Preparation method of bimodal titanium-based composite material with non-uniform net structure
A multi-scale non-uniform network structure titanium-based composite material was prepared by high-energy ball milling, field-assisted sintering and hot rolling processes, which solved the problem of strength-ductility trade-off in high-temperature titanium alloys and achieved a combination of high strength and high ductility.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-04
- Publication Date
- 2026-03-13
AI Technical Summary
Existing technologies struggle to effectively address the strength-ductility trade-off in high-temperature titanium alloys, especially when manufacturing dual-modal non-uniform network titanium matrix composites, where impurities and excessively large reinforcing phase sizes can easily be introduced, leading to reduced ductility.
By employing high-energy ball milling combined with field-assisted sintering technology and hot rolling deformation process, a (TiB2+LaB6+Si) reinforced Ti60 matrix composite material with ultrafine-scale αp and β phase matrix and micron-sized TiBw and nano-sized La2O3p reinforcements was prepared. The ceramic particles were refined by BGBM technology, and combined with rapid hot pressing sintering and hot rolling treatment, a multi-scale non-uniform network structure was formed.
The tensile properties and strength-ductility matching of the composite material were improved, with the ultimate tensile strength reaching 1544-1560 MPa and the elongation after fracture reaching 7.7-10.2%, thus realizing the preparation of high-performance titanium-based composite materials.
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Abstract
Description
Technical Field
[0001] This invention relates to a method for preparing a dual-modal non-uniform network structure titanium-based composite material, specifically a method for preparing (TiB2+LaB6+Si) reinforced Ti60-based composite material using high-energy ball milling combined with field-assisted sintering technology and hot rolling deformation, belonging to the field of metal matrix composite material preparation technology. Background Technology
[0002] With the rapid development of high-precision technologies such as aviation and aerospace, there are extremely high requirements for the weight of structural materials and their comprehensive mechanical properties under extreme service environments. High-temperature titanium alloys are considered promising candidates due to their excellent specific strength and thermal stability. However, the maximum service temperature of high-temperature titanium alloys is approaching their service limit, and traditional methods, such as changing the types and contents of alloying elements and heat treatment processes to alter the microstructure of the material, are no longer sufficient to further improve their performance. Discontinuous reinforced titanium matrix composites (DRTiMCs) have attracted widespread attention due to their large range of tunable composition and designable interface structure, and have been proven to be an effective method to improve strength at both room temperature and high temperatures. Unfortunately, this inevitably leads to a deterioration in room temperature ductility, i.e., the strength-ductility trade-off dilemma. In recent years, microstructured DRTiMCs have shown significant advantages in breaking through the performance bottleneck of titanium materials and have become a research focus. According to reports, gradient structures, layered structures, brick structures, multi-peak structures, and network structures can achieve further enhancements in whisker load transfer and strain hardening effects through special mechanisms such as efficient dislocation storage and dislocation distribution control, thereby realizing excellent strength and plasticity (toughness) combination of ceramic phase reinforced high-temperature titanium alloy composites.
[0003] While nano-designed or bio-inspired structurally designed DRTiMCs exhibit a good balance between strength and ductility, fabricating these composites remains a significant challenge. First, the ball milling process easily introduces O, Fe, and other uncontrollable impurity elements, leading to localized agglomeration of ceramic particles. Second, the large unit cell size and excessively high sintering temperature inevitably increase the size of the matrix structure and reinforcing phase, severely reducing ductility. For DRTiMCs with a bimodal non-uniform network structure, the limitations of previous surface modification methods are effectively overcome. An optimized ball milling process using built-in groove ball milling (BGBM) technology successfully refines the micron-sized ceramic particles within the composite powder to the nanoscale. Combined with rapid hot pressing sintering, micro / nano TiB... w and nano La2O 3p Introduced into titanium alloys, this lays the theoretical and technical foundation for breaking through the performance limits of DRTiMCs, and also provides important reference for the design and application of other advanced alloys and composite materials. Summary of the Invention
[0004] Therefore, the purpose of this invention is to provide a method for preparing a dual-modal non-uniform network structure titanium-based composite material, wherein the matrix microstructure of the DRTiMCs prepared by the method is an ultrafine α-structure. p The interface structure between the reinforcement and the matrix is TiB, consisting of β phase and silicide. w and La2O 3p This improves the tensile properties of the (TiB2+LaB6+Si) reinforced Ti60-based composite material.
