A periodic lattice configuration toughened ceramic composite material and a method of making the same
By using 3D printing and melt infiltration technology to prepare periodic lattice-structured tough ceramic composite materials, the problem of high brittleness of ceramic materials was solved, and their service capability under strong impact and vibration conditions was improved, thus realizing high-strength and high-toughness ceramic composite materials.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- LANZHOU INST OF TECH
- Filing Date
- 2024-07-09
- Publication Date
- 2026-06-09
AI Technical Summary
The brittleness of ceramic materials makes it difficult for them to maintain long-term service under harsh conditions such as strong impact and vibration, limiting their application in occasions where they need to withstand impact or tensile stress.
A body-centered cubic or face-centered cubic framework was prepared using 3D printing technology. A through-hole ceramic matrix was prepared by injection molding. Tungsten carbide was deposited on the surface of the through-hole ceramic matrix. A metal binder phase was filled by melt infiltration to form a periodic lattice tough ceramic composite material.
It significantly improves the fracture toughness, flexural strength and compressive strength of ceramic composite materials, and the relative density of the material also reaches more than 99.3%, realizing the long-term service capability of ceramic materials under harsh working conditions.
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Figure BDA0004935160860000111
Abstract
Description
Technical Field
[0001] This invention relates to the field of ceramic material preparation technology, and in particular to a periodic lattice configuration tough ceramic composite material and its preparation method. Background Technology
[0002] Ceramic materials possess properties such as insulation, corrosion resistance, high temperature resistance, and wear resistance, and are widely used in aerospace, power, mining, and machining fields. However, the inherent brittleness of ceramic materials has always been one of the insurmountable challenges, making it difficult for them to maintain long-term service under harsh conditions such as strong impact and vibration, thus reducing efficiency and increasing costs.
[0003] Ceramic materials possess a range of significant advantages, such as high strength, high hardness, high temperature resistance, and good chemical stability, which have led to their widespread application in aerospace, materials engineering, electronic engineering, chemical engineering, and mechanical engineering. However, ceramic materials also have some notable drawbacks, including high brittleness.
[0004] The brittleness of ceramic materials is one of their most significant drawbacks. Due to the characteristics of their internal microstructure, ceramic materials are prone to fracture or splitting when subjected to external forces, thus limiting their application in situations requiring the resistance to impact or tensile stress.
[0005] To overcome these shortcomings of ceramic materials, researchers are constantly exploring new preparation processes and modification methods. For example, they are enhancing the toughness of materials by adding a certain proportion of fibers and reducing the number of pores; employing advanced processing technologies and equipment to improve the processing precision and surface quality of ceramic materials; and developing new ceramic composite materials to optimize their performance. These efforts are expected to enable ceramic materials to be applied and developed in more fields. However, current research has not truly solved the problem of the high brittleness of ceramic materials. Summary of the Invention
[0006] This invention addresses the engineering problem that the inherent brittleness of ceramic materials makes it difficult for them to maintain long-term service under harsh conditions such as strong impact and vibration, and provides a periodic lattice configuration tough ceramic composite material and its preparation method.
[0007] To achieve the above objectives, the present invention adopts the following technical solution:
[0008] In a first aspect, the present invention provides a method for preparing a periodic lattice-configured tough ceramic composite material, comprising the following steps:
[0009] Using solid paraffin as raw material, a body-centered cubic or face-centered cubic framework is prepared by 3D printing, and a through-hole ceramic matrix is prepared on the body-centered cubic or face-centered cubic framework by injection molding.
[0010] Tungsten carbide was deposited on the surface of a porous ceramic matrix using a one-step carbonization method, and a metal binder phase was filled into the porous ceramic matrix using a melt infiltration method to obtain a periodic lattice configuration tough ceramic composite material.
[0011] As a further improvement of the present invention, the body-centered cubic or face-centered cubic configuration frame adopts a ball-and-stick model, specifically a template-printed configuration frame.
