Method for preparing fiber-reinforced cermet material

Abstract

The present invention belongs to the technical field of material preparation, and aims to solve the problem of the overall properties of an existing cermet material being affected by non-uniform microstructure of the material caused by the difficulty for accurately controlling the phase distribution and grain size of a cermet matrix by means of the material and the preparation process thereof. To this end, the present invention provides a method for preparing a fiber-reinforced cermet material. The method comprises: pre-treating silicon carbide fibers; mixing and grinding a titanium powder and a silicon carbide ceramic powder according to a predetermined proportion; then adding silicon carbide fiber particles thereto and placing same into an ultrasonic mixer; adding a dispersant and a binder thereto, and then mixing same; sequentially subjecting the mixture to cold isostatic pressing molding and hot press molding; and sequentially subjecting the obtained green body to pre-sintering, high-temperature sintering, cutting and surface treatments. The cermet material prepared in the present invention shows significant improvements in terms of strength, toughness, hardness, high-temperature resistance, wear resistance and corrosion resistance, thereby better satisfying the high-performance requirements in the aviation field and providing strong support for the aviation industry.

Description

A method for preparing fiber-reinforced metal-ceramic materials

[0001] Cross-references

[0002] This application is based on and claims priority to Chinese Patent Application No. 202411788122.1, filed on December 6, 2024, the entire contents of which are incorporated herein by reference. Technical Field

[0003] This invention relates to the field of materials preparation technology, and specifically to a method for preparing fiber-reinforced metal-ceramic materials. Background Technology

[0004] In modern industry, the performance and quality of materials often determine the performance and reliability of products. With the continuous advancement of science and technology, various new materials are emerging one after another, and material preparation technology is also constantly innovating and developing. Although traditional material preparation methods can meet the needs of production and life to a certain extent, they are gradually showing some limitations when facing increasingly complex and diverse application scenarios. In many fields, the requirements for the strength, hardness, toughness, high temperature resistance, corrosion resistance, and other properties of materials are becoming increasingly higher. Traditional single materials often cannot simultaneously possess these excellent comprehensive properties. In order to overcome this problem, the research and preparation of composite materials has gradually become a hot topic in the field of materials. Composite materials, by combining two or more materials with different properties, can give full play to their respective advantages, thereby obtaining superior performance compared to single materials.

[0005] For example, in the field of aerospace materials, the aerospace industry, as a high-end sector of modern industry, has extremely stringent requirements for material performance. Aircraft must withstand extreme and harsh environmental conditions during flight, including high temperatures, high pressures, high stresses, and high corrosion. Therefore, aerospace materials must possess superior performance to ensure the safe, reliable, and efficient operation of aircraft. In terms of strength, aerospace materials need sufficient strength to withstand various loads during flight, including the weight of the fuselage structure, aerodynamic loads, and engine thrust. Simultaneously, materials must possess good toughness to prevent fracture under impact or vibration. High-temperature resistance is another key performance requirement for aerospace materials. In the engine areas and high-temperature regions generated by friction with air during high-speed flight, materials must maintain their mechanical properties and physicochemical stability at high temperatures, without softening, deformation, or oxidation. Furthermore, aerospace materials must possess good corrosion resistance to resist the corrosive effects of atmospheric oxygen, moisture, pollutants, and fuel. At the same time, to meet the requirements of lightweight aircraft, materials should also have low density. However, meeting these numerous and stringent performance requirements simultaneously presents significant challenges to traditional material preparation methods and existing material systems.

[0006] As a commonly used aerospace material, the microstructure of the cermet matrix has a significant impact on the material's performance. However, existing preparation processes make it difficult to precisely control the distribution of each phase and grain size in the cermet matrix, resulting in an inhomogeneous microstructure. This affects the stability and consistency of the material's mechanical, thermal, and chemical properties. For example, an inhomogeneous microstructure can lead to a decrease in the material's strength and oxidation resistance at high temperatures, and it is prone to local deformation or fracture when subjected to external forces.

[0007] Therefore, there is a need in the art for a method for preparing fiber-reinforced metal-ceramic materials to solve the above problems. Summary of the Invention

[0008] In order to solve the above-mentioned technical problems, namely the difficulty in accurately controlling the distribution of each phase and grain size in the metal ceramic matrix in the existing preparation process of metal ceramic materials, which leads to the inhomogeneity of the material microstructure and thus affects the overall performance of the material.

[0009] This invention provides a method for preparing a fiber-reinforced metal-ceramic material, the method comprising:

[0010] S1: Pre-treat silicon carbide fibers to obtain silicon carbide fiber particles;

[0011] S2: Titanium metal powder and silicon carbide ceramic powder are mixed and ground in a predetermined ratio to obtain metal-ceramic powder;

[0012] S3: The metal ceramic powder and the silicon carbide fiber particles are placed in an ultrasonic mixer for mixing;

[0013] S4: Add dispersant and binder to the mixture obtained in step S3 and mix and grind again;

[0014] S5: The mixture obtained in step S4 is subjected to cold isostatic pressing and hot pressing in sequence. During the hot pressing process, argon gas is used for atmosphere protection.

[0015] S6: The hot-pressed blank is placed in a tube furnace and pre-sintered at low temperature under an argon atmosphere;

[0016] S7: The pre-sintered billet is placed in a hot isostatic pressing furnace and sintered at high temperature under an argon atmosphere, and then slowly cooled to room temperature in the furnace.

[0017] S8: The cooled material is cut and surface polished, then nitrogen ions are implanted into the material surface by ion implantation and annealing is performed to finally obtain fiber-reinforced metal ceramic material.

[0018] In some preferred embodiments, step S1 specifically includes:

[0019] S11: Immerse silicon carbide fibers in a hydrofluoric acid solution;

[0020] S12: After soaking, the silicon carbide fiber is thoroughly rinsed with deionized water and then dried.

[0021] S13: The dried silicon carbide fiber is placed in a chemical vapor deposition furnace, and chemical vapor deposition is performed at high temperature using trichloromethylsilane and hydrogen as reaction gases to deposit a silicon carbide coating on the surface of the silicon carbide fiber.

[0022] S14: Prepare a sol solution containing tetraethyl orthosilicate, ethanol and water according to a predetermined ratio, immerse the chemically vapor-deposited silicon carbide fiber in the sol solution, and then dry and heat-treat it to convert the sol into a silicon dioxide coating. In step S14, the immersion step to the heat treatment step is repeated 2-4 times.

[0023] S15: Silicon carbide fibers coated with silicon carbide and silicon dioxide are placed in a tube furnace and subjected to high-temperature annealing under an argon atmosphere.

[0024] S16: Grind the silicon carbide fibers after high-temperature annealing into silicon carbide fiber particles.

[0025] In some preferred embodiments, in step S11, the concentration of the hydrofluoric acid solution is 8-12%, and the soaking time is 25-35 minutes;

[0026] In step S12, the drying temperature is 75-90℃ and the drying time is 1.8-2.2 hours;

[0027] In step S13, the high-temperature treatment temperature is 1000-1300℃, the gas flow ratio of trichloromethylsilane to hydrogen is 1:(8.5-12), and the chemical vapor deposition time is 1.5-3 hours;

[0028] In step S14, the molar ratio of tetraethyl orthosilicate, ethanol and water is 1:(8-12):(4-6), the soaking time is 0.5-1.5 hours, the air drying time is 10-13 hours, and the heat treatment temperature is 580-680℃.

[0029] In step S15, the high-temperature annealing temperature is 950-1050℃, and the holding time is 1.8-2.3 hours.