[0005] The technical solution of this invention is:
[0006] A dual-modal non-uniform mesh structure titanium-based composite material, the titanium-based composite material comprising a matrix and a reinforcement;
[0007] The matrix is a Ti60 titanium alloy with an ultrafine α-structure. p β phase and silicide;
[0008] The reinforcing agents are TiB2, LaB6, and Si;
[0009] The interface structure between the reinforcement and the matrix is micron-sized TiB. w Nano TiB w Nano-La2O3 and nano-silicides form a bimodal non-uniform network structure with the matrix.
[0010] A method for preparing a dual-modal non-uniform mesh structure titanium-based composite material, comprising the following steps:
[0011] (1) TiB2, LaB6, Si and Ti60 titanium alloy powders were ball-milled and mixed, then the ball milling media were removed and dried to obtain composite powder;
[0012] With the total mass of TiB2, LaB6, Si, and Ti60 titanium alloy powders as 100%, the mass fraction of TiB2 is 0.05%–1.00%, the mass fraction of LaB6 is 0.20%–0.50%, the mass fraction of Si is 0.01%–0.05%, and the mass fraction of Ti60 titanium alloy powder is 98.0%–99.70%.
[0013] Preferably, the average particle size of the Ti60 titanium alloy powder is 0–15 μm and 25–60 μm;
[0014] Preferably, the average particle size of TiB2 is 1–3 μm, the average particle size of LaB6 is 1–2 μm, and the average particle size of Si is 30–60 nm.
[0015] Preferably, the ball milling parameters are as follows: the ball milling medium is anhydrous ethanol, and when the powder mass is 20-80g, the volume of anhydrous ethanol used is 150-300mL; the rotation speed is 250-350r / min, the time is 2-8h, the ball-to-material ratio is 8:1, and the grinding balls are composed of two sizes of agate balls, namely large-sized agate balls and small-sized agate balls. The diameter of the large-sized agate balls is 8-10mm, the diameter of the small-sized agate balls is 2-5mm, and the mass ratio of the large-sized agate balls to the small-sized agate balls is 5:1.
[0016] Preferably, rotary evaporation drying is used, the process of which is as follows: the mixed slurry is placed in a 500mL eggplant-shaped flask and vacuum dried at 75-85℃ for 15min to allow the anhydrous ethanol to evaporate completely, thereby obtaining a dry composite powder.
[0017] (2) The composite powder is sintered, cooled, polished, cleaned and dried using field-assisted sintering technology. The sintering parameters are: vacuum degree <15Pa, heating rate 80~150℃ / min, sintering temperature 1000~1200℃, sintering pressure 30~50MPa, and holding time 10~15min. After sintering, the powder is cooled, polished, cleaned and dried to obtain a preform with a thickness of 10~15mm.
[0018] Preferably, the vacuum degree is <15Pa, the heating rate is 80-150℃ / min, the sintering temperature is 1000-1200℃, the sintering pressure is 30-50MPa, and the holding time is 10-15min;
[0019] (3) The preformed billet was hot-rolled using a twin-roll mill to obtain the (TiB2+LaB6+Si) / Ti60 composite material. The specific hot-rolling deformation steps are as follows:
[0020] The preformed blank from step (2) is placed in an electric resistance furnace and held at 900-950°C for 10-15 minutes. Immediately afterward, it undergoes 3-6 passes of hot rolling with a deformation of 60%-70%. The blank is then held in the furnace for 1-2 minutes between passes. The hot-rolled sample is then placed in air to cool to room temperature, which is the (TiB2+LaB6+Si) / Ti60 composite material.
