specific steps for preparing the titanium-based composite material with nitrogen as the interstitial element in this embodiment are as follows:

[0092] Step 1: Prepare the raw material powder:

[0093] According to the designed interstitial element content and reinforcing phase content, weigh 3 kg of TA15 powder, 17.6470 g of TiB2 powder, and 20.0195 g of TiN powder. Place all the weighed powders into a ball mill jar, seal it, and purge it with high-purity argon gas. Then, ball milling is performed at a speed of 220 r / min. The mass ratio of material to steel balls during ball milling is 1:5. The diameter of the steel balls is 10 mm. The ball milling time is 4 h. The ball milling mode is forward rotation to obtain the raw material powder.

[0094] Step 2: Preparation of interstitial element-reinforced titanium-based composite powder:

[0095] The raw material powder obtained from ball milling in step one was placed in a mold for hot pressing and sintering at a temperature of 1300℃, a pressure of 20MPa, and a sintering time of 2 hours to obtain cylindrical raw material rods. The oxide layer on the surface of the raw material rods was removed using a lathe, and the rods were machined to a fixed size to meet a diameter of 75mm. One end of the rods was machined to obtain threads that would mate with the powder maker. The machined raw material rods were cleaned and assembled onto a plasma rotating electrode atomizing powder maker. Once the atomization chamber was filled with high-purity argon gas, atomization powder making began. The feed rate was 1.1mm / s, the arc current was 2600A, and the rod rotation speed was 20000r / min. The resulting powder was first cleaned of impurities and then screened to obtain powder with a particle size distribution range of 75–150μm, yielding interstitial element-reinforced titanium-based composite powder.

[0096] Step 3: Preparation of interstitial reinforced titanium-based composite materials:

[0097] The interstitial element-reinforced titanium-based composite powder obtained in step two was placed in a mold for hot pressing and sintering at a temperature of 1000℃, a pressure of 60MPa, and a sintering time of 6h. After removing the mold, the interstitial element-reinforced titanium-based composite material was obtained.

[0098] Figure 7Micrographs of the cross-sectional microstructure of the reinforced titanium-based composite powder with nitrogen as the interstitial element in Examples 4-5; from Figure 7 It can be seen that the nitrogen-reinforced titanium-based composite powder contains nano-sized TiB, which is beneficial to the strength and plasticity matching of the material. Its structure is uniform and free of defects, which is conducive to sintering and forming.

[0099] Figure 8 The image shows the microstructure of the titanium-based composite material with nitrogen as the interstitial element in Example 5. The left image is a SEM image, and the right image is an IPF image. Figure 8 It can be seen that the nitrogen-reinforced titanium-based composite material obtained by sintering has a fine and uniform microstructure and no small defects, which is beneficial to the strengthening and plasticization of the material.

[0100] Figure 9 This is a comparison chart of the room temperature properties of titanium-based composite materials with nitrogen as the interstitial element in Examples 4-5; from Figure 9 It can be seen that nitrogen-reinforced titanium-based composites have good room-temperature strength-plasticity matching.

[0101] The yield strength, ultimate strength, and elongation of the titanium-based composite materials with nitrogen as the interstitial element in Examples 4-5 are shown in Table 2.

[0102] Table 2

[0103] Test item Yield strength MPa Ultimate strength MPa Elongation % Example 4 967 1072 17.0 Example 5 1072 1133 5.1

[0104] Figure 10 This is a comparison chart of the high-temperature performance of titanium-based composite materials with nitrogen as the interstitial element in Examples 4-5; from Figure 10 It can be seen that nitrogen-reinforced titanium-based composite materials have good high-temperature strength within the range of 600-700℃.

[0105] Example 6

[0106] This embodiment provides a titanium-based composite material with carbon as the interstitial element and its preparation method.