[0012] As a further improvement of the present invention, the diameter of the sphere in the template printing configuration frame is 0.13-0.18 mm, the diameter of the rod is 0.03-0.05 mm, and the side length of the unit cell is 2.7-3.2 mm.
[0013] As a further improvement of the present invention, the preparation of a through-hole ceramic matrix on a body-centered cubic or face-centered cubic framework by injection molding includes:
[0014] Silicon carbide or silicon nitride powder is mixed with PVA solution to form a slurry, which is then injected into a 3D printed framework. The slurry is degreased at 320–350°C for 25–32 minutes and then sintered at 1720–1770°C for 62–71 minutes to obtain a through-hole ceramic matrix.
[0015] As a further improvement of the present invention, the average particle size of the silicon carbide or silicon nitride powder is 270-310 nanometers; the mass concentration of the PVA solution is 10%.
[0016] As a further improvement of the present invention, the silicon carbide or silicon nitride powder is mixed with the PVA solution at a mass percentage of (81-86):(14-19); the injection rate is 3-5 ml per second.
[0017] As a further improvement of the present invention, the deposition of tungsten carbide on the surface of a through-hole ceramic substrate using a one-step carbonization method includes:
[0018] Ammonium metatungstate and caramel were mixed into a solution, and a colloid was prepared at 105–115 °C for 12–16 hours.
[0019] The prepared colloid is injected into the pores inside the through-hole ceramic matrix and then treated at 1230–1260°C for 50–58 minutes.
[0020] As a further improvement of the present invention, ammonium metatungstate and caramel are prepared in a molar ratio of 1:(0.9 to 1.3) to form a solution with a concentration of 0.006 to 0.011 mol per liter.
[0021] As a further improvement of the present invention, the method of filling a porous ceramic matrix with a metallic binder phase by melt infiltration includes:
[0022] A cobalt-nickel binary alloy with a mass percentage of (61–70):(30–39) was infiltrated into the pores inside a ceramic matrix using a melting infiltration method at 1540–1580 °C for 14–19 minutes.
[0023] Secondly, the present invention provides a periodic lattice configuration tough ceramic composite material, which is prepared by the aforementioned preparation method.
[0024] As a further improvement of the present invention, the obtained tough ceramic composite material has a periodic lattice configuration, and the fracture toughness of the material is greater than or equal to 23.6 MPa·m. 1 / 2 The bending strength is greater than or equal to 1530 MPa, the compressive strength is greater than or equal to 3720 MPa, and the relative density is greater than or equal to 99.3%.
[0025] Compared with the prior art, the present invention has the following features and advantages:
[0026] This invention first uses solid paraffin wax as raw material to prepare a body-centered cubic (BCC) or face-centered cubic (FCC) framework using 3D printing. Then, a through-hole ceramic matrix is prepared on the BCC or FCC framework using injection molding. Next, tungsten carbide powder is deposited on the surface of the through-hole ceramic matrix using a one-step carbonization method. Finally, a metallic binder phase is filled into the through-hole ceramic matrix using a melt infiltration method. The solid paraffin wax framework with a periodic lattice configuration prepared by 3D printing serves two purposes: firstly, it occupies the periodic lattice positions at room temperature; secondly, at the debinding temperature, the solid paraffin wax vaporizes, leaving periodic lattice pores, laying the foundation for subsequent powder deposition and melt infiltration of the metallic phase, without affecting the injection molding performance of the silicon carbide or silicon nitride ceramic powder. The one-step carbonization method for depositing tungsten carbide powder on the inner wall of the periodic lattice through-holes facilitates the formation of a stable interface between the metallic binder phase and the ceramic matrix, improving the toughness and strength of the ceramic.
[0027] The tough ceramic composite material obtained by this invention has a periodic lattice configuration, and the fracture toughness of the material is greater than or equal to 23.6 MPa·m. 1 / 2 The bending strength is greater than or equal to 1530 MPa, the compressive strength is greater than or equal to 3720 MPa, and the relative density is greater than or equal to 99.3%. Detailed Implementation
[0028] To make the problems, solutions, and beneficial effects of this application clearer, the following detailed description is provided in conjunction with embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the scope of this application.