[0021] Beneficial effects:
[0022] (1) This invention provides a method for preparing a dual-modal non-uniform network structure titanium-based composite material. The method utilizes TiB2, LaB6, and Si powders and Ti60 alloy powder as raw materials, and employs high-energy ball milling, field-assisted sintering, and hot rolling processes to obtain micron-sized TiB2 with a special structure (dual-modal non-uniform network). w Nano TiB w and La2O3p Reinforced titanium-based composite materials. The matrix structure of the (TiB2+LaB6+Si) reinforced titanium-based composite material is ultrafine-scale α-structure. p β phase and nano-silicides, the interface structure between the reinforcement and the matrix is micron-sized TiB. w Nano TiB w and La2O 3p This improves the tensile properties of the DRTiMCs. In the dual-modal non-uniform network structure titanium-based composite material, micron-sized TiB... w Pinned at the grain boundaries of the matrix, some nano-TiB w The presence of DRTiMCs within the grains, along with spherical nano-La2O3, acts on the titanium alloy matrix to form a dual-mode non-uniform network with different scales, effectively improving the interfacial bonding strength.
[0023] (2) This invention provides a method for preparing a dual-modal non-uniform network structure titanium-based composite material, which consists of three stages. First, the reinforcing particles are effectively crushed by BGBM high-energy ball milling to achieve uniform dispersion with titanium alloy powder. Then, the composite powder is subjected to low-pressure high-temperature sintering using a field-assisted sintering process, realizing the preparation of a preformed billet in a short time, providing effective support for subsequent hot rolling. Finally, the preformed billet is hot-rolled to effectively refine the microstructure of DRTiMCs and generate micron-sized TiB in situ with the titanium alloy matrix. w Nano TiB w and La2O 3p In the aforementioned DRTiMCs, TiB2, LaB6, and Si powders react with the titanium alloy matrix to form a bimodal non-uniform network structure. The formation of precipitated phases significantly refines the matrix microstructure, strengthening the matrix through grain refinement and load transfer mechanisms, thereby increasing the strength of the DRTiMCs. When applied stress is transferred to the interface, it is distributed in a multidimensional space, which effectively alleviates local stress concentration and improves the stability of the interface structure.
[0024] (3) This invention provides a method for preparing a dual-modal non-uniform network structure titanium-based composite material. Compared with reported structurally reinforced titanium-based composite materials, this invention introduces three types of reinforcing particles at once for the first time, and achieves uniform dispersion of the composite powder through BGBM technology. The preparation process is short, the preparation efficiency is high, and the production cost is low, which is beneficial for industrial production applications. Moreover, the prepared DRTiMCs have excellent strength-plasticity matching, with an ultimate tensile strength of 1544 MPa and an elongation after fracture of 7.7%. The room temperature ultimate tensile strength of the hot-rolled (TiB2+LaB6+Si) / Ti60 composite material is 1560 MPa, and the elongation after fracture is 10.2%.
[0025] (4) This invention relates to a method for preparing a dual-modal non-uniform network structure titanium-based composite material, belonging to the field of metal matrix composite material preparation technology. Field-assisted sintering provides a new approach for preparing high-performance DRTiMCs. Attached Figure Description
[0026] Figure 1 SEM images and particle size distribution of Ti60 alloy powder and composite powder prepared in step (1) of this embodiment of the invention;
[0027] Figure 2 SEM image of the (TiB2+LaB6+Si) / Ti60 composite material prepared in step (2) of this embodiment of the invention;
[0028] Figure 3 TEM image of the (TiB2+LaB6+Si) / Ti60 composite material prepared in step (2) of this embodiment of the invention;
[0029] Figure 4 The IPF and grain size distribution of the (TiB2+LaB6+Si) / Ti60 composite material prepared in step (2) of this embodiment are shown in the figure.
[0030] Figure 5 Nanoindentation cloud map of the (TiB2+LaB6+Si) / Ti60 composite material prepared in step (2) of this embodiment of the invention;
[0031] Figure 6 The tensile curve of the (TiB2+LaB6+Si) / Ti60 composite material prepared in step (2) of this embodiment of the invention;
[0032] Figure 7 The tensile fracture morphology of the (TiB2+LaB6+Si) / Ti60 composite material prepared in step (2) of this embodiment is shown.