[0030] In some preferred embodiments, step S2 specifically includes:

[0031] S21: Mix titanium metal powder and silicon carbide ceramic powder in a mass ratio of 40:60;

[0032] S22: Place the mixed powder into a ball mill for ball milling. The ball milling time is 11-12 hours, the ball mill speed is 280-330 r / min, and the ball-to-powder ratio is (4.7-5.5):1.

[0033] In some preferred embodiments, in step S3, the volume fraction of the metal ceramic powder is 80-82%, the volume fraction of the silicon carbide fiber particles is 18-20%, the mixing time of the metal ceramic powder and the silicon carbide fiber particles in the ultrasonic mixer is 1-1.2 hours, and the ultrasonic power is 1000-1200W.

[0034] In some preferred embodiments, in step S4, the mass fraction of the mixture obtained in step S3 is 95.5-97%, the mass fraction of the dispersant is 1-1.5%, and the mass fraction of the binder is 2-3%, wherein the dispersant is polyvinyl alcohol and the binder is phenolic resin;

[0035] Step S4 specifically includes:

[0036] S41: Add dispersant and binder to the mixture obtained in step S3;

[0037] S42: Place the mixture obtained in step S41 into a ball mill and ball mill again for 6-7 hours. The speed of the ball mill is 200-250 r / min and the ball-to-material ratio is 3:1.

[0038] In some preferred embodiments, in step S5, the mixture obtained in step S4 is subjected to cold isostatic pressing using a cold isostatic pressing machine, wherein the set pressing pressure of the cold isostatic pressing machine is 180-210 MPa, and the holding time is 5-7 minutes; and / or,

[0039] In step S5, a hot press forming machine is used to hot press the material after cold isostatic pressing. The hot pressing temperature of the hot press forming machine is 1500-1600℃, the hot pressing pressure is 50-55MPa, and the holding time is 1.5-2 hours.

[0040] In some preferred embodiments, in step S6, the pre-sintering temperature of the tubular furnace is 800-900°C, and the holding time is 2-2.5 hours; and / or,

[0041] In step S7, the sintering temperature of the hot isostatic pressing sintering furnace is 1800-2000℃, the pressure is 100-120MPa, and the holding time is 4-5 hours.

[0042] In some preferred embodiments, a magnetic field generating device is provided in both the tubular furnace and the hot isostatic pressing furnace, and the magnetic field strength generated by the magnetic field generating device is 0.5-2 Tesla during the pre-sintering and high-temperature sintering of the billet.

[0043] In some preferred embodiments, in step S8, the ion implantation energy is 100-110 keV and the dose is 1×10⁻⁶. 17 ions / cm 2 .

[0044] The present invention has the following beneficial effects:

[0045] In terms of fiber treatment and reinforcement, this invention pre-treats silicon carbide fibers to effectively remove surface impurities and oxide layers, laying the foundation for subsequent coating adhesion and good bonding with the cermet matrix. This improves the interfacial bonding strength between the fiber and the matrix, better leveraging the fiber reinforcement effect and enhancing the overall strength and toughness of the material. Processing the fibers into granules increases the contact area with the cermet powder, improves dispersion uniformity, reduces agglomeration and localized stress concentration, and makes the material properties more stable and reliable. Through a specific process, the cermet powder and silicon carbide fiber particles are thoroughly mixed and tightly bonded. The fiber-reinforced structure effectively transfers loads, prevents crack propagation, absorbs dispersed energy, and significantly improves the material's fracture toughness. In terms of material preparation processes and microstructure optimization, ultrasonic mixers ensure uniform mixing of cermet powder and silicon carbide fiber particles at the microscale, guaranteeing consistent macroscopic properties. The combination of cold isostatic pressing and hot pressing allows for uniform material filling of the mold, reducing porosity defects. Hot pressing, under argon atmosphere protection, utilizes high temperature and pressure to densify the material, resulting in tight particle bonding, improved density, strength, and microstructure uniformity, comprehensively enhancing mechanical and physical properties. Low-temperature pre-sintering and high-temperature sintering are performed in stages to remove organic matter and moisture from the green body. Low-temperature pre-sintering forms a structural framework that facilitates densification and performance improvement during high-temperature sintering. High-temperature sintering in the hot isostatic pressing furnace... Under an argon atmosphere and high pressure, warm sintering allows for full diffusion and fusion of particles, eliminating porosity defects and resulting in a uniform and stable microstructure. This significantly improves properties such as density, strength, hardness, and wear resistance. Post-processing, including cutting and surface polishing, ensures precise dimensions and a smooth surface, improving appearance quality and dimensional accuracy, reducing friction and wear, and extending service life. Ion implantation technology injects nitrogen ions into the material surface, altering its chemical composition and microstructure, enhancing surface hardness, wear resistance, and corrosion resistance. Annealing eliminates implantation defects, stabilizes the surface structure, and strengthens surface properties, enabling the material to resist erosion and wear in complex aerospace environments, ensuring reliability and stability. Through this comprehensive preparation process, the fiber-reinforced metal-ceramic material prepared by this invention exhibits significantly improved strength, toughness, hardness, high-temperature resistance, wear resistance, and corrosion resistance. Its overall performance surpasses that of materials prepared using existing technologies, better meeting the high-performance requirements of the aerospace field. It is suitable for various aerospace components, providing strong support for the aerospace industry. Attached Figure Description

[0046] The features and advantages of the invention will be more clearly understood by referring to the accompanying drawings, which are schematic and should not be construed as limiting the invention in any way. In the drawings:

[0047] Figure 1 is a flowchart of the preparation method of the fiber-reinforced metal-ceramic material of the present invention. Detailed Implementation

[0048] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0049] Based on the background art, existing metal-ceramic materials suffer from difficulties in precisely controlling the distribution of phases and grain size within the metal-ceramic matrix during preparation, leading to inhomogeneous microstructure and affecting the overall performance of the material. This invention provides a method for preparing fiber-reinforced metal-ceramic materials, aiming to significantly improve the strength, toughness, hardness, high-temperature resistance, wear resistance, and corrosion resistance of the prepared materials. This better meets the high-performance requirements of the aerospace field and provides strong support for the aerospace industry.

[0050] As shown in Figure 1, the preparation method of the fiber-reinforced metal-ceramic material provided by the present invention includes:

[0051] S1: Pre-treat silicon carbide fibers to obtain silicon carbide fiber particles;

[0052] Preferably, step S1 specifically includes:

[0053] S11: Immerse silicon carbide fibers in an 8-12% hydrofluoric acid solution for 25-35 minutes. Hydrofluoric acid is highly corrosive and can effectively remove impurities and oxide layers from the fiber surface, providing a good foundation for the adhesion of subsequent coatings.

[0054] S12: After soaking, thoroughly rinse the silicon carbide fiber with deionized water to remove residual hydrofluoric acid and impurities on the fiber surface. Then, put the silicon carbide fiber into an oven and dry it at 75-90℃ for 1.8-2.2 hours to ensure that the moisture on the surface of the silicon carbide fiber is completely evaporated and it is in a dry state, which is convenient for subsequent processing steps.

[0055] S13: The dried silicon carbide fibers are placed in a chemical vapor deposition furnace, and chemical vapor deposition is carried out at a high temperature of 1000-1300℃ for 1.5-3 hours using trichloromethylsilane (MTS) and hydrogen as reaction gases. The gas flow ratio of trichloromethylsilane (MTS) to hydrogen is 1:(8.5-12) to deposit a silicon carbide coating of 0.3-0.8μm on the surface of the silicon carbide fibers. This coating can further enhance the performance of the fibers, improve their wear resistance and oxidation resistance, and also facilitate better bonding with the metal ceramic matrix.