[0029] In this application, the term "and / or" describes the relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A existing alone, A and B existing simultaneously, or B existing alone. A and B can be singular or plural. The character " / " generally indicates that the preceding and following related objects have an "or" relationship.
[0030] In this application, "at least one" means one or more, and "more than one" means two or more. "At least one of the following" or similar expressions refer to any combination of these items, including any combination of single or multiple items. For example, "at least one of a, b, or c", or "at least one of a, b, and c", can both mean: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, and c can be single or multiple.
[0031] It should be understood that in the various embodiments of this application, the order of the above processes does not imply the order of execution. Some or all steps may be executed in parallel or sequentially. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of this application.
[0032] The terminology used in the embodiments of this application is for the purpose of describing particular embodiments only and is not intended to be limiting of this application. The singular forms "a" and "the" as used in the embodiments of this application and the appended claims are also intended to include the plural forms, unless the context clearly indicates otherwise.
[0033] The weights of the relevant components mentioned in the embodiments of this application can refer not only to the specific content of each component, but also to the proportional relationship between the weights of the components. Therefore, any scaling up or down of the content of the relevant components according to the embodiments of this application is within the scope disclosed in the embodiments of this application. Specifically, the mass in the embodiments of this application can be a well-known unit of mass in the chemical industry, such as μg, mg, g, or kg.
[0034] The terms "first" and "second" are used only to describe purposes and to distinguish objects, such as substances, from one another, and should not be construed as indicating or implying relative importance or implicitly specifying the number of method features indicated. For example, without departing from the scope of the embodiments of this application, a first XX may also be referred to as a second XX, and similarly, a second XX may also be referred to as a first XX. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature.
[0035] This invention discloses a method for preparing a periodic lattice-structured tough ceramic composite material, comprising the following steps:
[0036] Using solid paraffin as raw material, a body-centered cubic or face-centered cubic framework is prepared by 3D printing, and a through-hole ceramic matrix is prepared on the body-centered cubic or face-centered cubic framework by injection molding.
[0037] Tungsten carbide was deposited on the surface of a porous ceramic matrix using a one-step carbonization method, and a metal binder phase was filled into the porous ceramic matrix using a melt infiltration method to obtain a periodic lattice configuration tough ceramic composite material.
[0038] Using a periodic lattice configuration as the basic framework, a series of technologies such as 3D printing, injection molding, one-step deposition, and melt infiltration are effective means to improve the toughness of ceramic composite materials.
[0039] The principle of this invention is as follows:
[0040] Using 3D printing technology, solid paraffin wax is used as a raw material to precisely construct body-centered cubic or face-centered cubic frames. This frame design features a periodic lattice structure, which can effectively disperse and mitigate external forces while ensuring the overall strength of the material and improving its toughness.
[0041] A porous ceramic matrix is fabricated on a 3D-printed frame using injection molding. This technique ensures a uniform distribution of the ceramic matrix within the frame, and the porous structure helps increase the material's toughness.
[0042] Tungsten carbide was deposited on the surface of a porous ceramic matrix using a one-step carbide deposition method. Tungsten carbide possesses high hardness, high wear resistance, and good thermal stability, which can effectively enhance the surface properties of the ceramic matrix. At the same time, its bonding strength with the ceramic matrix is also high, which helps to improve the overall toughness of the composite material.
[0043] A metallic binder phase is filled into a porous ceramic matrix using a melt infiltration method. The metallic binder phase can fill the voids in the ceramic matrix, increasing the density of the material. At the same time, the good plasticity and toughness of the metallic material can also effectively improve the toughness of the ceramic composite material.
[0044] The periodic lattice configuration effectively disperses and mitigates external forces, improving the material's toughness. Simultaneously, the fabrication of a porous ceramic matrix allows for more free space within the material, further enhancing its toughness.