[0033] Figure 8 SEM image of the (TiB2+LaB6+Si) / Ti60 composite material prepared in step (3) of this embodiment of the invention;
[0034] Figure 9 The tensile curve of the (TiB2+LaB6+Si) / Ti60 composite material prepared in step (3) of the present invention;
[0035] Figure 10 The tensile fracture morphology of the (TiB2+LaB6+Si) / Ti60 composite material prepared in step (3) of the present invention is shown in the figure. Detailed Implementation
[0036] To make the objectives and technical solutions of this invention clearer, the technical solutions of this invention will be fully described below with reference to specific examples. It should be noted that these examples are only a part of the embodiments of this invention. Other examples obtained by those skilled in the art based on the embodiments of this invention without creative effort are all within the protection scope of this invention. It should be noted that, unless otherwise specified, the experimental methods described in the following embodiments are conventional methods, and the reagents and materials, unless otherwise specified, can be obtained commercially.
[0037] A method for preparing a dual-modal non-uniform mesh structure titanium-based composite material, the specific steps of which are as follows:
[0038] (1) TiB2, LaB6, Si and Ti60 titanium alloy powders were ball-milled and mixed, then the ball milling media were removed and dried to obtain composite powder.
[0039] (2) The composite powder is sintered, cooled, polished, cleaned and dried using field-assisted sintering technology. After sintering, it is cooled, polished, cleaned and dried to obtain a preform with a thickness of 10-15 mm.
[0040] (3) The preformed billet was hot-rolled and deformed using a twin-roll mill to obtain the (TiB2+LaB6+Si) / Ti60 composite material.
[0041] The total mass of TiB2, LaB6, and Si is 0.30%–2.0%, the mass fraction of LaB6 is 0.20%–0.50%, the mass fraction of Si is 0.01%–0.05%, and the mass fraction of Ti60 titanium alloy powder is 98.0%–99.70%. The average particle size of Ti60 titanium alloy powder is 0–15 μm and 25–60 μm; the average particle size of TiB2 is 1–3 μm, the average particle size of LaB6 is 1–2 μm, and the average particle size of Si is 30–60 nm. The ball milling media are used. The volume of anhydrous ethanol was 150–300 mL; the rotation speed was 250–350 r / min; the time was 2–8 h; and the ball-to-powder ratio was 8:1. The grinding balls consisted of two sizes of agate balls: a large agate ball and a small agate ball. The diameter of the large agate ball was 8–10 mm, and the diameter of the small agate ball was 2–5 mm. The mass ratio of the large agate ball to the small agate ball was 5:1. The mixture was vacuum dried at 75–85 °C for 15 min to allow the anhydrous ethanol to evaporate completely, resulting in a dry composite powder.
[0042] The sintering parameters are: vacuum degree <15Pa, heating rate 80~150℃ / min, sintering temperature 1000~1200℃, sintering pressure 30~50MPa, and holding time 10~15min.
[0043] The thickness is 10-15 mm, the rolling temperature is 900-950℃, the rolling deformation is 60%-70%, the first pass holding time is 10-15 min, the inter-pass holding time is 1-2 min, and the process is completed in 3-6 passes.
[0044] In the following embodiments:
[0045] The Ti60 powder was purchased from GREE (Beijing) New Materials Technology Co., Ltd., and had an average particle size of 44 μm.
[0046] The TiB2 and LaB6 were purchased from Shanghai Chaoqin New Materials Technology Co., Ltd., and the Si powder was purchased from Xianfeng Nanomaterials Co., Ltd., with purities of 99.1%, 99.5%, and 98.8%, respectively, and average particle sizes of 1–3 μm, 1–2 μm, and 30–60 nm, respectively.
[0047] The field-assisted sintering furnace system is model FHP-828 and was purchased from Suzhou Hateng Technology Co., Ltd.
[0048] The twin-roll mill, model LG-02, was purchased from Zhengzhou Hengzhong Heavy Industry Machinery Manufacturing Co., Ltd.
