Ceramic composite material and method for producing the same

Abstract

The application relates to a ceramic composite material and a preparation method thereof, and relates to the technical field of ceramic materials. The technical problem solved is how to improve the toughness and bending strength of the ceramic material. The main technical scheme adopted is that the preparation method of the ceramic composite material comprises the following steps: step 1): preparing a ceramic piece; wherein an internal gap to be filled or to be filled is reserved in the ceramic piece; the gap is in a spatial continuous lattice structure; step 2): filling or filling a metal material for toughening into the gap in the spatial continuous lattice structure of the ceramic piece to obtain a ceramic piece containing the metal material; and step 3): performing hot isostatic pressing treatment on the ceramic piece containing the metal material to obtain the ceramic composite material. The ceramic composite material prepared by the application has the characteristics of high strength and high toughness, and promotes the further application of the ceramic material in the fields of aviation and aerospace.

Description

Technical Field

[0001] This invention relates to the field of ceramic materials technology, and in particular to a ceramic composite material and its preparation method. Background Technology

[0002] Advanced ceramic materials, as an important part of new materials, have become key materials for the development of many high-tech fields. Ceramic materials can be divided into two main categories according to their properties and applications: structural ceramic materials and functional ceramic materials. Structural ceramic materials possess superior properties compared to metals and polymers, including high strength, high hardness, high wear resistance, high modulus, high temperature resistance, and corrosion resistance. Functional ceramic materials exhibit excellent functional properties such as acoustic, optical, electrical, superconducting, and biocompatibility.

[0003] With the rapid development of the national economy, higher requirements have been placed on the performance of ceramic materials, especially their toughness and tensile strength.

[0004] However, as ceramic materials are ionic or covalently bonded chemicals, they possess high compressive strength but extremely poor toughness, deformation capacity, and flexural strength. This significantly hinders their practical application and has become a bottleneck in their development and application. Therefore, improving the toughness and flexural strength of ceramic materials is a major scientific challenge facing the field of ceramic materials. Summary of the Invention

[0005] In view of this, the present invention provides a ceramic composite material and its preparation method, the main purpose of which is to improve the toughness and flexural strength of ceramic materials.

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

[0007] On one hand, embodiments of the present invention provide a method for preparing a ceramic composite material, wherein the method for preparing the ceramic composite material includes the following steps:

[0008] Step 1): Prepare a ceramic part; wherein, the interior of the ceramic part has a pre-reserved gap for pouring or filling; the gap has a spatial continuous lattice structure;

[0009] Step 2): Inject or fill the gaps in the spatial continuous lattice structure of the ceramic part with the toughening metal material to obtain a ceramic part containing the metal material;

[0010] Step 3): The ceramic part containing the metal material is subjected to hot isostatic pressing to obtain a ceramic composite material.

[0011] Preferably, in step 1), the ceramic raw material is prepared into an additive part using additive manufacturing technology; wherein, the additive part has gaps with a spatial continuous lattice structure reserved inside; the additive part is subjected to high-temperature sintering treatment, low-temperature sintering treatment, and hot isostatic pressing treatment to obtain a ceramic part.

[0012] Preferably, in step 1), the additive manufacturing technology is selected from any one of stereolithography additive manufacturing technology, binder spraying additive manufacturing technology, selective laser sintering additive manufacturing technology, and direct ink writing additive manufacturing technology.

[0013] Preferably, in step 1), the material of the ceramic part includes one or more of alumina, zirconium oxide, silicon carbide, and silicon nitride.

[0014] Preferably, the high-temperature sintering treatment is performed at a temperature of 1850℃-2000℃ for 1-2 hours.

[0015] Preferably, the temperature of the low-temperature sintering treatment is 1400℃-1700℃, and the time of the low-temperature sintering treatment is 4h-6h.

[0016] Preferably, in step 2): the temperature of the hot isostatic pressing (HIP) treatment is 1800℃-2000℃, the pressure of the HIP treatment is 140MPa-160MPa, and the time of the HIP treatment is 2h-4h; during the HIP treatment, the pressure of the inert gas introduced is 10 MPa. -2 Pa-10 -3 Pa.

[0017] Preferably, in step 2), the toughening metal material includes any one of titanium alloy, high-temperature alloy, tungsten alloy, molybdenum alloy, niobium alloy, and high-entropy alloy.

[0018] Preferably, in step 2), liquid metal material for toughening is injected into the gaps of the ceramic part in the spatially continuous lattice structure to obtain a ceramic part containing metal material.

[0019] Preferably, in step 3):

[0020] The ceramic part containing the metal material is subjected to a first hot isostatic pressing treatment and a second hot isostatic pressing treatment to obtain the ceramic material.

[0021] The first hot isostatic pressing (HIP) treatment is performed at a temperature of 850℃-1050℃, at a pressure of 160MPa-180MPa, and for a time of 1-2 hours. During the first HIP treatment, the pressure of the inert gas introduced is 10 MPa. -2 Pa-10-3 Pa; After the first hot isostatic pressing treatment, cooling is performed by gas quenching;

[0022] The second hot isostatic pressing (HIP) treatment is performed at a temperature of 800℃-950℃, at a pressure of 180MPa-200MPa, and for a time of 2-4 hours. During the second HIP treatment, the inert gas introduced is pressurized to a pressure of 10 MPa. -2 Pa-10 -3 Pa.