[0107] In this embodiment, the interstitial element is carbon, and the corresponding additive powder is graphite powder with a particle size of 1 μm. The reinforcing phase is TiB, and the reinforcing phase reactant powder is TiB2 powder with a particle size of 5 μm. The titanium alloy matrix is ​​TC4 powder with a particle size distribution range of 75-150 μm. In this embodiment, the volume fraction of the reinforcing phase TiB is designed to be 1 vol.%, and the mass fraction of the interstitial element C is 0.2 wt%, denoted as 1 vol.% TiB + 0.2 wt% C + TC4.

[0108] The specific steps for preparing the titanium-based composite material with carbon as the interstitial element in this embodiment are as follows:

[0109] Step 1: Prepare the raw material powder:

[0110] According to the designed interstitial element content and reinforcing phase content, weigh 3 kg of TC4 powder, 17.6470 g of TiB2 powder, and 0.6 g of graphite powder. Place all the weighed powders into a ball mill jar, seal it, and purge it with high-purity argon gas. Then, ball milling is performed at a speed of 220 r / min. The mass ratio of material to steel ball during ball milling is 1:5, the diameter of the steel ball is 10 mm, the ball milling time is 4 h, and the ball milling mode is forward rotation to obtain raw material powder.

[0111] Step 2: Preparation of interstitial element-reinforced titanium-based composite powder:

[0112] The raw material powder obtained from ball milling in step one was placed in a mold for hot pressing and sintering at a temperature of 1300℃, a pressure of 20MPa, and a sintering time of 2 hours to obtain cylindrical raw material rods. The oxide layer on the surface of the raw material rods was removed using a lathe, and the rods were machined to a fixed size to meet a diameter of 75mm. One end of the rods was machined to obtain threads that would mate with the powder maker. The machined raw material rods were cleaned and assembled onto a plasma rotating electrode atomizing powder maker. Once the atomization chamber was filled with high-purity argon gas, atomization powder making began. The feed rate was 1.1mm / s, the arc current was 2600A, and the rod rotation speed was 20000r / min. The resulting powder was first cleaned of impurities and then screened to obtain powder with a particle size distribution range of 75–150μm, yielding interstitial element-reinforced titanium-based composite powder.

[0113] Step 3: Preparation of interstitial reinforced titanium-based composite materials:

[0114] The interstitial element-reinforced titanium-based composite powder obtained in step two was placed in a mold for hot pressing and sintering at a temperature of 1000℃, a pressure of 60MPa, and a sintering time of 6h. After removing the mold, the interstitial element-reinforced titanium-based composite material was obtained.

[0115] Example 7

[0116] This embodiment provides a titanium-based composite material with carbon as the interstitial element and its preparation method.

[0117] In this embodiment, the interstitial element is carbon, and the corresponding additive powder is graphite powder with a particle size of 1 μm. The reinforcing phase is TiB, and the reinforcing phase reactant powder is TiB2 powder with a particle size of 5 μm. The titanium alloy matrix is ​​TC4 powder with a particle size distribution range of 75-150 μm. In this embodiment, the volume fraction of the reinforcing phase TiB is designed to be 0.5 vol.%, and the mass fraction of the interstitial element C is 0.03 wt%, denoted as 0.5 vol.% TiB + 0.03 wt% C + TC4.

[0118] The specific steps for preparing the titanium-based composite material with carbon as the interstitial element in this embodiment are as follows:

[0119] Step 1: Prepare the raw material powder:

[0120] According to the designed interstitial element content and reinforcing phase content, weigh 3 kg of TC4 powder, 8.8235 g of TiB2 powder, and 0.09 g of graphite powder. Place all the weighed powders into a ball mill jar, seal it, and purge it with high-purity argon gas. Then, ball milling is performed at a speed of 220 r / min. The mass ratio of material to steel ball during ball milling is 1:5. The diameter of the steel ball is 10 mm. The ball milling time is 4 h. The ball milling mode is forward rotation to obtain the raw material powder.