[0049] The DRTiMCs prepared in each embodiment were tested as follows:
[0050] (1) Tensile testing equipment: A universal tensile tester (AGS-X, Zhongji, China) was used and equipped with a laser X tens laser extensometer.
[0051] (2) SEM test: The scanning electron microscope (SEM) instrument model is FSEM, Hitachi S-4800N, (Japan).
[0052] (3) TEM test: The instrument model of the transmission electron microscope (TEM) is TEM,FEI Tecnai G2 F20 (USA).
[0053] (4) EBSD test: The instrument model for grain size statistics (EBSD) is MIRA3. The high-energy ball mill uses a self-developed ball milling jar (with built-in groove) (see utility model patent application number 202420463951.1).
[0054] (5) Nanoindentation test: Nanoindenter (Imicro, KLA, USA), maximum load set to 30 mN, loading rate to 0.5 nm / s, nanoindentation area to 150 × 150 μm 2 (225 indentations).
[0055] Example
[0056] (1) Weigh 30g of Ti60 titanium alloy powder with an average particle size of 44μm and 0.15g of TiB2, 0.09g of LaB6 and 0.006g of Si powder and mix them in a ball mill. The ball milling medium is 150ML of anhydrous ethanol, the ball-to-material ratio is 8:1, the ball mill speed is 300r / min, and the ball milling time is 8h. After removing the grinding balls, the slurry after ball milling is placed in a 500ML eggplant-shaped flask for vacuum rotary evaporation treatment. The temperature of the water bath is 75℃. After rotary drying, the composite powder is obtained.
[0057] (2) Place 20g of composite powder in a graphite mold with a diameter of 25mm, and sinter the composite powder into a block using a field-assisted sintering system. The specific sintering parameters are: heating rate 100℃ / s, sintering temperature 1200℃, holding time 8min, sintering pressure 50MPa, and cooling rate 100℃ / s. After sintering, remove the powder and air cool it to room temperature.
[0058] (3) Grind and clean the block obtained in step (2) to remove surface defects. Hold it in a resistance furnace at 900℃ for 12 minutes after preheating. Immediately remove it for rolling. Roll it for 5 passes with a deformation of 70%. Hold it in the furnace for 2 minutes between passes. After the last pass is completed, air cool it to room temperature. This is the (TiB2+LaB6+Si) / Ti60 composite material.
[0059] The composite powder and the prepared (TiB2+LaB6+Si) / Ti60 composite material in this embodiment were subjected to corresponding tests, and the results are as follows:
[0060] (1) The TiB2, LaB6, Si and Ti60 titanium alloy composite powder was observed using field emission scanning electron microscopy. The test results are shown in the figure. Figure 1 The Ti60 titanium alloy spheres did not show obvious deformation or breakage, and TiB2, LaB6 and Si were evenly distributed on the Ti60 titanium alloy spheres.
[0061] (2) The microstructure of the (TiB2+LaB6+Si) / Ti60 composite material was observed using field emission scanning electron microscopy and transmission electron microscopy. The test results are shown in [Figure number missing]. Figure 2 , Figure 3 No obvious pores were observed in the matrix, indicating good density of the composite material. When the TiB2 content was 0.5 wt.%, a multi-scale "non-uniform network structure" was formed, with micron-sized TiB2... w La2O grows at the α-phase and β-phase grain boundaries. 3p Silicides exist within the α-phase grains and at the interface between the α-phase and β-phase grains, exhibiting a needle-like fibrous structure. The results show that as the TiB2 content increases, but TiB... wThe size has not increased; it could be TiB. w The interfacial reaction between TiB2 and the titanium matrix was suppressed, suggesting that the network structure of the reinforcing material has a significant impact on the mechanical properties of DRTiMCs. TEM results indicate that some TiB2... w Significantly refined into nanofibers and absorbed within the grains, forming a unique interface / intracrystalline structure, TiB exhibits a typical orientation relationship with α-Ti: and TiB w The interplanar spacing is 0.447 nm. EDS energy dispersive spectroscopy analysis revealed enrichment of La, O, and Si elements, but B was not prominent, which differs from previous findings that the nanoparticles were La2O. 3p .