[0023] Preferably, in step 3):

[0024] When the metal material is a refractory alloy, the temperature of the first hot isostatic pressing treatment is 950℃-1050℃; the temperature of the second hot isostatic pressing treatment is 900℃-950℃.

[0025] When the metal material is a non-refractory alloy, the temperature of the first hot isostatic pressing treatment is 850℃-900℃; the temperature of the second hot isostatic pressing treatment is 800℃-850℃.

[0026] The refractory alloys include tungsten alloys, molybdenum alloys, niobium alloys, and tantalum alloys.

[0027] Preferably, in step 2), powdered metal material is filled into the gaps of the ceramic part in the spatial continuous lattice structure to obtain a ceramic part containing metal material.

[0028] Preferably, in step 3):

[0029] The ceramic part containing the metal material is subjected to a first hot isostatic pressing treatment and a second hot isostatic pressing treatment to obtain the ceramic material.

[0030] The first hot isostatic pressing (HIP) treatment is performed at a temperature of 920-1250℃, at a pressure of 160MPa-180MPa, and for a duration of 1-2 hours. During the first HIP treatment, the pressure of the inert gas introduced is 10 MPa. -2 -10 -3 Pa; After the first hot isostatic pressing treatment, cooling is performed by gas quenching;

[0031] The second hot isostatic pressing (HIP) treatment is performed at a temperature of 850-1100℃, a pressure of 180MPa-200MPa, and a time of 2-4 hours. During the second HIP treatment, the inert gas pressure is 10 MPa. -2 -10 -3 Pa.

[0032] Preferably, in step 3):

[0033] When the metal material is a refractory alloy, the temperature of the first hot isostatic pressing treatment is 920℃-1050℃; the temperature of the second hot isostatic pressing treatment is 1050℃-1250℃.

[0034] When the metal material is a non-refractory alloy, the temperature of the first hot isostatic pressing treatment is 850℃-950℃; the temperature of the second hot isostatic pressing treatment is 1000℃-1100℃.

[0035] The refractory alloys include tungsten alloys, molybdenum alloys, niobium alloys, and tantalum alloys.

[0036] On the other hand, embodiments of the present invention provide a ceramic composite material, wherein the ceramic composite material is prepared by the preparation method of the ceramic composite material described in any one of the above claims; wherein the ceramic composite material includes a ceramic matrix and a biomimetic structure with continuous metal space located inside the ceramic matrix.

[0037] Compared with the prior art, the ceramic composite material and its preparation method of the present invention have at least the following beneficial effects:

[0038] This invention provides a method for preparing a ceramic composite material, mainly including the following steps: Step 1): Preparing a ceramic part; wherein, the interior of the ceramic part has a pre-reserved continuous lattice structure to be infused or filled; Step 2): Infusing or filling the gaps in the continuous lattice structure of the ceramic part with a toughening metal material to obtain a ceramic part containing a metal material; Step 3): Performing hot isostatic pressing on the ceramic part containing the metal material to obtain a ceramic composite material. The above scheme should be explained as follows: This invention achieves the composite of ceramic and metal materials, utilizing the metal material to toughen the ceramic material, significantly improving the toughness and flexural strength of the ceramic material (wherein, the flexural strength is increased by more than 50 MPa, and the fracture toughness is increased by more than 50% compared to traditional ceramic materials). The principle behind this invention's improvement in toughness and flexural strength is as follows: Due to the nature of its chemical bonds (ionic / covalent bonds) and crystal structure (covalent bonds make dislocation movement difficult), ceramic materials have poor flexural strength, but excellent compressive strength. Metallic materials exhibit non-directional and unsaturated metallic bonds, relatively gentle interatomic bonding forces, and numerous dislocation slip systems in their crystals (e.g., face-centered cubic metals have 12 slip systems). At room temperature, dislocations can slip under low stress, leading to plastic deformation. Furthermore, when a metal is bent, stress concentration at defects is released through dislocation movement and grain slip, "passivating" crack tips and preventing rapid propagation. Therefore, metals possess high bending strength and exhibit ductile fracture. Thus, the solution of this invention retains the excellent compressive strength of ceramic materials while using metallic materials to improve toughness and bending strength (to withstand bending loads).

[0039] Furthermore, the material design in this invention is very flexible, allowing for the selection of different ceramic materials and toughening metal materials for different usage environments and performance requirements, so that the characteristics and advantages of each material coexist. Moreover, by flexibly changing the structure and distribution of each component material, the performance requirements of different parts can be met.

[0040] The above description is merely an overview of the technical solution of the present invention. In order to better understand the technical means of the present invention and to implement it in accordance with the contents of the specification, the preferred embodiments of the present invention are described in detail below with reference to the accompanying drawings. Attached Figure Description

[0041] Figure 1 This is a schematic diagram of the ceramic composite material prepared in Example 1;

[0042] Figure 2 This is a schematic diagram of the digital model of the metal space continuous lattice structure of the ceramic composite material prepared in Example 1;

[0043] Figure 3This is a schematic diagram of the digital model of the metal space continuous lattice structure of the ceramic composite material prepared in Example 2;

[0044] Figure 4 This is a schematic diagram of the digital model of the metal space continuous lattice structure of the ceramic composite material prepared in Example 3;

[0045] Figure 5 This is a schematic diagram of the digital model of the metal space continuous lattice structure of the ceramic composite material prepared in Example 4.