[0056] S14: Prepare a sol solution containing tetraethyl orthosilicate, ethanol, and water at a molar ratio of 1:(8-12):(4-6). Immerse the chemically vapor-deposited silicon carbide fiber in the sol solution for 0.5-1.5 hours to allow the fiber to fully absorb the sol. Then dry it in the air for 10-13 hours to allow the solvent in the sol to evaporate and initially form a coating. Then perform heat treatment at a temperature of 580-680℃ to convert the sol into a silicon dioxide coating. In step S14, the immersion step to the heat treatment step is repeated 2-4 times, preferably 3 times, to increase the thickness and uniformity of the coating. The silicon dioxide coating can improve the chemical stability and high temperature resistance of the fiber. Together with the silicon carbide coating, it further enhances the overall performance of the fiber.

[0057] S15: Silicon carbide fibers coated with silicon carbide and silicon dioxide coatings are placed in a tube furnace and subjected to high-temperature annealing under an argon atmosphere. The high-temperature annealing temperature is 950-1050℃ and the holding time is 1.8-2.3 hours. The argon atmosphere can prevent the fibers from oxidizing at high temperatures. The annealing treatment can improve the bonding state between the coating and the fiber, increase the bonding strength, reduce defects in the coating, and make the fibers more stable and reliable in subsequent use, so as to better play a reinforcing role.

[0058] S16: Grind the silicon carbide fibers after high-temperature annealing into silicon carbide fiber particles.

[0059] S2: Titanium metal powder and silicon carbide ceramic powder are mixed and ground in a predetermined ratio to obtain a metal-ceramic powder. Titanium metal has good toughness and machinability, enabling the material to have a certain degree of deformation capability and ease of processing during molding and use; silicon carbide ceramic has high hardness, high strength, and high temperature resistance, which can improve the overall strength and high temperature resistance of the material. The combination of the two is expected to yield a metal-ceramic material with excellent comprehensive performance, meeting the high-performance requirements of aerospace and other fields.

[0060] Preferably, step S2 specifically includes:

[0061] S21: Mix titanium metal powder and silicon carbide ceramic powder in a mass ratio of 40:60;

[0062] S22: The mixed powder is put into a ball mill for ball milling. The ball milling time is 11-12 hours, the speed of the ball mill is 280-330 r / min, and the ball-to-powder ratio is (4.7-5.5):1. During the ball milling process, the rotation of the ball mill drives the ball material to move, so that the powders collide and rub against each other continuously, thereby achieving uniform mixing. The uniformly mixed metal-ceramic powder lays the foundation for subsequent mixing with fibers and the forming and performance of materials.

[0063] S3: Place the cermet powder and silicon carbide fiber particles into an ultrasonic mixer for mixing. The volume fraction of the cermet powder is 80-82%, and the volume fraction of the silicon carbide fiber particles is 18-20%. The mixing time is 1-1.2 hours, and the ultrasonic power of the ultrasonic mixer is 1000-1200W. Silicon carbide particles have the characteristics of small size and large specific surface area, which can play a role in refining grains, thereby improving the strength and toughness of the material. The ultrasonic waves generate high-frequency vibrations in the mixture, which enable the fibers to be evenly dispersed in the powder and avoid fiber agglomeration. The uniform dispersion of fibers is crucial for improving the overall performance of the material and enables the fibers to better play a reinforcing role in the material.

[0064] S4: Add dispersant and binder to the mixture obtained in step S3 and mix and grind again. The mass fraction of the mixture obtained in step S3 is 95.5-97%, the mass fraction of the dispersant is 1-1.5%, and the mass fraction of the binder is 2-3%. The dispersant is polyvinyl alcohol and the binder is phenolic resin.

[0065] Preferably, step S4 specifically includes:

[0066] S41: Add dispersant and binder to the mixture obtained in step S3. The dispersant helps to further improve the dispersion uniformity of powder and fiber in the mixing system and prevents re-agglomeration. The binder can play a binding role in the subsequent molding process, so that the material blank has a certain initial strength.

[0067] S42: Place the mixture obtained in step S41 into a ball mill and ball mill again for 6-7 hours. The speed of the ball mill is 200-250 r / min and the ball-to-material ratio is 3:1. By ball milling again, the additives are fully mixed with the powder and fibers, ensuring that the additives can be evenly distributed in the entire mixture system and play their due role, providing good material preparation for the subsequent molding process.

[0068] S5: The mixture obtained in step S4 is subjected to cold isostatic pressing and hot pressing in sequence. During the hot pressing process, argon gas is used for atmosphere protection.

[0069] Preferably, in step S5, a cold isostatic pressing (CIP) machine is used to perform CIP on the mixture obtained in step S4. The CIP machine is set to a pressing pressure of 180-210 MPa and a holding time of 5-7 minutes. Under high pressure, the gap between material particles is reduced, the density uniformity of the blank is improved, and a certain initial strength is also obtained. The advantage of CIP is that it can apply pressure more evenly, reduce stress concentration and defects inside the blank, and provide a high-quality blank for the subsequent thermoforming process.

[0070] Preferably, in step S5, a hot press forming machine is used to hot press the material after cold isostatic pressing. The hot pressing temperature of the hot press forming machine is 1500-1600℃, the hot pressing pressure is 50-55MPa, and the holding time is 1.5-2 hours. During the hot pressing process, an argon atmosphere is used for protection to prevent the material from oxidizing at high temperature. The combined effect of high temperature and high pressure further densifies the material, making the bonding between particles tighter, thereby improving the material's performance. The argon atmosphere can isolate air, prevent the material from reacting chemically with oxygen, and ensure the purity and performance stability of the material.

[0071] S6: The hot-pressed blank is placed in a tube furnace and pre-sintered at low temperature under an argon atmosphere. The pre-sintering temperature of the tube furnace is 800-900℃, and the holding time is 2-2.5 hours. Low-temperature pre-sintering helps to remove organic matter and moisture from the blank. At a temperature of 800-900℃, organic matter will decompose and volatilize, and moisture will also be evaporated, preparing for high-temperature sintering. At the same time, low-temperature pre-sintering can also cause some components in the blank to react initially and form a certain structural framework, which is beneficial to the densification and performance improvement of the material during high-temperature sintering.

[0072] S7: The pre-sintered green body is placed in a hot isostatic pressing (HIP) furnace and sintered at high temperature under an argon atmosphere. Then, it is slowly cooled to room temperature in the furnace. The sintering temperature of the HIP furnace is 1800-2000℃, the pressure is 100-120MPa, and the holding time is 4-5 hours. During the high-temperature sintering process, an argon atmosphere is also used to protect the material and prevent oxidation. The high temperature and high pressure environment allows the material particles to fully diffuse and fuse, making the material denser and significantly improving its performance, such as strength, hardness, and wear resistance. HIP can effectively eliminate internal pores and defects in the material, making the material's microstructure more uniform and stable, further improving the material's comprehensive performance and meeting the high-performance requirements of high-end fields such as aerospace.