[0062] (3) The IPF images of titanium alloys and DRTiMCs visually demonstrate that ( Figure 4 and 5 As the ceramic particle content increases, the microstructure gradually changes from coarse Widmanstätten to equiaxed grains, and the matrix grains are refined. The coarse original α grains are effectively removed, and the grain size is refined from 23.1 μm to 14.8 μm. The above provides a relatively intuitive demonstration of nano-TiB. w and La2O 3p The non-uniform network grain refinement effect, and the carefully designed interface / intragranular structure, may bring about ideal improvements to the mechanical properties of DRTiMCs. Results show that, under the same load, TiB... w The nanohardness of TiB is higher than that of the FG region and exceeds that of the CG region. w The nanohardness differences in the FG and CG regions reflect the hardness differences between these regions, which leads to back stress hardening during deformation and ultimately affects the strength of DRTiMCs.
[0063] (4) Room temperature tensile test, test results are shown in […]. Figure 6 The (TiB2+LaB6+Si) / Ti60 composite material has a room temperature ultimate tensile strength of 1544 MPa and an elongation after fracture of 7.7%.
[0064] (5) Numerous fractures of TiB2+LaB6+Si) / Ti60 composite material were observed on the room temperature fracture surface. w And microscopic pores; research revealed that these pores were formed by extracted La2O. 3p Furthermore, the dimples are obvious, indicating that TiB w and La2O 3p It is beneficial to adjust the strength and ductility of DRTiMCs.
[0065] (6) The (TiB2+LaB6+Si) / Ti60 composite material described in step (3) was observed using a field emission scanning electron microscope. The test results are shown in […]. Figure 7 After hot rolling, TiB whiskers are generated at the DRTiMCs interface to form a network structure, which significantly improves the interfacial bonding between the reinforcing phase and the matrix material.
[0066] (7) Room temperature tensile test, test results are shown in […]. Figure 9 The (TiB2+LaB6+Si) / Ti60 composite material exhibits a room-temperature ultimate tensile strength of 1560 MPa and an elongation after fracture of 10.2%. After hot rolling, numerous dimples of varying sizes are observed in the tensile fracture surface of the (TiB2+LaB6+Si) / Ti60 composite material, indicating good plasticity. Furthermore, torn whiskers are visible at the fracture surface, suggesting that whiskers play a crucial role in delaying crack propagation and deflecting cracks, indicating the existence of multiple strengthening mechanisms that further enhance the strength and plasticity of the composite material.
[0067] This invention uses titanium alloy powder as the matrix material, with reinforcing particles uniformly dispersed on the surface of the titanium alloy powder matrix material, and possessing micro / nano TiB whiskers (TiB). w A bimodal non-uniform network structure composed of La2O3 and TiB particles. DRTiMCs were prepared using a self-developed BGBM combined with field-assisted sintering technology (low pressure, high temperature) and hot rolling technology. La2O3 and TiB... w The introduction of [a specific substance] forms a unique bimodal non-uniform network structure on the Ti60 matrix material, effectively hindering dislocation slip and delaying crack deflection, passivation, and propagation. This is particularly evident in the formation of nanoscale TiB at the composite material interface and within the grains. w By incorporating La2O3 nanoparticles into the metal powder matrix in a network structure, the interfacial bonding between DRTiMCs and the matrix material is improved, achieving a good balance between strength and plasticity, and effectively solving the problem of prioritizing strength over plasticity.
[0068] The above embodiments are merely illustrative of the present invention and do not limit the technical solutions of the present invention. Those skilled in the art can make certain modifications or substitutions to the present invention, and those skilled in the art can easily implement other modifications. Therefore, any modifications that do not depart from the spirit of the present invention should be covered within the scope of the claims of the present invention.
Claims
1. A method for preparing a titanium-based composite material with a dual-modal non-uniform network structure, characterized in that: This discontinuous reinforced titanium matrix composite material comprises a matrix of two particle sizes and three reinforcing materials; The matrix is a Ti60 titanium alloy; The reinforcing agents are titanium diboride (TiB2), lanthanum hexaboride (LaB6), and silicon powder (Si); The interface structure between the reinforcement and the matrix is micron-sized TiB. w Nano TiB w Nano-La2O3 and nano-silicides form a bimodal non-uniform network structure with the matrix.