[0045] Optionally, the deposition of tungsten carbide and the filling of a metallic binder phase can significantly improve the surface properties and overall toughness of ceramic composites. The high hardness and high wear resistance of tungsten carbide can enhance the wear resistance and impact resistance of the material, while the addition of the metallic binder phase can improve the plasticity and toughness of the material.
[0046] Preferably, this preparation method combines 3D printing, injection molding, one-step deposition, and melt infiltration technologies to achieve high-precision preparation and performance optimization of ceramic composite materials. The combination of these technologies makes the preparation process more flexible and controllable, enabling it to meet the performance requirements of ceramic composite materials in various fields.
[0047] Therefore, the preparation method of the periodic lattice tough ceramic composite material of the present invention, by combining advanced preparation technology and unique structural design, effectively improves the toughness performance of the ceramic composite material, and has important practical application value and development prospects.
[0048] In the preparation of tough ceramic composite materials, this invention addresses the engineering problem that the inherent brittleness of ceramic materials makes it difficult to maintain long-term service under harsh conditions such as strong impact and vibration. Using a periodic lattice configuration as the basic framework, and employing a series of technologies including 3D printing, injection molding, one-step deposition, and melt infiltration, the relationship between the lattice framework index, matrix composition, injection molding process parameters, one-step carbonization process, melt infiltration process, and the mechanical properties of the tough ceramic composite material is investigated. As a further improvement, the process parameters for each step are as follows:
[0049] 1) Using solid paraffin wax as raw material and a ball-and-stick model with a body-centered cubic or face-centered cubic structure as a template, a 3D printing method is used to prepare the configuration frame. The diameter of the ball in the frame is 0.13-0.18 mm, the diameter of the stick is 0.03-0.05 mm, the side length of the unit cell is 2.7-3.2 mm, and the number of unit cells and the frame size are determined according to specific size requirements. Then, silicon carbide or silicon nitride powder with an average particle size of 270-310 nm is mixed with 10% PVA solution at a mass percentage of 81-86:14-19 to prepare a slurry. The slurry is injected into the 3D printed configuration frame at a rate of 3-5 ml per second. The slurry is degreased at 320-350℃ for 25-32 minutes and sintered at 1720-1770℃ for 62-71 minutes to obtain a through-hole ceramic matrix.
[0050] 2) Tungsten carbide powder is deposited on the surface of a porous ceramic matrix using a one-step carbonization method. Specifically, ammonium metatungstate and caramel are mixed at a molar ratio of 1:0.9-1.3 to prepare a solution with a concentration of 0.006-0.011 mol / L. The solution is prepared into a colloid at 105-115℃ for 12-16 hours and then injected into the pores inside the porous ceramic matrix. The matrix is then treated at 1230-1260℃ for 50-58 minutes. Finally, a cobalt-nickel binary alloy with a mass percentage of 61-70:30-39 is melt-infiltrated into the pores inside the deposited ceramic matrix at 1540-1580℃ for 14-19 minutes using a melt-infiltration method, ultimately obtaining a periodic lattice-structured tough ceramic composite material.
[0051] Therefore, for tough ceramic composites, the optimal lattice framework index, matrix composition, injection molding process parameters, one-step carbonization process, and melt infiltration process are crucial for maintaining high mechanical properties. This method offers high precision in composition control, strong process stability and repeatability, and can simultaneously improve the strength and toughness of tough ceramic composites.
[0052] The mechanical properties of the periodic lattice-configured tough ceramic composites prepared in the following examples are shown in Table 1.
[0053] Example 1
[0054] 1) Using solid paraffin wax as raw material and a ball-and-stick model with a body-centered cubic structure as a template, a 3D printing method was used to prepare the morphological framework. The diameter of the ball in the framework was 0.13 mm, the diameter of the stick was 0.03 mm, the side length of the unit cell was 2.7 mm, and the number of unit cells and the size of the framework were determined according to specific size requirements. Then, silicon carbide powder with an average particle size of 270 nm was mixed with 10% PVA solution at a mass percentage of 81:19 to prepare a slurry. The slurry was injected into the 3D printed morphological framework at a rate of 3 ml / s. The slurry was degreased at 320°C for 25 minutes and sintered at 1720°C for 62 minutes to obtain a through-hole ceramic matrix.