[0046] The reference numerals in the attached figures are as follows: 1. Ceramic material matrix; 2. Metal space continuous lattice structure. Detailed Implementation

[0047] To further illustrate the technical means and effects adopted by the present invention to achieve the intended purpose, the specific embodiments, structures, features, and effects according to the present invention will be described in detail below with reference to the accompanying drawings and preferred embodiments. In the following description, different "embodiments" or "embodiments" do not necessarily refer to the same embodiment. Furthermore, specific features, structures, or characteristics in one or more embodiments can be combined in any suitable form.

[0048] This invention provides a ceramic composite material and its preparation method, which utilizes a spatial continuous lattice structure to improve the toughness and flexural strength of the ceramic material, in order to meet the current demand in aerospace and other fields for ceramic materials with both high strength and high toughness, thereby achieving weight reduction and efficiency improvement and promoting the application of new ceramic materials.

[0049] The design concept of this invention is as follows: This invention proposes for the first time the preparation concept of "dual composite ceramic materials," organically combining the performance advantages of metallic and ceramic materials, and employing "composite materials + composite manufacturing" technology to prepare the required ceramic materials. This innovative structural design and material combination method gives this invention a significant advantage in improving the comprehensive performance of ceramic materials, providing a new solution for the demand for high-performance ceramic materials in fields such as aerospace.

[0050] The main features of this invention are as follows:

[0051] On one hand, embodiments of the present invention provide a method for preparing a ceramic composite material, wherein the method for preparing the ceramic composite material includes the following steps:

[0052] Step 1): Prepare a ceramic part; wherein, the interior of the ceramic part has reserved gaps for pouring or filling; the gaps are in the form of a continuous spatial lattice structure. The continuous spatial lattice structure typically refers to a structure with long-range translational symmetry, whose arrangement can be described by a continuous, infinitely extending mathematical lattice.

[0053] Among them, the structural characteristics used for the spatial continuous lattice structure can be selected according to the stress characteristics of the required ceramic parts.

[0054] In this step, additive manufacturing technology is used to prepare ceramic raw materials into additive parts with internally reserved spatial continuous lattice structure gaps; the additive parts are subjected to high-temperature sintering treatment, low-temperature sintering treatment, and hot isostatic pressing treatment to obtain ceramic parts.

[0055] Preferably, the additive manufacturing technology is selected from any one of stereolithography additive manufacturing technology, binder jet additive manufacturing technology, selective laser sintering additive manufacturing technology, and direct ink writing additive manufacturing technology.

[0056] Preferably, the ceramic component is made of one or more of alumina, zirconium oxide, silicon carbide, and silicon nitride.

[0057] The high-temperature sintering treatment is carried out at a temperature of 1850℃-2000℃ for 1-2 hours. This high-temperature sintering process achieves the purpose of solidification. After the high-temperature sintering treatment, the sample must be cooled to room temperature before proceeding to the next step.

[0058] The low-temperature sintering treatment is carried out at a temperature of 1400℃-1700℃ for 4-6 hours. This low-temperature sintering process aims to achieve homogenization. After sintering, the sample must be cooled to room temperature before proceeding to the next step.

[0059] The hot isostatic pressing (HIP) treatment is performed at a temperature of 1800℃-2000℃, at a pressure of 140MPa-160MPa, and for a duration of 2-4 hours. During the HIP treatment, the inert gas introduced is pressurized to a pressure of 10 MPa. -2 Pa-10 -3 Pa. The purpose of the hot isostatic pressing treatment here is to further eliminate internal defects such as pores and cracks; after the hot isostatic pressing treatment, the furnace is cooled to room temperature.

[0060] Step 2): Inject or fill the gaps in the spatially continuous lattice structure of the ceramic part with toughening metal material to obtain a ceramic part containing metal material.

[0061] In this step, the toughening metal material can be selected based on the operating temperature of the ceramic structural material. For example, the higher the operating temperature of the ceramic structural material, the higher the melting point of the toughening metal material.

[0062] Preferably, the toughening metal material is any one of titanium alloy, high-temperature alloy, tungsten alloy, molybdenum alloy, niobium alloy, and high-entropy alloy.

[0063] In this step, casting technology is used to pour liquid metal material for toughening into the gaps of the spatially continuous lattice structure of the ceramic part, resulting in a ceramic part containing metal material. Alternatively, powder metallurgy technology is used to fill powdered metal material into the gaps of the spatially continuous lattice structure of the ceramic part, resulting in a ceramic part containing metal material.

[0064] Step 3): The ceramic part containing the metal material is subjected to hot isostatic pressing to obtain the ceramic material.

[0065] Wherein, when step 2) uses casting technology, step 3) includes:

[0066] The ceramic part containing the metal material is subjected to a first hot isostatic pressing treatment and a second hot isostatic pressing treatment to obtain the ceramic material.