[0121] Step 2: Preparation of interstitial element-reinforced titanium-based composite powder:

[0122] The raw material powder obtained from ball milling in step one was placed in a mold for hot pressing and sintering at a temperature of 1300℃, a pressure of 20MPa, and a sintering time of 2 hours to obtain cylindrical raw material rods. The oxide layer on the surface of the raw material rods was removed using a lathe, and the rods were machined to a fixed size to meet a diameter of 75mm. One end of the rods was machined to obtain threads that would mate with the powder maker. The machined raw material rods were cleaned and assembled onto a plasma rotating electrode atomizing powder maker. Once the atomization chamber was filled with high-purity argon gas, atomization powder making began. The feed rate was 1.1mm / s, the arc current was 2600A, and the rod rotation speed was 20000r / min. The resulting powder was first cleaned of impurities and then screened to obtain powder with a particle size distribution range of 75–150μm, yielding interstitial element-reinforced titanium-based composite powder.

[0123] Step 3: Preparation of interstitial reinforced titanium-based composite materials:

[0124] The interstitial element-reinforced titanium-based composite powder obtained in step two was placed in a mold for hot pressing and sintering at a temperature of 1000℃, a pressure of 60MPa, and a sintering time of 6h. After removing the mold, the interstitial element-reinforced titanium-based composite material was obtained.

[0125] Figure 11 This is a comparison chart of the room temperature properties of titanium-based composite materials with carbon as the interstitial element in Examples 6-7; from Figure 11 It can be seen that carbon-reinforced titanium-based composites have good room-temperature strength-plasticity matching.

[0126] The yield strength, ultimate strength, and elongation of the titanium-based composite materials with carbon as the interstitial element in Examples 6-7 are shown in Table 3.

[0127] Table 3

[0128] Test item Yield strength MPa Ultimate strength MPa Elongation % Example 6 966 1103 6.6 Example 7 954 1058 19.9

[0129] Comparative Example 1

[0130] This comparative example provides a method for preparing O-containing titanium-based composite materials using ball milling and high-temperature sintering, as detailed below:

[0131] Step 1, ball milling:

[0132] Weigh out 3 kg of TA15 powder with a particle size distribution range of 75-150 μm, 17.6470 g of TiB2 powder with a particle size of 5 μm, and 7.5065 g of TiO2 powder with a particle size of 50 nm. Place all the weighed powders into a ball mill jar, seal it, and purge it with high-purity argon gas. Then, ball milling is performed at a speed of 220 r / min, a material-to-steel ball mass ratio of 1:5, a steel ball diameter of 10 mm, a milling time of 4 h, and a forward rotation of the ball mill to obtain the raw material powder.

[0133] Step 2: Hot pressing and sintering:

[0134] The raw material powder obtained from ball milling in step one was placed in a mold for hot pressing and sintering. The sintering temperature was 1000℃, the pressure was 60MPa, and the sintering time was 6h. After removing the mold, the titanium-based composite material containing O was obtained.

[0135] Figure 12 Here are metallographic micrographs of the O-containing titanium-based composite material prepared in this comparative example, such as... Figure 12 As shown, there is a large area of ​​inhomogeneous structure in the metallographic structure.