[0055] 2) Tungsten carbide powder was deposited on the surface of a porous ceramic matrix using a one-step carbonization method. Specifically, ammonium metatungstate and caramel were mixed at a molar ratio of 1:0.9 to prepare a solution with a concentration of 0.006 mol / L. The solution was prepared into a colloid at 105 °C for 12 hours and then injected into the pores inside the porous ceramic matrix. The matrix was then treated at 1230 °C for 50 minutes. Finally, a 61:39 cobalt-nickel binary alloy was melt-infiltrated into the pores inside the deposited ceramic matrix at 1540 °C for 14 minutes using a melt-infiltration method, resulting in a periodic lattice-structured tough ceramic composite material.
[0056] Example 2
[0057] 1) Using solid paraffin wax as raw material and a face-centered cubic ball-and-stick model as a template, a 3D printing method was used to prepare the morphological framework. The diameter of the ball in the framework was 0.18 mm, the diameter of the stick was 0.05 mm, the side length of the unit cell was 3.2 mm, and the number of unit cells and the size of the framework were determined according to specific size requirements. Then, silicon nitride powder with an average particle size of 310 nm was mixed with 10% PVA solution at a mass percentage of 86:14 to prepare a slurry. The slurry was injected into the 3D printed morphological framework at a rate of 5 ml / s. The slurry was degreased at 350 °C for 32 minutes and sintered at 1720 °C for 71 minutes to obtain a through-hole ceramic matrix.
[0058] 2) Tungsten carbide powder was deposited on the surface of a porous ceramic matrix using a one-step carbonization method. Specifically, ammonium metatungstate and caramel were mixed in a molar ratio of 1:1.3 to prepare a solution with a concentration of 0.011 mol / L. The solution was prepared into a colloid at 115°C for 16 hours and then injected into the pores inside the porous ceramic matrix. The matrix was then treated at 1230°C for 58 minutes. Finally, a 70:30 cobalt-nickel binary alloy was melt-infiltrated into the pores inside the deposited ceramic matrix at 1580°C for 14 minutes using a melt-infiltration method, resulting in a periodic lattice-structured tough ceramic composite material.
[0059] Example 3
[0060] 1) Using solid paraffin wax as raw material and a ball-and-stick model with a body-centered cubic structure as a template, a 3D printing method was used to prepare the morphological framework. The diameter of the ball in the framework was 0.15 mm, the diameter of the stick was 0.04 mm, the side length of the unit cell was 2.9 mm, and the number of unit cells and the size of the framework were determined according to specific size requirements. Then, silicon carbide powder with an average particle size of 290 nm was mixed with 10% PVA solution at a mass percentage of 84:16 to prepare a slurry. The slurry was injected into the 3D printed morphological framework at a rate of 4 ml / s. The slurry was degreased at 340℃ for 29 minutes and sintered at 1740℃ for 67 minutes to obtain a through-hole ceramic matrix.
[0061] 2) Tungsten carbide powder was deposited on the surface of a porous ceramic matrix using a one-step carbonization method. Specifically, ammonium metatungstate and caramel were mixed in a molar ratio of 1:1.1 to prepare a solution with a concentration of 0.009 mol / L. The solution was prepared into a colloid at 110°C for 14 hours and then injected into the pores inside the porous ceramic matrix. The matrix was then treated at 1250°C for 54 minutes. Finally, a 68:32 cobalt-nickel binary alloy was melt-infiltrated into the pores inside the deposited ceramic matrix at 1560°C for 17 minutes using a melt-infiltration method, resulting in a periodic lattice-structured tough ceramic composite material.