[0067] The first hot isostatic pressing (HIP) treatment is performed at a temperature of 850℃-1050℃, at a pressure of 160MPa-180MPa, and for a time of 1-2 hours. During the first HIP treatment, the pressure of the inert gas introduced is 10 MPa. -2 Pa-10 -3 Pa; After the first hot isostatic pressing treatment, cooling is performed by gas quenching;

[0068] The second hot isostatic pressing (HIP) treatment is performed at a temperature of 800℃-950℃, at a pressure of 180MPa-200MPa, and for a time of 2-4 hours. During the second HIP treatment, the inert gas introduced is pressurized to a pressure of 10 MPa. -2 Pa-10 -3 Pa.

[0069] Wherein, when the metal material is a refractory alloy, the temperature of the first hot isostatic pressing treatment is 950℃-1050℃; the temperature of the second hot isostatic pressing treatment is 900℃-950℃;

[0070] When the metal material is a non-refractory alloy, the temperature of the first hot isostatic pressing treatment is 850℃-900℃; the temperature of the second hot isostatic pressing treatment is 800℃-850℃.

[0071] The refractory alloys include tungsten alloys, molybdenum alloys, niobium alloys, and tantalum alloys.

[0072] In this step, the purpose of the first hot isostatic pressing (HIP) treatment is to control the grain size and prevent grain growth. The purpose of the second HIP treatment is to homogenize the microstructure and regulate its properties.

[0073] Wherein, when step 2) employs powder metallurgy technology, step 3) includes:

[0074] The ceramic part containing the metal material is subjected to a first hot isostatic pressing treatment and a second hot isostatic pressing treatment to obtain the ceramic material.

[0075] The first hot isostatic pressing (HIP) treatment is performed at a temperature of 920-1250℃, at a pressure of 160MPa-180MPa, and for a duration of 1-2 hours. During the first HIP treatment, the pressure of the inert gas introduced is 10 MPa. -2 -10 -3 Pa; After the first hot isostatic pressing treatment, cooling is performed by gas quenching;

[0076] The second hot isostatic pressing (HIP) treatment is performed at a temperature of 850-1100℃, a pressure of 180MPa-200MPa, and a time of 2-4 hours. During the second HIP treatment, the inert gas pressure is 10 MPa. -2 -10 -3 Pa.

[0077] Wherein, when the metal material is a refractory alloy, the temperature of the first hot isostatic pressing treatment is 920℃-1050℃; the temperature of the second hot isostatic pressing treatment is 1050℃-1250℃;

[0078] When the metal material is a non-refractory alloy, the temperature of the first hot isostatic pressing treatment is 850℃-950℃; the temperature of the second hot isostatic pressing treatment is 1000℃-1100℃.

[0079] The refractory alloys include tungsten alloys, molybdenum alloys, niobium alloys, and tantalum alloys.

[0080] In this step, the purpose of the first hot isostatic pressing (HIP) treatment is to control the grain size and prevent grain growth. The purpose of the second HIP treatment is to homogenize the microstructure and regulate its properties.

[0081] Regarding the above-described solution of the present invention, at least the following advantages exist:

[0082] 1): The solution of the present invention makes the design of ceramic composite materials very flexible. Different toughening materials can be selected for different usage environments and performance requirements, so that the characteristics and advantages of ceramic materials and metal materials coexist. Moreover, by flexibly changing the structure and distribution of each component material, the performance requirements of different parts of the material can be met.

[0083] 2): The solution of the present invention can effectively improve the comprehensive mechanical properties of ceramic materials and overcome the problem of insufficient toughness of existing ceramic materials.

[0084] 3): The present invention is the first to achieve the preparation of a ceramic composite material that combines high strength and high toughness.

[0085] 4): The solution of this invention breaks through the technical bottleneck of improving the comprehensive performance of ceramic materials in the current aerospace and other fields, and promotes the further application of ceramic materials in aerospace and other fields.

[0086] The present invention will be further illustrated below with specific embodiments:

[0087] Example 1

[0088] This embodiment prepares a ceramic composite material, including the following steps:

[0089] Step 1): Selective laser sintering technology is used to prepare ceramic raw materials (Al2O3 powder, particle size of 10-150μm) into additive parts, and gaps with a spatial continuous lattice structure to be injected are reserved inside; wherein, the spatial continuous lattice structure is a rhombic dodecahedral structure.

[0090] The additive manufacturing process involved high-temperature sintering, low-temperature sintering, and hot isostatic pressing (HIP) to obtain ceramic parts. The high-temperature sintering was performed at 1850℃ for 2 hours (followed by cooling to room temperature before low-temperature sintering). The low-temperature sintering was performed at 1450℃ for 5 hours (followed by cooling to room temperature before HIP). The HIP was performed at 1800℃ for 3 hours at a pressure of 150 MPa. During HIP, an inert gas was introduced at a pressure of 3 × 10⁻⁶ MPa. -3 Pa; after hot isostatic pressing, it is cooled with the furnace.

[0091] Step 2): Using casting technology, liquid tungsten alloy for toughening is poured into the gaps of the spatially continuous lattice structure inside the ceramic part to obtain a ceramic part containing metal material.

[0092] Step 3): The ceramic part containing the metal material is subjected to a first hot isostatic pressing treatment and a second hot isostatic pressing treatment in sequence to obtain a ceramic composite material with high toughness.

[0093] The first hot isostatic pressing (HIP) treatment was performed at a temperature of 1050℃, a pressure of 175 MPa, a duration of 2 hours, and an inert gas pressure of 5 × 10⁻⁶ MPa. -3Pa. After the first hot isostatic pressing treatment, cooling is performed by gas quenching.