Claims

1. A method for preparing a gap-reinforced titanium-based composite material with room-temperature high plasticity and high-temperature strength, characterized in that, Includes the following steps: Step 1: Prepare the raw material powder: Oxygen, nitrogen, or carbon are used as interstitial elements. When oxygen is used as the interstitial element, the corresponding additive powder is TiO2 powder with a particle size of 50 nm. When nitrogen is used as the interstitial element, the corresponding additive powder is TiN powder with a particle size of 1 μm. When carbon is used as the interstitial element, the corresponding additive powder is graphite powder with a particle size of 1 μm. TiB is used as the reinforcing phase, and the reinforcing phase reactant powder is TiB2 powder with a particle size of 5 μm. The titanium alloy matrix powder is TC4 powder or TA15 powder with a particle size of 75~150 μm. Weigh the interstitial element additive powder, reinforcing phase reactant powder, and titanium alloy matrix powder according to the designed interstitial element content and reinforcing phase content. Mix the interstitial element additive powder, reinforcing phase reactant powder, and titanium alloy matrix powder and ball mill them to obtain the raw material powder. Step 2: Preparation of interstitial element-reinforced titanium-based composite powder: The raw material powder obtained by ball milling is hot-pressed and sintered or hot isostatically pressed to obtain raw material rods, which are then powdered by plasma rotating electrode atomization to obtain interstitial element reinforced titanium-based composite powder with a particle size distribution range of 75~150μm. Step 3: Preparation of interstitial reinforced titanium-based composite materials: The obtained interstitial element-reinforced titanium-based composite powder is subjected to hot pressing sintering or hot isostatic pressing to obtain interstitial-reinforced titanium-based composite material with an interstitial element content of 0.01~1wt% and a reinforcing phase content of 0.1~6vol.%.

2. The method for preparing a gap-reinforced titanium-based composite material with room-temperature high plasticity and high-temperature strength matching as described in claim 1, characterized in that, The ball mill speed in step one is 100~400 r / min, the mass ratio of material to steel balls during ball milling is 1:1~7, the diameter of the steel balls is 6mm or 10mm, the ball milling time is 2~8h, and the ball mill rotation mode is forward rotation, reverse rotation or alternating forward and reverse rotation.

3. The method for preparing a gap-reinforced titanium-based composite material with room-temperature high plasticity and high-temperature strength matching as described in claim 2, characterized in that, Step two, hot pressing sintering, involves placing the raw material powder obtained in step one into a mold for sintering at a temperature of 1200~1400 ℃, a pressure of 10~40MPa, and a sintering time of 1.5~2.5h. Step two, hot isostatic pressing, involves placing the raw material powder obtained in step one into a titanium sheath, at a temperature of 1200~1400 ℃, a pressure of 100~200MPa, and a sintering time of 1.5~2.5h.

4. The method for preparing a gap-reinforced titanium-based composite material with room-temperature high plasticity and high-temperature strength matching as described in claim 3, characterized in that, The processing diameter of the raw material bar in step two is 25mm, 50mm or 75mm.

5. The method for preparing a gap-reinforced titanium-based composite material with room-temperature high plasticity and high-temperature strength matching according to claim 4, characterized in that, In step two, the feed rate of the plasma rotating electrode atomization powder production is 0.5~3mm / s, the arc current is 1500~3000A, and the rod rotation speed is 10000~30000r / min.

6. The method for preparing a gap-reinforced titanium-based composite material with room-temperature high plasticity and high-temperature strength matching according to claim 5, characterized in that, Step 3, hot pressing sintering, involves placing the interstitial element-reinforced titanium-based composite powder obtained in step 2 into a mold for sintering at a temperature of 950~1100 ℃, a pressure of 20~80 MPa, and a sintering time of 1~10 h. Step 3, hot isostatic pressing, involves placing the interstitial element-reinforced titanium-based composite powder obtained in step 2 into a titanium sheath, at a temperature of 900~1100 ℃, a pressure of 100~200 MPa, and a sintering time of 1~10 h.

7. A gap-reinforced titanium-based composite material prepared by the preparation method according to any one of claims 1-6, characterized in that, The interstitial element content is 0.01~1wt%, and the reinforcing phase content is 0.1~6vol.%.

8. The interstitial reinforced titanium-based composite material with room-temperature high plasticity and high-temperature strength matching according to claim 7, characterized in that, When the interstitial element is oxygen, the oxygen content is 0.15~0.25wt%; when the interstitial element is nitrogen, the nitrogen content is 0.075~0.15wt%; when the interstitial element is carbon, the carbon content is 0.03~0.2wt%.

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