[0073] Preferably, a magnetic field generating device is installed in both the tube furnace and the hot isostatic pressing furnace. During the pre-sintering and high-temperature sintering of the green body, the magnetic field strength generated by the magnetic field generating device is 0.5-2 Tesla. Through repeated experiments, comparisons and analyses, the inventors found that if the magnetic field strength is lower than 0.5 Tesla, it is impossible to generate sufficient Lorentz force on the charged particles in the material, making it difficult to achieve the purpose of inducing crystal structure adjustment and reducing defects. In actual preparation, the direction of the magnetic field is set to be parallel to or the same as the growth direction of the crystal, so that the crystal grows more orderly. For example, for material components in aerospace parts that need to withstand unidirectional tensile force, the direction of the magnetic field is set to be the same as the direction of the tensile force. In this way, during the magnetic field-assisted sintering process, the crystal structure in the material will grow more orderly along the direction of the magnetic field (that is, the direction of the tensile force), thereby better resisting tensile stress. Meanwhile, the duration of the magnetic field application is matched with the duration of the sintering process. During the high-temperature sintering stage, the temperature is 1800-2000℃ and the holding time is 4-5 hours. The magnetic field can continue to act throughout the holding time. During this high-temperature stage, the material particles are in an active state of diffusion and fusion. The continuous action of the magnetic field helps to guide the orderly arrangement of the crystal structure during the densification process of the material.

[0074] More preferably, in the initial stage of sintering, when the material just begins to heat up and the particles begin to initially bond, a relatively weak magnetic field (0.5-1 Tesla) is applied for a short period (the first 1-2 hours) to help the material form a preliminary ordered structure. Then, in the later stage of sintering (after 1-2 hours), the magnetic field strength is increased (1-2 Tesla) and continues until the end of sintering to further optimize the crystal structure, making the material more dense and uniform. This segmented setting of magnetic field parameters allows for more precise control of the microstructure evolution process of the material, improving material performance. Specifically, in the above, the initial sintering time can be 0-1 hours, and the later sintering time can be 1-4 hours, or the initial sintering time can be 2 hours, and the later sintering time can be 2-5 hours.

[0075] S8: The cooled material is cut and surface polished, then nitrogen ions are implanted into the material surface by ion implantation and then annealed to finally obtain fiber-reinforced metal ceramic material.

[0076] Preferably, the material is cut to a suitable length and width using a cutting process, and the surface is ground using a grinding process to make it smoother and more even. During processing, low-stress processing methods, such as electrical discharge machining (EDM) or laser processing, are employed. Using low-stress processing methods avoids introducing stress and damaging the material surface, ensuring that the material's performance is not affected by the processing. After processing, polishing is performed to further improve the surface quality of the material, making it smoother, reducing surface roughness, and improving the material's aesthetics and performance. Ion implantation technology is used to implant nitrogen ions into the material surface. The ion implantation energy is 100-110 keV, and the dose is 1×10⁻⁶. 17 ions / cm 2 Nitrogen ion implantation can alter the chemical composition and microstructure of a material surface, thereby improving its hardness, wear resistance, and corrosion resistance. After implantation, the material is annealed in a vacuum furnace. The annealing temperature and time are determined based on the material characteristics and process requirements. Annealing can eliminate defects generated during the implantation process, making the material surface structure more stable and its performance superior. Through surface strengthening treatment, the surface properties of the material can be significantly improved, extending its service life and meeting the requirements for use in complex environments.

[0077] The technical solution of the present invention will be further illustrated below through multiple embodiments and comparative examples.

[0078] Example 1

[0079] Silicon carbide fibers were immersed in an 8% hydrofluoric acid solution for 25 minutes. After immersion, the silicon carbide fibers were thoroughly rinsed with deionized water, and then placed in an oven and dried at 75°C for 1.8 hours. The dried silicon carbide fibers were then placed in a chemical vapor deposition furnace, and chemical vapor deposition was performed at 1000°C for 1.5 hours using trichloromethylsilane (MTS) and hydrogen as reactant gases. The gas flow rate ratio of trichloromethylsilane (MTS) to hydrogen was 1:8.5, and the molar ratio was 1:8:4. A sol solution containing tetraethyl orthosilicate, ethanol, and water was prepared. The chemically vapor-deposited silicon carbide fibers were immersed in the sol solution for 0.5 hours, then dried in air for 10 hours, followed by heat treatment at 580℃. The immersion, drying, and heat treatment steps were repeated twice. The silicon carbide fibers coated with both silicon carbide and silicon dioxide were placed in a tube furnace and subjected to high-temperature annealing at 950℃ for 1.8 hours under an argon atmosphere. The annealed silicon carbide fibers were then ground into silicon carbide fiber particles.

[0080] Titanium metal powder and silicon carbide ceramic powder were mixed at a mass ratio of 40:60. The mixed powder was then ball-milled for 11 hours at a speed of 280 r / min and a ball-to-powder ratio of 4.7:1. Metal ceramic powder and silicon carbide fiber particles were then mixed in an ultrasonic mixer with a volume fraction of 80% for the metal ceramic powder and 20% for the silicon carbide fiber particles. The mixing time was 1 hour, and the ultrasonic power of the ultrasonic mixer was 1000 W. Polyvinyl alcohol and phenolic resin were added to the resulting mixture, with a mass fraction of 95.5%, 1% for polyvinyl alcohol, and 3.5% for phenolic resin. The resulting mixture was then ball-milled again for 6 hours at a speed of 200 r / min and a ball-to-powder ratio of 3:1.

[0081] The material is cold isostatically pressed using a cold isostatic pressing machine, with a set pressing pressure of 180 MPa and a holding time of 5 minutes. The cold isostatically pressed material is then hot-pressed using a hot pressing machine, with a hot pressing temperature of 1500℃, a hot pressing pressure of 50 MPa, and a holding time of 1.5 hours. Argon atmosphere protection is used during the hot pressing process.

[0082] The hot-pressed billet is placed in a tube furnace and pre-sintered at a low temperature under an argon atmosphere. The pre-sintering temperature of the tube furnace is 800℃, and the holding time is 2 hours. The pre-sintered billet is then placed in a hot isostatic pressing (HIP) furnace and sintered at a high temperature under an argon atmosphere. It is then slowly cooled to room temperature in the sintering furnace. The sintering temperature of the HIP furnace is 1800℃, the pressure is 100MPa, and the holding time is 4 hours. During the high-temperature sintering process, an argon atmosphere is used for protection. During the pre-sintering and high-temperature sintering of the billet, a magnetic field with a strength of 0.5 Tesla is generated by a magnetic field generator.

[0083] The cooled material was cut and surface polished, then nitrogen ions were implanted into the surface using ion implantation followed by annealing. The ion implantation energy was 100 keV and the dose was 1 × 10⁻⁶. 17 ions / cm 2 Ultimately, fiber-reinforced metal-ceramic materials were obtained.

[0084] Example 2

[0085] Silicon carbide fibers were immersed in a 10% hydrofluoric acid solution for 30 minutes. After immersion, the silicon carbide fibers were thoroughly rinsed with deionized water, and then placed in an oven and dried at 80°C for 2 hours. The dried silicon carbide fibers were then placed in a chemical vapor deposition furnace, and chemical vapor deposition was performed at 1150°C for 2 hours using trichloromethylsilane (MTS) and hydrogen as reactant gases. The gas flow ratio of trichloromethylsilane (MTS) to hydrogen was 1:10. A mixture was prepared according to a molar ratio of 1:10:5. A sol solution containing tetraethyl orthosilicate, ethanol, and water was placed in which the chemically vapor-deposited silicon carbide fibers were immersed for 1 hour, then dried in air for 11.5 hours, and then subjected to heat treatment at 630°C. The immersion, drying, and heat treatment steps were repeated 3 times. The silicon carbide fibers coated with silicon carbide and silicon dioxide were placed in a tube furnace and subjected to high-temperature annealing at 1000°C for 2 hours under an argon atmosphere. The high-temperature annealing temperature was then 1000°C, and the holding time was 2 hours. The high-temperature annealed silicon carbide fibers were then ground into silicon carbide fiber particles.