[0062] Example 4
[0063] 1) Using solid paraffin wax as raw material and a face-centered cubic ball-and-stick model as a template, a 3D printing method was used to prepare the morphological framework. The diameter of the ball in the framework was 0.17 mm, the diameter of the stick was 0.05 mm, the side length of the unit cell was 3.2 mm, and the number of unit cells and the size of the framework were determined according to specific size requirements. Then, silicon nitride powder with an average particle size of 310 nm was mixed with 10% PVA solution at a mass percentage of 85:15 to prepare a slurry. The slurry was injected into the 3D printed morphological framework at a rate of 5 ml / s. The slurry was degreased at 350 °C for 32 minutes and sintered at 1720 °C for 69 minutes to obtain a through-hole ceramic matrix.
[0064] 2) Tungsten carbide powder was deposited on the surface of a porous ceramic matrix using a one-step carbonization method. Specifically, ammonium metatungstate and caramel were mixed in a molar ratio of 1:1.2 to prepare a solution with a concentration of 0.01 mol / L. The solution was prepared into a colloid at 115°C for 12 hours and then injected into the pores inside the porous ceramic matrix. The matrix was then treated at 1260°C for 50 minutes. Finally, a 69:31 cobalt-nickel binary alloy was melt-infiltrated into the pores inside the deposited ceramic matrix at 1580°C for 14 minutes using a melt-infiltration method, resulting in a periodic lattice-structured tough ceramic composite material.
[0065] The performance parameters of the tough ceramic composites prepared in Examples 1-4 are shown in Table 1:
[0066] Table 1
[0067]
[0068] As can be seen from the table above, the tough ceramic composite material prepared by this invention has a periodic lattice configuration, and the fracture toughness of the material is greater than or equal to 23.6 MPa·m. 1 / 2 The bending strength is greater than or equal to 1530 MPa, the compressive strength is greater than or equal to 3720 MPa, and the relative density is greater than or equal to 99.3%.
[0069] Example 5
[0070] 1) Using solid paraffin wax as raw material and a ball-and-stick model with a body-centered cubic structure as a template, a 3D printing method was used to prepare the morphological framework. The diameter of the ball in the framework was 0.14 mm, the diameter of the stick was 0.035 mm, the side length of the unit cell was 2.8 mm, and the number of unit cells and the size of the framework were determined according to specific size requirements. Then, silicon carbide powder with an average particle size of 280 nm was mixed with 10% PVA solution at a mass percentage of 82:18 to prepare a slurry. The slurry was injected into the 3D printed morphological framework at a rate of 3.5 ml / s. The slurry was degreased at 330 °C for 26 minutes and sintered at 1730 °C for 65 minutes to obtain a through-hole ceramic matrix.
[0071] 2) Tungsten carbide powder was deposited on the surface of a porous ceramic matrix using a one-step carbonization method. Specifically, ammonium metatungstate and caramel were mixed in a molar ratio of 1:1 to prepare a solution with a concentration of 0.007 mol / L. The solution was prepared into a colloid at 108 °C for 13 hours and then injected into the pores inside the porous ceramic matrix. The matrix was then treated at 1240 °C for 52 minutes. Finally, a 62:38 cobalt-nickel binary alloy was melt-infiltrated into the pores inside the deposited ceramic matrix at 1550 °C for 15 minutes using a melt-infiltration method, resulting in a periodic lattice-structured tough ceramic composite material.
[0072] Example 6
[0073] 1) Using solid paraffin wax as raw material and a face-centered cubic ball-and-stick model as a template, a 3D printing method was used to prepare the morphological framework. The diameter of the ball in the framework was 0.15 mm, the diameter of the stick was 0.045 mm, the side length of the unit cell was 3.1 mm, and the number of unit cells and the size of the framework were determined according to specific size requirements. Then, silicon nitride powder with an average particle size of 300 nm was mixed with 10% PVA solution at a mass percentage of 85:15 to prepare a slurry. The slurry was injected into the 3D printed morphological framework at a rate of 4.5 ml / s. The slurry was degreased at 345℃ for 31 minutes and sintered at 1770℃ for 70 minutes to obtain a through-hole ceramic matrix.