[0094] The second hot isostatic pressing (HIP) treatment was performed at a temperature of 930℃, a pressure of 200 MPa, and a time of 2.5 h. The pressure of the inert gas introduced during the HIP treatment was 3 × 10⁻⁶ MPa. -3 Pa. After the second hot isostatic pressing treatment, cooling is performed using furnace cooling.

[0095] Figure 1 This is a schematic diagram of the ceramic composite material prepared in this embodiment, which includes a ceramic material matrix 1 and a continuous metal space lattice structure 2 located inside the ceramic material matrix 1.

[0096] Figure 2 A schematic diagram of a digital model of a continuous metal lattice structure inside a ceramic composite material.

[0097] In this embodiment, the ceramic composite material has a continuous biomimetic structure (tungsten alloy) with metallic space inside. The use of tungsten alloy as a toughening material effectively improves the toughness and flexural strength of the ceramic composite material. Using Al2O3 ceramic as the matrix material ensures the high strength, high hardness, high wear resistance, high modulus, high temperature resistance, and corrosion resistance of the ceramic composite material.

[0098] The performance indicators of the ceramic composite material prepared in this embodiment are as follows: flexural strength of 332 MPa and fracture toughness of 10.27 MPa·m. 1 / 2 Compared with traditional Al2O3 ceramic materials (bending strength of 273 MPa, fracture toughness of 2.26 MPa·m), 1 / 2 Compared to the previous method, the ceramic composite material prepared in this embodiment exhibits significantly improved flexural strength, fracture toughness, and other properties.

[0099] Example 2

[0100] This embodiment prepares a ceramic composite material, including the following steps:

[0101] Step 1): Using binder spraying technology, ceramic raw materials (ZrO2 powder, particle size 53~150μm) are used to prepare additive parts, and gaps with a spatial continuous lattice structure to be injected are reserved inside them; wherein, the spatial continuous lattice structure is a gradient structure.

[0102] The additive manufacturing process involved high-temperature sintering, low-temperature sintering, and hot isostatic pressing (HIP) to obtain ceramic parts. The high-temperature sintering was performed at 1950℃ for 1.5 hours (after which the parts were cooled to room temperature before low-temperature sintering). The low-temperature sintering was performed at 1500℃ for 4.5 hours (after which the parts were cooled to room temperature before HIP). The HIP was performed at 1900℃ at 160 MPa for 2.5 hours; during HIP, an inert gas was introduced at a pressure of 5 × 10⁻⁶ MPa. -3 Pa; after hot isostatic pressing, it is cooled with the furnace.

[0103] Step 2): Using casting technology, liquid niobium alloy for toughening is poured into the gaps of the ceramic part, which has a spatial continuous lattice structure, to obtain a ceramic part containing metal material.

[0104] Step 3): The ceramic part containing the metal material is subjected to a first hot isostatic pressing treatment and a second hot isostatic pressing treatment in sequence to obtain a ceramic composite material with high toughness.

[0105] The first hot isostatic pressing (HIP) treatment was performed at a temperature of 1000℃, a pressure of 180 MPa, a time of 1.5 h, and an inert gas pressure of 1 × 10⁻⁶ during the first HIP treatment. -3 Pa. After the first hot isostatic pressing treatment, cooling is performed by gas quenching.

[0106] The temperature of the second hot isostatic pressing (HIP) treatment was 950℃, the pressure was 195MPa, the time was 2 hours, and the pressure of the inert gas introduced during the HIP treatment was 3×10⁻⁶. -3 Pa. After the second hot isostatic pressing treatment, cooling is performed using furnace cooling.

[0107] Figure 3 A schematic diagram of a digital model of a continuous metal lattice structure inside a ceramic composite material.

[0108] In this embodiment, the ceramic composite material has a continuous biomimetic structure (niobium alloy) with metallic space inside. The use of niobium alloy as a toughening material effectively improves the toughness and flexural strength of the ceramic composite material. Using ZrO2 ceramic as the matrix material ensures the high strength, high hardness, high wear resistance, high modulus, high temperature resistance, and corrosion resistance of the ceramic composite material.

[0109] The performance indicators of the ceramic composite material prepared in this embodiment are as follows: flexural strength of 743 MPa and fracture toughness of 13.03 MPa·m.1 / 2 Compared with traditional ZrO2 ceramic materials (bending strength of 610 MPa, fracture toughness of 2.98 MPa·m), 1 / 2 Compared to the previous method, the ceramic composite material prepared in this embodiment exhibits significantly improved flexural strength, fracture toughness, and other properties.

[0110] Example 3

[0111] This embodiment prepares a ceramic composite material, including the following steps:

[0112] Step 1): Selective laser sintering additive manufacturing technology is used to prepare additive parts from ceramic raw materials (Si3N4 powder, particle size of 10-150μm), and gaps with a spatial continuous lattice structure to be filled are reserved inside; wherein, the spatial continuous lattice structure is a three-period minimum surface structure.