[0086] Titanium metal powder and silicon carbide ceramic powder were mixed at a mass ratio of 40:60. The mixed powder was then ball-milled for 11.5 hours at a speed of 300 r / min and a ball-to-powder ratio of 5:1. The cermet powder and silicon carbide fiber particles were then mixed in an ultrasonic mixer with a volume fraction of 81% for the cermet powder and 19% for the silicon carbide fiber particles. The mixing time was 1.1 hours, and the ultrasonic power of the ultrasonic mixer was 1100 W. Polyvinyl alcohol and phenolic resin were added to the resulting mixture, with a mass fraction of 96%, 1.5% for polyvinyl alcohol, and 2.5% for phenolic resin. The resulting mixture was then ball-milled again for 6.5 hours at a speed of 220 r / min and a ball-to-powder ratio of 3:1.

[0087] The material was cold isostatically pressed using a cold isostatic pressing machine, with a set pressing pressure of 195 MPa and a holding time of 6 minutes. The cold isostatically pressed material was then hot-pressed using a hot pressing machine, with a hot pressing temperature of 1550℃, a hot pressing pressure of 52 MPa, and a holding time of 1.8 hours. Argon atmosphere protection was used during the hot pressing process.

[0088] The hot-pressed billet is placed in a tube furnace and pre-sintered at a low temperature under an argon atmosphere. The pre-sintering temperature of the tube furnace is 850℃, and the holding time is 2.2 hours. The pre-sintered billet is then placed in a hot isostatic pressing (HIP) furnace and sintered at a high temperature under an argon atmosphere. It is then slowly cooled to room temperature in the sintering furnace. The sintering temperature of the HIP furnace is 1900℃, the pressure is 110MPa, and the holding time is 4.5 hours. During the high-temperature sintering process, an argon atmosphere is used for protection. During the pre-sintering and high-temperature sintering of the billet, a magnetic field with a strength of 1.2 Tesla is generated by a magnetic field generator.

[0089] The cooled material was cut and surface polished, then nitrogen ions were implanted into the surface using ion implantation followed by annealing. The ion implantation energy was 105 keV and the dose was 1×10⁻⁶. 17 ions / cm 2 Ultimately, fiber-reinforced metal-ceramic materials were obtained.

[0090] Example 3

[0091] Silicon carbide fibers were immersed in a 12% hydrofluoric acid solution for 35 minutes. After immersion, the silicon carbide fibers were thoroughly rinsed with deionized water, and then placed in an oven and dried at 90°C for 2.2 hours. The dried silicon carbide fibers were then placed in a chemical vapor deposition furnace and subjected to chemical vapor deposition at 1300°C for 3 hours using trichloromethylsilane (MTS) and hydrogen as reactants. The gas flow ratio of trichloromethylsilane (MTS) to hydrogen was 1:12. A mixture was prepared according to a molar ratio of 1:12:6. A sol solution containing tetraethyl orthosilicate, ethanol, and water was placed in which the chemically vapor-deposited silicon carbide fibers were immersed for 1.5 hours, then dried in air for 13 hours, and then subjected to heat treatment at a temperature of 680℃. The immersion, drying, and heat treatment steps were repeated 4 times. The silicon carbide fibers coated with silicon carbide and silicon dioxide were placed in a tube furnace and subjected to high-temperature annealing under an argon atmosphere at a temperature of 1050℃ for 2.3 hours. The high-temperature annealed silicon carbide fibers were then ground into silicon carbide fiber particles.

[0092] Titanium metal powder and silicon carbide ceramic powder were mixed at a mass ratio of 40:60. The mixed powder was then ball-milled for 12 hours at a speed of 330 r / min and a ball-to-powder ratio of 5.5:1. Metal ceramic powder and silicon carbide fiber particles were then mixed in an ultrasonic mixer with a volume fraction of 82% for the metal ceramic powder and 18% for the silicon carbide fiber particles. The mixing time was 1.2 hours, and the ultrasonic power of the ultrasonic mixer was 1200 W. Polyvinyl alcohol and phenolic resin were added to the resulting mixture, with a mass fraction of 97% for the mixture, 1% for polyvinyl alcohol, and 2% for phenolic resin. The resulting mixture was then ball-milled again for 7 hours at a speed of 250 r / min and a ball-to-powder ratio of 3:1.

[0093] The material is cold isostatically pressed using a cold isostatic pressing machine, with a set pressing pressure of 210 MPa and a holding time of 7 minutes. The cold isostatically pressed material is then hot-pressed using a hot pressing machine, with a hot pressing temperature of 1600℃, a hot pressing pressure of 55 MPa, and a holding time of 2 hours. Argon atmosphere is used for protection during the hot pressing process.

[0094] The hot-pressed billet is placed in a tube furnace and pre-sintered at a low temperature under an argon atmosphere. The pre-sintering temperature of the tube furnace is 900℃, and the holding time is 2.5 hours. The pre-sintered billet is then placed in a hot isostatic pressing (HIP) furnace and sintered at a high temperature under an argon atmosphere. It is then slowly cooled to room temperature in the sintering furnace. The sintering temperature of the HIP furnace is 2000℃, the pressure is 120MPa, and the holding time is 5 hours. During the high-temperature sintering process, an argon atmosphere is used for protection. During the pre-sintering and high-temperature sintering of the billet, a magnetic field generating device generates a magnetic field with a strength of 2 Tesla.

[0095] The cooled material was cut and surface polished, then nitrogen ions were implanted into the surface using ion implantation followed by annealing. The ion implantation energy was 110 keV and the dose was 1 × 10⁻⁶. 17 ions / cm 2 Ultimately, fiber-reinforced metal-ceramic materials were obtained.

[0096] Example 4

[0097] Silicon carbide fibers were immersed in a 9% hydrofluoric acid solution for 32 minutes. After immersion, the silicon carbide fibers were thoroughly rinsed with deionized water, and then placed in an oven and dried at 85°C for 2 hours. The dried silicon carbide fibers were then placed in a chemical vapor deposition furnace and subjected to chemical vapor deposition at 1200°C for 2.5 hours using trichloromethylsilane (MTS) and hydrogen as reactants. The gas flow ratio of trichloromethylsilane (MTS) to hydrogen was 1:11. The mixture was prepared according to a molar ratio of 1:11:5. A sol solution containing tetraethyl orthosilicate, ethanol, and water was used to immerse silicon carbide fibers after chemical vapor deposition for 1.2 hours, followed by air drying for 12 hours, and then heat treatment at 650°C. The immersion, drying, and heat treatment steps were repeated three times. The silicon carbide fibers coated with silicon carbide and silicon dioxide were placed in a tube furnace and subjected to high-temperature annealing at 1020°C for 2.1 hours under an argon atmosphere. The high-temperature annealed silicon carbide fibers were then ground into silicon carbide fiber particles.

[0098] Titanium metal powder and silicon carbide ceramic powder were mixed at a mass ratio of 40:60. The mixed powder was then ball-milled for 11.8 hours at a speed of 310 r / min and a ball-to-powder ratio of 5.2:1. The cermet powder and silicon carbide fiber particles were then mixed in an ultrasonic mixer with a volume fraction of 81.5% for the cermet powder and 18.5% for the silicon carbide fiber particles. The mixing time was 1.15 hours, and the ultrasonic power of the ultrasonic mixer was 1150 W. Polyvinyl alcohol and phenolic resin were added to the resulting mixture, with a mass fraction of 96.5%, 1.2% for polyvinyl alcohol, and 2.3% for phenolic resin. The resulting mixture was then ball-milled again for 6.8 hours at a speed of 230 r / min and a ball-to-powder ratio of 3:1.