[0074] 2) Tungsten carbide powder was deposited on the surface of a porous ceramic matrix using a one-step carbonization method. Specifically, ammonium metatungstate and caramel were mixed in a molar ratio of 1:1.2 to prepare a solution with a concentration of 0.010 mol / L. The solution was prepared into a colloid at 110°C for 15 hours and then injected into the pores inside the porous ceramic matrix. The matrix was then treated at 1250°C for 57 minutes. Finally, a 69:31 cobalt-nickel binary alloy was melt-infiltrated into the pores inside the deposited ceramic matrix at 1570°C for 19 minutes using a melt-infiltration method, resulting in a periodic lattice-structured tough ceramic composite material.
[0075] Example 7
[0076] 1) Using solid paraffin wax as raw material and a ball-and-stick model with a body-centered cubic structure as a template, a 3D printing method was used to prepare the morphological framework. The diameter of the ball in the framework was 0.16 mm, the diameter of the stick was 0.045 mm, the side length of the unit cell was 3.0 mm, and the number of unit cells and the size of the framework were determined according to specific size requirements. Then, silicon carbide powder with an average particle size of 300 nm was mixed with 10% PVA solution at a mass percentage of 85:15 to prepare a slurry. The slurry was injected into the 3D printed morphological framework at a rate of 4.6 ml / s. The slurry was degreased at 330℃ for 30 minutes and sintered at 1745℃ for 65 minutes to obtain a through-hole ceramic matrix.
[0077] 2) Tungsten carbide powder was deposited on the surface of a porous ceramic matrix using a one-step carbonization method. Specifically, ammonium metatungstate and caramel were mixed in a molar ratio of 1:1.2 to prepare a solution with a concentration of 0.0095 mol / L. The solution was prepared into a colloid at 108°C for 15 hours and then injected into the pores inside the porous ceramic matrix. The matrix was then treated at 1240°C for 56 minutes. Finally, a 65:35 cobalt-nickel binary alloy was melt-infiltrated into the pores inside the deposited ceramic matrix at 1565°C for 18 minutes using a melt-infiltration method, resulting in a periodic lattice-structured tough ceramic composite material.
[0078] Example 8
[0079] 1) Using solid paraffin wax as raw material and a face-centered cubic ball-and-stick model as a template, a 3D printing method was used to prepare the morphological framework. The diameter of the ball in the framework was 0.175 mm, the diameter of the stick was 0.035 mm, the side length of the unit cell was 3.0 mm, and the number of unit cells and the size of the framework were determined according to specific size requirements. Then, silicon nitride powder with an average particle size of 305 nm was mixed with 10% PVA solution at a mass percentage of 83:17 to prepare a slurry. The slurry was injected into the 3D printed morphological framework at a rate of 4.6 ml / s. The slurry was degreased at 330℃ for 31 minutes and sintered at 1700℃ for 65 minutes to obtain a through-hole ceramic matrix.
[0080] 2) Tungsten carbide powder was deposited on the surface of a porous ceramic matrix using a one-step carbonization method. Specifically, ammonium metatungstate and caramel were mixed in a molar ratio of 1:1.25 to prepare a solution with a concentration of 0.007 mol / L. The solution was prepared into a colloid at 114 °C for 13 hours and then injected into the pores inside the porous ceramic matrix. The matrix was then treated at 1250 °C for 52 minutes. Finally, a 64:36 cobalt-nickel binary alloy was melt-infiltrated into the pores inside the deposited ceramic matrix at 1570 °C for 16 minutes using a melt-infiltration method, resulting in a periodic lattice-structured tough ceramic composite material.