2. The method for preparing a dual-modal non-uniform network structure titanium-based composite material as described in claim 1, characterized in that: The matrix has an ultrafine α-structure. p β phase and nano-silicides.
3. A method for preparing a dual-modal non-uniform network structure titanium-based composite material, characterized by the following steps: include: (1) TiB2, LaB6, Si and Ti60 titanium alloy powders were ball-milled and mixed, then the ball milling media were removed and dried to obtain composite powder; (2) The composite powder obtained in step (1) is sintered to obtain a preformed blank; (3) The preform obtained in step (1) is subjected to hot rolling deformation treatment to obtain (TiB2+LaB6+Si) / Ti60 composite material.
4. The method for preparing a dual-modal non-uniform network structure titanium-based composite material according to claim 3, characterized in that: In step (1), based on a total mass of 100 wt.% for TiB2, LaB6, Si, and Ti60 titanium alloy powder, the mass fraction of TiB2 is 0.05%–1.00%, the mass fraction of LaB6 is 0.20%–0.50%, the mass fraction of Si is 0.01%–0.05%, and the mass fraction of Ti60 titanium alloy powder is 98.0%–99.70%.
5. A method for preparing a dual-modal non-uniform network structure titanium-based composite material according to claim 3 or 4, characterized in that: The average particle size of the Ti60 titanium alloy powder is 0–15 μm and 25–60 μm; The average particle size of TiB2 is 1–3 μm, that of LaB6 is 1–2 μm, and that of Si is 30–60 nm.
6. The method for preparing a dual-modal non-uniform network structure titanium-based composite material according to claim 3, characterized in that: In step (1), the ball milling parameters are as follows: the ball milling medium is anhydrous ethanol, and when the powder mass is 20-80g, the volume of anhydrous ethanol used is 150-300mL; the rotation speed is 250-350r / min, the time is 2-8h, the ball-to-material ratio is 8:1, and the grinding balls are composed of two sizes of agate balls, namely large-sized agate balls and small-sized agate balls. The diameter of the large-sized agate balls is 8-10mm, the diameter of the small-sized agate balls is 2-5mm, and the mass ratio of the large-sized agate balls to the small-sized agate balls is 5:
1.
7. The method for preparing a dual-modal non-uniform network structure titanium-based composite material according to claim 3, characterized in that: In step (1), rotary evaporation drying is used for drying. The process is as follows: the mixed slurry is placed in a 500mL eggplant-shaped flask and vacuum dried at 75-85℃ for 15min to allow the anhydrous ethanol to evaporate completely, thereby obtaining the dried composite powder.
8. The method for preparing a dual-modal non-uniform network structure titanium-based composite material according to claim 3, characterized in that: In step (2), the composite powder is sintered using field-assisted sintering technology. The sintering parameters are: vacuum degree <15Pa, heating rate 80~150℃ / min, sintering temperature 1000~1200℃, sintering pressure 30~50MPa, and holding time 10~15min. After sintering, the powder is cooled, polished, cleaned, and dried.
9. The method for preparing a dual-modal non-uniform network structure titanium-based composite material according to claim 8, characterized in that: In step (2), the thickness of the preform obtained is 10-15 mm.
10. The method for preparing a dual-modal non-uniform network structure titanium-based composite material according to claim 8, characterized in that: In step (3), the preformed billet is hot-rolled and deformed using a twin-roll mill. The hot-rolling deformation method is as follows: the preformed billet is placed in an electric resistance furnace and held at 900-950°C for 10-15 minutes. Then, it is immediately subjected to 3-6 passes of hot rolling with a deformation amount of 60%-70%. The billet is then returned to the furnace for 1-2 minutes between passes. Finally, the hot-rolled sample is placed in the air to cool to room temperature.
Citation Information
Patent Citations
Gradient annular groove ball milling tank
CN222175945U