[0099] The material was cold isostatically pressed using a cold isostatic pressing machine, with a set pressing pressure of 200 MPa and a holding time of 6.5 minutes. The cold isostatically pressed material was then hot-pressed using a hot pressing machine, with a hot pressing temperature of 1580℃, a hot pressing pressure of 53 MPa, and a holding time of 1.9 hours. An argon atmosphere was used for protection during the hot pressing process.

[0100] The hot-pressed billet is placed in a tube furnace and pre-sintered at a low temperature under an argon atmosphere. The pre-sintering temperature of the tube furnace is 880℃, and the holding time is 2.3 hours. The pre-sintered billet is then placed in a hot isostatic pressing (HIP) furnace and sintered at a high temperature under an argon atmosphere. It is then slowly cooled to room temperature in the sintering furnace. The sintering temperature of the HIP furnace is 1950℃, the pressure is 115MPa, and the holding time is 4.8 hours. During the high-temperature sintering process, an argon atmosphere is used for protection. During the pre-sintering and high-temperature sintering of the billet, a magnetic field generating device generates a magnetic field with a strength of 1.8 Tesla.

[0101] The cooled material was cut and surface polished, then nitrogen ions were implanted into the surface using ion implantation followed by annealing. The ion implantation energy was 108 keV and the dose was 1×10⁸ keV. 17 ions / cm 2 Ultimately, fiber-reinforced metal-ceramic materials were obtained.

[0102] Example 5

[0103] Silicon carbide fibers were immersed in an 11% hydrofluoric acid solution for 28 minutes. After immersion, the silicon carbide fibers were thoroughly rinsed with deionized water, and then placed in an oven and dried at 78°C for 1.9 hours. The dried silicon carbide fibers were then placed in a chemical vapor deposition furnace, and chemical vapor deposition was performed at 1050°C for 1.8 hours using trichloromethylsilane (MTS) and hydrogen as reactants. The gas flow ratio of MTS to hydrogen was 1:9. A molar ratio of 1:9:4.5 was used to prepare... A sol solution containing tetraethyl orthosilicate, ethanol, and water was placed in which the chemically vapor-deposited silicon carbide fibers were immersed for 0.8 hours, then dried in air for 10.5 hours, and then subjected to heat treatment at 600℃. The immersion, drying, and heat treatment steps were repeated twice. The silicon carbide fibers coated with silicon carbide and silicon dioxide were placed in a tube furnace and subjected to high-temperature annealing at 980℃ for 1.9 hours under an argon atmosphere. The high-temperature annealed silicon carbide fibers were then ground into silicon carbide fiber particles.

[0104] Titanium metal powder and silicon carbide ceramic powder were mixed at a mass ratio of 40:60. The mixed powder was then ball-milled for 11.2 hours at a speed of 290 r / min and a ball-to-powder ratio of 4.8:1. Metal ceramic powder and silicon carbide fiber particles were then mixed in an ultrasonic mixer with a volume fraction of 80.5% for the metal ceramic powder and 19.5% for the silicon carbide fiber particles. The mixing time was 1.05 hours, and the ultrasonic power of the ultrasonic mixer was 1050 W. Polyvinyl alcohol and phenolic resin were added to the resulting mixture, with a mass fraction of 95.8%, 1.3% for polyvinyl alcohol, and 2.9% for phenolic resin. The resulting mixture was then ball-milled again for 6.2 hours at a speed of 210 r / min and a ball-to-powder ratio of 3:1.

[0105] The material was cold isostatically pressed using a cold isostatic pressing machine, with a set pressing pressure of 185 MPa and a holding time of 5.5 minutes. The cold isostatically pressed material was then hot-pressed using a hot pressing machine, with a hot pressing temperature of 1520℃, a hot pressing pressure of 51 MPa, and a holding time of 1.6 hours. Argon atmosphere protection was used during the hot pressing process.

[0106] The hot-pressed billet is placed in a tube furnace and pre-sintered at a low temperature under an argon atmosphere. The pre-sintering temperature of the tube furnace is 820℃, and the holding time is 2.1 hours. The pre-sintered billet is then placed in a hot isostatic pressing (HIP) furnace and sintered at a high temperature under an argon atmosphere. It is then slowly cooled to room temperature in the sintering furnace. The sintering temperature of the HIP furnace is 1850℃, the pressure is 105MPa, and the holding time is 4.2 hours. During the high-temperature sintering process, an argon atmosphere is used for protection. During the pre-sintering and high-temperature sintering of the billet, a magnetic field generating device generates a magnetic field with a strength of 1.5 Tesla.

[0107] The cooled material was cut and surface polished, then nitrogen ions were implanted into the surface using ion implantation followed by annealing. The ion implantation energy was 103 keV and the dose was 1×10⁻⁶. 17 ions / cm 2 Ultimately, fiber-reinforced metal-ceramic materials were obtained.

[0108] Comparative Example 1

[0109] Titanium metal powder and silicon carbide ceramic powder were mixed at a mass ratio of 40:60. The mixed powder was then placed in a ball mill for ball milling for 12 hours at a speed of 300 r / min and a ball-to-material ratio of 5:1.

[0110] The ball-milled powder was cold isostatically pressed using a cold isostatic pressing machine with a pressing pressure of 200 MPa and a holding time of 6 minutes. Then, a hot pressing machine was used for hot pressing with a pressing temperature of 1550℃, a pressing pressure of 50 MPa, and a holding time of 1.8 hours. Argon atmosphere protection was used during the hot pressing process.

[0111] The hot-pressed blank is placed in a tube furnace and pre-sintered at a low temperature of 850°C for 2 hours under an argon atmosphere. Then, the pre-sintered blank is placed in a hot isostatic pressing furnace and sintered at a high temperature of 1900°C and 110 MPa for 4.5 hours under an argon atmosphere. After sintering, the blank is slowly cooled to room temperature in the furnace.

[0112] The sintered material was cut and surface polished, then nitrogen ions were implanted into the surface using ion implantation followed by annealing. The ion implantation energy was 105 keV and the dose was 1×10⁻⁶. 17 ions / cm 2 This yields a metal-ceramic material.

[0113] Comparative Example 2

[0114] Titanium metal powder and silicon carbide ceramic powder were mixed at a mass ratio of 40:60. The mixed powder was then placed in a ball mill for ball milling for 11 hours at a speed of 280 r / min and a ball-to-material ratio of 4.5:1.

[0115] The ball-milled powder was cold isostatically pressed using a cold isostatic pressing machine, with a pressing pressure of 190 MPa and a holding time of 5.5 minutes. Then, a hot pressing machine was used for hot pressing, with a hot pressing temperature of 1500℃, a hot pressing pressure of 45 MPa, and a holding time of 1.6 hours. Argon atmosphere protection was used during the hot pressing process.

[0116] The hot-pressed blank is placed in a tube furnace and pre-sintered at a low temperature of 800℃ for 1.8 hours under an argon atmosphere. Then, the pre-sintered blank is placed in a hot isostatic pressing furnace and sintered at a high temperature of 1800℃ and a pressure of 100MPa for 4 hours under an argon atmosphere. After sintering, the blank is slowly cooled to room temperature in the furnace.

[0117] The sintered material was cut and surface polished, then nitrogen ions were implanted into the surface using ion implantation followed by annealing. The ion implantation energy was 100 keV and the dose was 1 × 10⁻⁶. 17 ions / cm 2 This yields a metal-ceramic material.