[0081] The tough ceramic composites prepared in Examples 5-8 were subjected to performance tests. The results showed that the obtained tough ceramic composites had a periodic lattice configuration and a fracture toughness greater than or equal to 23.6 MPa·m. 1 / 2 The flexural strength is greater than or equal to 1530 MPa, the compressive strength is greater than or equal to 3720 MPa, and the relative density is greater than or equal to 99.3%. This means that the overall toughness and strength of the ceramic are improved.
[0082] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.
Claims
1. A method for preparing a periodic lattice-structured tough ceramic composite material, characterized in that, Includes the following steps: Using solid paraffin as raw material, a body-centered cubic or face-centered cubic framework is prepared by 3D printing, and a through-hole ceramic matrix is prepared on the body-centered cubic or face-centered cubic framework by injection molding. Tungsten carbide was deposited on the surface of a through-hole ceramic matrix using a one-step carbonization method, and a metal binder phase was filled into the through-hole ceramic matrix using a melt infiltration method to obtain a periodic lattice configuration tough ceramic composite material. The method of depositing tungsten carbide on the surface of a porous ceramic substrate using a one-step carbide deposition method includes: Ammonium metatungstate and caramel were mixed into a solution, and a colloid was prepared at 105~115℃ for 12~16 hours. The prepared colloid is injected into the pores inside the through-hole ceramic matrix and then treated at 1230~1260℃ for 50~58 minutes.
2. The method for preparing the periodic lattice-structured tough ceramic composite material as described in claim 1, characterized in that, The body-centered cubic or face-centered cubic configuration frame adopts a ball-and-stick model, specifically a template-printed configuration frame.
3. The method for preparing the periodic lattice-structured tough ceramic composite material as described in claim 2, characterized in that, The diameter of the sphere in the template printing configuration frame is 0.13~0.18 mm, the diameter of the rod is 0.03~0.05 mm, and the side length of the unit cell is 2.7~3.2 mm.
4. The method for preparing the periodic lattice-structured tough ceramic composite material as described in claim 1, characterized in that, The preparation of a through-hole ceramic matrix on a body-centered cubic or face-centered cubic framework using injection molding includes: Silicon carbide or silicon nitride powder is mixed with PVA solution to form a slurry, which is then injected into a 3D printed framework. The slurry is degreased at 320-350℃ for 25-32 minutes and then sintered at 1720-1770℃ for 62-71 minutes to obtain a through-hole ceramic matrix.
5. The method for preparing the periodic lattice-structured tough ceramic composite material as described in claim 4, characterized in that, The average particle size of the silicon carbide or silicon nitride powder is 270-310 nanometers; the mass concentration of the PVA solution is 10%.
6. The method for preparing the periodic lattice-structured tough ceramic composite material as described in claim 4, characterized in that, The silicon carbide or silicon nitride powder is mixed with the PVA solution at a mass percentage of (81~86):(14~19); the injection rate is 3~5 ml per second.
7. The periodic lattice-structured tough ceramic composite material and its preparation method as described in claim 1, characterized in that, Ammonium metatungstate and caramel are mixed in a molar ratio of 1:(0.9~1.3) to prepare a solution with a concentration of 0.006~0.011 mol / L.
8. The periodic lattice-structured tough ceramic composite material and its preparation method as described in claim 1, characterized in that, The method of filling a porous ceramic matrix with a metallic binder phase by melt infiltration includes: A cobalt-nickel binary alloy with a mass percentage of (61-70):(30-39) was infiltrated into the pores inside a ceramic matrix using a melting infiltration method at 1540-1580℃ for 14-19 minutes.
9. A periodic lattice configuration tough ceramic composite material, characterized in that, The tough ceramic composite material is prepared by the preparation method according to any one of claims 1 to 8; the prepared tough ceramic composite material has a periodic lattice configuration and the fracture toughness of the material is greater than or equal to 23.6 MPa·m. 1 / 2 The bending strength is greater than or equal to 1530 MPa, the compressive strength is greater than or equal to 3720 MPa, and the relative density is greater than or equal to 99.3%.