[0113] The additive manufacturing process involved high-temperature sintering, low-temperature sintering, and hot isostatic pressing (HIP) to obtain ceramic parts. The high-temperature sintering was performed at 1900℃ for 2 hours (after which the parts were cooled to room temperature before low-temperature sintering). The low-temperature sintering was performed at 1430℃ for 6 hours (after which the parts were cooled to room temperature before HIP). The HIP was performed at 1950℃ for 160 MPa for 2.5 hours; during HIP, the inert gas pressure was 3 × 10⁻⁶ MPa. -3 Pa; after hot isostatic pressing, it is cooled with the furnace.

[0114] Step 3): Using powder metallurgy technology, high-temperature titanium alloy powder for toughening is injected into the gaps of the ceramic part in a spatial continuous lattice structure to obtain a ceramic part containing metal material.

[0115] Step 4): The ceramic part containing the metal material is subjected to a first hot isostatic pressing treatment and a second hot isostatic pressing treatment in sequence to obtain a ceramic composite material with high toughness.

[0116] The first hot isostatic pressing (HIP) treatment was performed at a temperature of 950℃, a pressure of 175 MPa, a time of 1.5 h, and an inert gas pressure of 2 × 10⁻⁶ during the first HIP treatment. -3 Pa. After the first hot isostatic pressing treatment, cooling is performed by gas quenching.

[0117] The temperature of the second hot isostatic pressing (HIP) treatment was 1050℃, the pressure was 200MPa, the time was 3 hours, and the pressure of the gas introduced during the HIP treatment was 5×10⁻⁶. -3Pa. After the second hot isostatic pressing treatment, cooling is performed using furnace cooling.

[0118] Figure 4 A schematic diagram of a digital model of a continuous metal lattice structure inside a ceramic composite material.

[0119] In this embodiment, the ceramic composite material has a continuous biomimetic structure (titanium alloy) with metallic space inside. The use of high-temperature titanium alloy as a toughening material effectively improves the toughness and flexural strength of the ceramic composite material. Using Si3N4 ceramic as the matrix material ensures the high strength, high hardness, high wear resistance, high modulus, high temperature resistance, and corrosion resistance of the ceramic composite material.

[0120] The performance indicators of the ceramic composite material prepared in this embodiment are as follows: flexural strength of 702 MPa and fracture toughness of 15.83 MPa·m. 1 / 2 Compared with traditional Si3N4 ceramic materials (bending strength of 613 MPa, fracture toughness of 7.49 MPa·m), 1 / 2 Compared to the previous method, the ceramic composite material prepared in this embodiment exhibits significantly improved flexural strength, fracture toughness, and other properties.

[0121] Example 4

[0122] This embodiment prepares a ceramic composite material, including the following steps:

[0123] Step 1): Using stereolithography, ceramic material (SiC powder, particle size 53-150μm) is used to prepare additive parts, and gaps with a spatial continuous lattice structure to be filled are reserved inside; wherein, the spatial continuous lattice structure is a regular hexahedral structure.

[0124] The additive manufacturing process involves high-temperature sintering, low-temperature sintering, and hot isostatic pressing (HIP) to obtain a ceramic part after HIP treatment. The high-temperature sintering temperature is 2000℃, and the sintering time is 1 hour (after high-temperature sintering, the part needs to be cooled to room temperature before low-temperature sintering). The low-temperature sintering temperature is 1650℃, and the sintering time is 6 hours (after low-temperature sintering, the part needs to be cooled to room temperature before HIP). The HIP treatment temperature is 1850℃, the HIP pressure is 155 MPa, and the HIP time is 3 hours. During the HIP process, the pressure of the inert gas introduced is 1 × 10⁻⁶ MPa. -3 Pa; after hot isostatic pressing, it is cooled with the furnace.

[0125] Step 2): Using powder metallurgy technology, high-entropy alloy powder (Ti0.3Zr0.3Hf0.3Fe0.05Ni0.05) is filled into the gaps of the ceramic part in a spatially continuous lattice structure to obtain a ceramic part containing metallic material.

[0126] Step 3): The ceramic part containing the metal material is subjected to a first hot isostatic pressing treatment and a second hot isostatic pressing treatment in sequence to obtain a ceramic composite material with high toughness.

[0127] The first hot isostatic pressing (HIP) treatment was performed at a temperature of 950℃, a pressure of 180MPa, a duration of 2 hours, and an inert gas pressure of 1×10⁻⁶ during the first HIP treatment. -3 Pa. After the first hot isostatic pressing treatment, cooling is performed by gas quenching.

[0128] The temperature of the second hot isostatic pressing (HIP) treatment was 1100℃, the pressure was 195 MPa, the time was 3 hours, and the pressure of the inert gas introduced during the HIP treatment was 3 × 10⁻⁶. -3 Pa. After the second hot isostatic pressing treatment, cooling is performed using furnace cooling.

[0129] Figure 5 A schematic diagram of a digital model of a continuous lattice structure of metal space inside a ceramic material.

[0130] In this embodiment, the ceramic material has an internal biomimetic structure of continuous metallic space (titanium alloy). The use of a high-entropy alloy as a toughening material effectively improves the toughness and flexural strength of the ceramic material. Using SiC ceramic as the matrix material ensures the ceramic material's high strength, high hardness, high wear resistance, high modulus, high temperature resistance, and corrosion resistance.

[0131] The ceramic material prepared in this embodiment has the following performance indicators: flexural strength of 217 MPa and fracture toughness of 9.21 MPa·m. 1 / 2 Compared with traditional SiC ceramic materials (bending strength of 146 MPa, fracture toughness of 3.77 MPa·m), 1 / 2 Compared to the previous method, the ceramic material prepared in this embodiment exhibits significantly improved flexural strength, fracture toughness, and other properties.