[0118] Comparative Example 3

[0119] Titanium metal powder and silicon carbide ceramic powder were mixed at a mass ratio of 40:60. The mixed powder was then placed in a ball mill for ball milling for 10 hours at a speed of 250 r / min and a ball-to-material ratio of 4:1.

[0120] The ball-milled powder was cold isostatically pressed using a cold isostatic pressing machine, with a pressing pressure of 180 MPa and a holding time of 5 minutes. Then, a hot pressing machine was used for hot pressing, with a hot pressing temperature of 1450℃, a hot pressing pressure of 40 MPa, and a holding time of 1.5 hours. Argon atmosphere protection was used during the hot pressing process.

[0121] The hot-pressed blank is placed in a tube furnace and pre-sintered at a low temperature of 750°C under an argon atmosphere for 1.5 hours. Then, the pre-sintered blank is placed in a hot isostatic pressing furnace and sintered at a high temperature of 1700°C under an argon atmosphere for 3.5 hours. After sintering, the blank is slowly cooled to room temperature in the furnace.

[0122] The sintered material was cut and surface polished, then nitrogen ions were implanted into the surface using ion implantation followed by annealing. The ion implantation energy was 95 keV and the dose was 1 × 10⁻⁶. 17 ions / cm 2 This yields a metal-ceramic material.

[0123] The hardness, flexural strength, toughness, density, and high-temperature resistance of the metal-ceramic materials prepared in Examples 1 to 5 and Comparative Examples 1 to 3 were measured respectively. The specific measurement results are as follows:

[0124] As shown in the table above, the hardness values ​​of Examples 1 to 5 are significantly higher than those of the comparative examples. Example 1 has a hardness of 2200.25 HV, Example 5 has a hardness of 2250.3 HV, while the comparative example 3 only has a hardness of 1500.1 HV, a significant difference. Within the example groups, the hardness fluctuates with changes in process parameters. For example, Example 3 has a relatively high hardness of HV 2400.42. This is because the higher chemical vapor deposition temperature (1300℃) and longer deposition time (3 hours) during the silicon carbide fiber treatment process resulted in a denser and more uniform silicon carbide coating on the fiber surface, enhancing the overall material hardness. Simultaneously, the ball milling parameters in this example (12 hours of ball milling time, 330 r / min rotation speed, ball-to-material ratio of 5.5:1) ensured more thorough mixing of the cermet powder and silicon carbide fiber particles, which is beneficial for improving the material's hardness. The hardness of Comparative Examples 1 to 3 is relatively low and similar. This is because the comparative examples did not undergo complex pretreatment and addition of silicon carbide fibers. They were simply mixed with titanium metal powder and silicon carbide ceramic powder and then subjected to conventional operations such as molding and sintering. The reinforcing effect of silicon carbide fibers and related coating treatments were lacking. As a result, the microstructure of the materials was relatively loose and the bonding force between particles was weak, leading to lower hardness.

[0125] Regarding flexural strength, the flexural strength of Examples 1 to 5 is generally at a high level. The flexural strength of Example 1 is 850.32 MPa, and that of Example 5 is 860.4 MPa, with relatively small differences between the examples. This is because the addition of silicon carbide fibers has a good reinforcing effect. The fibers can effectively transfer stress in the material and prevent crack propagation, thereby improving the flexural strength of the material. At the same time, the process parameters in the powder mixing, molding, and sintering processes in the example group are relatively optimized. For example, the reasonable setting of ball milling time and speed makes the powder particles fine and uniformly mixed, which can form a good bonding interface during sintering, further improving the flexural performance of the material. The flexural strength of Comparative Examples 1 to 3 is significantly lower than that of the example group. The flexural strength of Comparative Example 3 is only 650.18 MPa, which is significantly lower than that of the example group. This is because the comparative examples did not utilize silicon carbide fibers for reinforcement and toughening, and the molding and sintering processes were relatively imprecise, resulting in more defects and pores inside the material. When subjected to bending stress, it is prone to fracture, resulting in lower flexural strength.

[0126] Regarding toughness, Examples 1 to 5 exhibited relatively stable toughness, with Example 1 showing a toughness of 12.55 MPa·m^1 / 2 and Example 5 showing a toughness of 12.88 MPa·m^1 / 2. The presence of silicon carbide fibers is a key factor in improving toughness. When the material is subjected to external forces, the fibers can absorb energy through mechanisms such as pull-out and fracture, preventing the rapid propagation of cracks and thus improving the toughness of the material. In addition, the surface treatment of silicon carbide fibers in the examples, such as chemical vapor deposition and sol solution immersion, improved the interfacial bonding between the fibers and the matrix, further enhancing the toughness of the material. Comparative Examples 1 to 3 showed relatively low toughness, with Comparative Example 3 showing a toughness of only 8.88 MPa·m^1 / 2. Due to the lack of toughening effect from silicon carbide fibers and the possible absence of effective measures to improve the microstructure and interfacial properties of the material during preparation, the material exhibited poor toughness and was more prone to brittle fracture under external impact.

[0127] Regarding density, Examples 1 to 5 all exhibited high densities, exceeding 98%, with Example 2 reaching 98.5%. This was attributed to the various processing methods employed in the examples. During the silicon carbide fiber treatment, steps such as chemical vapor deposition and sol-gel solution treatment resulted in a tighter bond between the fiber and the matrix, reducing porosity. Simultaneously, appropriate process parameters (such as cold isostatic pressing pressure, hot pressing temperature and pressure, and sintering temperature and pressure) during molding and sintering also contributed to material densification, increasing the material's density. Comparative Examples 1 to 3 showed relatively lower densities, ranging from 95.50% to 96.50%. These comparative examples did not undergo special treatment of the silicon carbide fibers and had some deficiencies in their molding and sintering processes, leading to more porosity and defects within the material, resulting in lower density. Lower density affects the material's mechanical properties and other properties, such as hardness, flexural strength, and high-temperature resistance.

[0128] In terms of high-temperature resistance, Examples 1 to 5 exhibit significantly better high-temperature resistance than the comparative examples. Example 1 has a high-temperature resistance of 1600.50℃, Example 5 has a high-temperature resistance of 1620.55℃, while Comparative Example 3 only has a high-temperature resistance of 1150.3℃. Silicon carbide fibers themselves have excellent high-temperature resistance and play a key role in the material. The treatment of silicon carbide fibers in the examples and the use of high-temperature and argon atmosphere protection during sintering enable the material to maintain good structural stability at high temperatures. In addition, the high density of the material also helps to improve its high-temperature resistance, reducing the intrusion of gases and impurities at high temperatures, thereby improving the material's high-temperature limit. Comparative Examples 1 to 3 have poor high-temperature resistance. Due to the lack of silicon carbide fiber reinforcement and the relatively simple process in preparation, the structure of the material is prone to changes at high temperatures, such as grain growth and phase transformation, leading to a decrease in material performance and a reduction in high-temperature resistance.

[0129] Furthermore, none of the comparative examples 1 to 3 involved pretreatment of the silicon carbide fibers. Examples 1 to 5, however, used acid etching to remove impurities and the natural oxide layer from the surface of the silicon carbide fibers, roughening the surface and increasing the adhesion between the subsequent coating and the fiber. Drying removed moisture from the fiber surface, preventing adverse effects such as pores and cracks during subsequent high-temperature processes like chemical vapor deposition. Chemical vapor deposition and sol-gel treatment formed silicon carbide and silica coatings on the silicon carbide fiber surface, further enhancing fiber performance and improving its adhesion to the matrix material, while also improving its high-temperature resistance. High-temperature annealing eliminated internal stress in the coating, making the coating structure more stable and improving the overall performance of the fiber. Grinding allowed for better mixing with the cermet powder, ensuring uniform fiber distribution within the material and effectively enhancing its reinforcing effect. Through these pretreatment processes, the overall performance of the fiber-reinforced cermet materials prepared in Examples 1 to 5 was significantly higher than that of the ordinary cermet materials prepared in Comparative Examples 1 to 3.

[0130] It should be noted that the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0131] The various embodiments in this invention are described in a progressive manner. Similar or identical parts between embodiments can be referred to mutually. Each embodiment focuses on describing the differences from other embodiments. In particular, the system embodiments are basically similar to the method embodiments, so the description is relatively simple; relevant parts can be referred to the descriptions in the method embodiments.

[0132] Those skilled in the art should understand that the discussion of any of the above embodiments is merely exemplary and is not intended to imply that the scope of this disclosure is limited to these examples; within the framework of this disclosure, the technical features of the above embodiments or different embodiments can also be combined, the steps can be implemented in any order, and there are many other variations of different aspects of one or more embodiments of the present invention as described above, which are not provided in detail for the sake of brevity.

[0133] Although this disclosure has been described in conjunction with specific embodiments thereof, many substitutions, modifications and variations of these embodiments will be apparent to those skilled in the art from the foregoing description.

[0134] One or more embodiments of the present invention are intended to cover all such substitutions, modifications, and variations that fall within the scope of protection of the present invention. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of one or more embodiments of the present invention should be included within the scope of protection of this disclosure.

Claims

1. A method for preparing a fiber-reinforced metal-ceramic material, characterized in that, The preparation method includes: S1: Pre-treat silicon carbide fibers to obtain silicon carbide fiber particles; S2: Titanium metal powder and silicon carbide ceramic powder are mixed and ground in a predetermined ratio to obtain metal ceramic powder; S3: The metal ceramic powder and the silicon carbide fiber particles are placed in an ultrasonic mixer for mixing; S4: Add dispersant and binder to the mixture obtained in step S3 and mix and grind again; S5: The mixture obtained in step S4 is subjected to cold isostatic pressing and hot pressing in sequence. During the hot pressing process, argon gas is used for atmosphere protection. S6: The hot-pressed blank is placed in a tube furnace and pre-sintered at low temperature under an argon atmosphere; S7: The pre-sintered billet is placed in a hot isostatic pressing furnace and sintered at high temperature under an argon atmosphere, and then slowly cooled to room temperature in the furnace. S8: The cooled material is cut and surface polished, then nitrogen ions are implanted into the material surface by ion implantation and annealing is performed to finally obtain fiber-reinforced metal ceramic material.

2. The method for preparing fiber-reinforced metal-ceramic materials according to claim 1, characterized in that, Step S1 specifically includes: S11: Immerse silicon carbide fibers in hydrofluoric acid solution; S12: After soaking, the silicon carbide fiber is thoroughly rinsed with deionized water and then dried. S13: The dried silicon carbide fiber is placed in a chemical vapor deposition furnace, and chemical vapor deposition is performed at high temperature using trichloromethylsilane and hydrogen as reaction gases to deposit a silicon carbide coating on the surface of the silicon carbide fiber. S14: Prepare a sol solution containing tetraethyl orthosilicate, ethanol and water according to a predetermined ratio, immerse the chemically vapor-deposited silicon carbide fiber in the sol solution, and then dry and heat-treat it to convert the sol into a silicon dioxide coating. In step S14, the immersion step to the heat treatment step is repeated 2-4 times. S15: Silicon carbide fibers coated with silicon carbide and silicon dioxide are placed in a tube furnace and subjected to high-temperature annealing under an argon atmosphere. S16: Grind the silicon carbide fibers after high-temperature annealing into silicon carbide fiber particles.

3. The method for preparing fiber-reinforced metal-ceramic materials according to claim 2, characterized in that, In step S11, the concentration of the hydrofluoric acid solution is 8-12%, and the soaking time is 25-35 minutes; In step S12, the drying temperature is 75-90℃ and the drying time is 1.8-2.2 hours; In step S13, the high-temperature treatment temperature is 1000-1300℃, the gas flow ratio of trichloromethylsilane to hydrogen is 1:(8.5-12), and the chemical vapor deposition time is 1.5-3 hours. In step S14, the molar ratio of tetraethyl orthosilicate, ethanol and water is 1:(8-12):(4-6), the soaking time is 0.5-1.5 hours, the air drying time is 10-13 hours, and the heat treatment temperature is 580-680℃. In step S15, the high-temperature annealing temperature is 950-1050℃, and the holding time is 1.8-2.3 hours.

4. The method for preparing fiber-reinforced metal-ceramic materials according to claim 1, characterized in that, Step S2 specifically includes: S21: Mix titanium metal powder and silicon carbide ceramic powder in a mass ratio of 40:60; S22: Place the mixed powder into a ball mill for ball milling. The ball milling time is 11-12 hours, the ball mill speed is 280-330 r / min, and the ball-to-powder ratio is (4.7-5.5):

1.

5. The method of producing a fiber-reinforced cermet material according to claim 1, characterized by, In step S3, the volume fraction of the metal ceramic powder is 80-82%, the volume fraction of the silicon carbide fiber particles is 18-20%, the mixing time of the metal ceramic powder and the silicon carbide fiber particles in the ultrasonic mixer is 1-1.2 hours, and the ultrasonic power is 1000-1200W.

6. The method of producing a fiber-reinforced cermet material according to claim 1, characterized by, In step S4, the mass fraction of the mixture obtained in step S3 is 95.5-97%, the mass fraction of the dispersant is 1-1.5%, and the mass fraction of the binder is 2-3%, wherein the dispersant is polyvinyl alcohol and the binder is phenolic resin; Step S4 specifically includes: S41: Add dispersant and binder to the mixture obtained in step S3; S42: Place the mixture obtained in step S41 into a ball mill and ball mill again for 6-7 hours. The speed of the ball mill is 200-250 r / min and the ball-to-material ratio is 3:

1.

7. The method for preparing fiber-reinforced metal-ceramic material according to claim 1, characterized in that, In step S5, the mixture obtained in step S4 is subjected to cold isostatic pressing using a cold isostatic pressing machine, wherein the set pressing pressure of the cold isostatic pressing machine is 180-210 MPa, and the holding time is 5-7 minutes; and / or, In step S5, a hot press forming machine is used to hot press the material after cold isostatic pressing. The hot pressing temperature of the hot press forming machine is 1500-1600℃, the hot pressing pressure is 50-55MPa, and the holding time is 1.5-2 hours.

8. The method of producing a fiber-reinforced cermet material according to claim 1, characterized by, In step S6, the pre-sintering temperature of the tubular furnace is 800-900℃, and the holding time is 2-2.5 hours; and / or, In step S7, the sintering temperature of the hot isostatic pressing sintering furnace is 1800-2000℃, the pressure is 100-120MPa, and the holding time is 4-5 hours.

9. The method for preparing the fiber-reinforced metal-ceramic material according to claim 1 or 8, characterized in that, Both the tubular furnace and the hot isostatic pressing furnace are equipped with magnetic field generating devices. During the pre-sintering and high-temperature sintering of the billet, the magnetic field strength generated by the magnetic field generating devices is 0.5-2 Tesla.

10. The method of producing a fiber-reinforced cermet material according to claim 1, characterized by, In step S8, the ion implantation energy is 100-110 keV, and the dose is 1×10⁻⁶. 17 ions / cm 2 .

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