[0132] Example 5

[0133] This embodiment prepares a ceramic composite material, including the following steps:

[0134] Step 1): Selective laser sintering technology is used to prepare ceramic raw materials (Al2O3 powder, particle size of 10-150μm) into additive parts, and gaps with a spatial continuous lattice structure to be injected are reserved inside; wherein, the spatial continuous lattice structure is a rhombic dodecahedral structure.

[0135] The additive manufacturing parts were subjected to high-temperature sintering and low-temperature sintering to obtain ceramic parts. The high-temperature sintering temperature was 1850℃, and the sintering time was 2 hours (after high-temperature sintering, the parts needed to be cooled to room temperature before low-temperature sintering). The low-temperature sintering temperature was 1450℃, and the sintering time was 5 hours (after low-temperature sintering, the parts needed to be cooled to room temperature).

[0136] Step 2): Using casting technology, liquid tungsten alloy for toughening is poured into the gaps of the continuous lattice structure inside the ceramic part to obtain a ceramic part containing metal material.

[0137] Step 3): The ceramic part containing the metal material is subjected to hot isostatic pressing to obtain a ceramic composite material with high toughness.

[0138] The hot isostatic pressing (HIP) treatment was performed at a temperature of 1050℃, a pressure of 175MPa, a time of 2 hours, and a gas pressure of 5×10⁻⁶ during the HIP treatment. -3 Pa. After hot isostatic pressing, cooling is performed by gas quenching.

[0139] In this embodiment, the ceramic composite material has an internal continuous lattice structure of metal space (tungsten alloy). The use of tungsten alloy as a toughening material effectively improves the toughness of the ceramic composite material. Using Al2O3 ceramic as the matrix material ensures the high strength, high hardness, high wear resistance, high modulus, high temperature resistance, and corrosion resistance of the ceramic composite material.

[0140] The performance indicators of the ceramic composite material prepared in this embodiment are as follows: flexural strength of 298 MPa and fracture toughness of 6.87 MPa·m. 1 / 2 Compared with traditional Al2O3 ceramic materials (bending strength of 273 MPa, fracture toughness of 2.26 MPa·m), 1 / 2 Compared to the previous embodiment, the ceramic composite material prepared in this embodiment has significantly improved properties such as flexural strength and fracture toughness. However, compared to the ceramic composite material after multiple hot isostatic pressings, the performance in this embodiment is lower than that in Example 1.

[0141] Comparative Example 1

[0142] This comparative example uses Si3N4 powder as raw material and Y2O3 and Al2O3 as sintering aids. The ceramic raw material powder and sintering aids are mixed by mechanical ball milling, and a series of silicon nitride ceramic samples are prepared through subsequent processing. First, the resin monomer and photoinitiator are mixed in a certain proportion and stirred evenly in a high-speed planetary mixer at 400 r / min to obtain a photosensitive resin mixture. Second, the weighed sintering aid is added to the photosensitive resin mixture and stirred at 800 r / min for 10 minutes. Finally, the weighed silicon nitride powder and a certain proportion of dispersant are added to the mixture step by step, and stirred at 1000 r / min for 10 minutes after each addition. After all the powder is added, it is stirred at 1500 r / min for 30 minutes, finally obtaining a photocurable Si3N4 ceramic paste with a solid content.

[0143] Subsequently, a stereolithography ceramic printer was used for printing. The ceramic paste was placed in the hopper of the 3D printing equipment, and the printing parameters were adjusted to a layer thickness of 20 μm, a laser power of 240 mW, a scanning speed of 1700 mm / s, and a scanning spacing of 0.01, finally producing a Si3N4 ceramic sample green body.

[0144] Finally, a tubular vacuum furnace was used for sintering. Before sintering, heat treatment was used to remove organic components such as photocuring resin and dispersant from the photocured silicon nitride ceramic preform. After heat treatment, the silicon nitride preform was sintered at 1800℃ under a nitrogen atmosphere.

[0145] Comparative Example 1 uses the traditional Si3N4 ceramic material preparation process, and the prepared Si3N4 ceramic material has a flexural strength of 613 MPa and a fracture toughness of 7.49 MPa·m. 1 / 2 Compared with Comparative Example 1, the ceramic composite material prepared in Example 3 showed significantly improved flexural strength, fracture toughness, and other properties.

[0146] The above description is merely a partial representation of the embodiments of the present invention and should not be construed as limiting the scope of the invention. For those skilled in the art, the metal materials, spatial continuous lattice structures, ceramic matrix, and sintering processes used to enhance toughness can be adjusted and combined according to actual needs. Therefore, various other corresponding changes and modifications made based on the technical solutions and concepts of the present invention still fall within the scope of protection covered by the present invention.

Claims

1. A method for preparing a ceramic composite material, characterized in that, The preparation method of the ceramic composite material includes the following steps: Step 1): Preparing a ceramic part; wherein, the ceramic part has a pre-reserved gap for pouring; the gap has a spatial continuous lattice structure; wherein, additive manufacturing technology is used to prepare the ceramic raw material into an additive part; wherein, the additive part has a pre-reserved gap with a spatial continuous lattice structure; the additive part is subjected to high-temperature sintering, low-temperature sintering, and hot isostatic pressing to obtain the ceramic part; wherein, the material of the ceramic part includes one or more of alumina, zirconium oxide, silicon carbide, and silicon nitride; wherein, the high-temperature sintering temperature is 1850℃-2000℃, and the high-temperature sintering time is 1h-2h; wherein, the low-temperature sintering temperature is 1400℃-1700℃, and the low-temperature sintering time is 4h-6h; Step 2): Injecting liquid metal material for toughening into the gaps of the ceramic part in the spatially continuous lattice structure to obtain a ceramic part containing metal material; Step 3): The ceramic part containing the metal material is subjected to hot isostatic pressing to obtain a ceramic composite material; In step 3), the ceramic part containing the metal material undergoes a first hot isostatic pressing (HIP) treatment and a second HIP treatment to obtain the ceramic material. The temperature of the first HIP treatment is 850℃-1050℃, the pressure is 160MPa-180MPa, and the time is 1h-2h. During the first HIP treatment, the pressure of the inert gas introduced is 10 MPa. -2 Pa-10 -3 Pa; after the first hot isostatic pressing (HIP) treatment, cooling is performed by gas quenching; wherein, the temperature of the second HIP treatment is 800℃-950℃, the pressure of the second HIP treatment is 180MPa-200MPa, and the time of the second HIP treatment is 2h-4h; during the second HIP treatment, the pressure of the inert gas introduced is 10 MPa. -2 Pa-10 -3 Pa; wherein, when the metal material is a refractory alloy, the temperature of the first hot isostatic pressing treatment is 950℃-1050℃; the temperature of the second hot isostatic pressing treatment is 900℃-950℃; when the metal material is a non-refractory alloy, the temperature of the first hot isostatic pressing treatment is 850℃-900℃; the temperature of the second hot isostatic pressing treatment is 800℃-850℃; wherein, the refractory alloy includes tungsten alloy, molybdenum alloy, niobium alloy, and tantalum alloy.

2. The method for preparing the ceramic composite material according to claim 1, characterized in that, In step 1), the additive manufacturing technology is selected from any one of the following: stereolithography additive manufacturing technology, binder spraying additive manufacturing technology, selective laser sintering additive manufacturing technology, and direct ink writing additive manufacturing technology.

3. A method for preparing a ceramic composite material, characterized in that, The preparation method of the ceramic composite material includes the following steps: Step 1): Preparing a ceramic part; wherein the ceramic part has pre-reserved gaps to be filled; the gaps have a continuous spatial lattice structure; wherein the ceramic raw material is prepared into an additive part using additive manufacturing technology; wherein the additive part has pre-reserved gaps with a continuous spatial lattice structure; the additive part is subjected to high-temperature sintering, low-temperature sintering, and hot isostatic pressing to obtain the ceramic part; wherein the material of the ceramic part includes one or more of alumina, zirconium oxide, silicon carbide, and silicon nitride; wherein the high-temperature sintering temperature is 1850℃-2000℃, and the high-temperature sintering time is 1h-2h; wherein the low-temperature sintering temperature is 1400℃-1700℃, and the low-temperature sintering time is 4h-6h; Step 2): Fill the gaps in the spatially continuous lattice structure of the ceramic part with powdered metal material for toughening to obtain a ceramic part containing metal material; Step 3): The ceramic part containing the metal material is subjected to hot isostatic pressing to obtain a ceramic composite material; In step 3), the ceramic part containing the metal material undergoes a first hot isostatic pressing (HIP) treatment and a second HIP treatment to obtain the ceramic material. The temperature of the first HIP treatment is 920-1250℃, the pressure is 160MPa-180MPa, and the time is 1-2 hours. During the first HIP treatment, the pressure of the inert gas introduced is 10 MPa. -2 -10 -3 Pa; after the first hot isostatic pressing (HIP) treatment, cooling is performed by gas quenching; wherein, the temperature of the second HIP treatment is 850℃-1100℃, the pressure of the second HIP treatment is 180MPa-200MPa, and the time of the second HIP treatment is 2-4h; during the second HIP treatment, the pressure of the inert gas introduced is 10 MPa. -2 -10 -3 Pa; when the metal material is a refractory alloy, the temperature of the first hot isostatic pressing treatment is 920℃-1050℃; the temperature of the second hot isostatic pressing treatment is 1050℃-1250℃; when the metal material is a non-refractory alloy, the temperature of the first hot isostatic pressing treatment is 850℃-950℃; the temperature of the second hot isostatic pressing treatment is 1000℃-1100℃; wherein, the refractory alloy includes tungsten alloy, molybdenum alloy, niobium alloy, and tantalum alloy.

4. The method for preparing the ceramic composite material according to claim 3, characterized in that, In step 1), the additive manufacturing technology is selected from any one of the following: stereolithography additive manufacturing technology, binder spraying additive manufacturing technology, selective laser sintering additive manufacturing technology, and direct ink writing additive manufacturing technology.

5. A ceramic composite material, characterized in that, The ceramic composite material is prepared by the method for preparing the ceramic composite material according to any one of claims 1-4; wherein the ceramic composite material includes a ceramic matrix and a continuous metal space lattice structure located inside the ceramic matrix.

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