A method for preparing a high-performance alumina fiber reinforced ceramic matrix composite
By using an aqueous sol-gel process for magnesium aluminum spinel and a vacuum-assisted impregnation process, alumina fiber-reinforced magnesium aluminum spinel ceramic matrix composites were prepared, solving the problems of decreased mechanical properties at high temperatures and environmental unfriendliness. This enabled the preparation of high-performance and environmentally friendly composite materials suitable for applications in extreme environments.
Patent Information
- Application Number
- CN202411946402.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-27
- Publication Date
- 2025-12-16
- Estimated Expiration
- 2044-12-27
AI Technical Summary
Existing alumina fiber-reinforced alumina ceramic matrix composites exhibit decreased mechanical properties at high temperatures. Aerogel technology is costly and environmentally unfriendly, making it difficult to meet the requirements for wave transmission performance and chemical stability under extreme conditions.
Alumina fiber-reinforced magnesium aluminate spinel ceramic matrix composites were prepared by using magnesium aluminate spinel aqueous sol as a precursor and low-temperature sintering and vacuum-assisted impregnation processes to control grain growth and improve material density.
It improves the mechanical strength and wave transmission performance of materials under high temperature and extreme environments, reduces production costs, enhances the environmental friendliness and process controllability of materials, and is suitable for aerospace, military and other fields.
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Figure CN119797904B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of ceramic matrix composite material preparation, and particularly relates to a preparation method of high-performance alumina fiber reinforced ceramic matrix composite material. BACKGROUND
[0002] Ceramic matrix composites (CMCs) combine the high-temperature stability and wave transparency of ceramic materials, and significantly improve the mechanical strength and toughness of the material by introducing reinforcing bodies such as fibers or particles. This kind of material is particularly important in high-end industrial applications that require extreme temperature and chemical environment, especially in the fields of aerospace, energy, automobile and military, which can provide performance beyond traditional ceramics.
[0003] Magnesium aluminate spinel (MgAl2O4) is a highly heat-resistant ceramic material known for its cubic crystal structure, which contributes to its many excellent physical and chemical properties. With a high melting point (about 2100°C) and good thermal stability, magnesium aluminate spinel performs well in high-temperature applications, maintaining physical and chemical properties stable in long-term high-temperature environments. The thermal shock resistance of this material makes it less likely to break when subjected to rapid temperature changes, making it ideal for applications such as aerospace, furnace windows and high-temperature furnace linings. Magnesium aluminate spinel is highly chemically inert, remaining stable even in harsh chemical environments, and is not easily reacted with most acids and bases. This makes it an ideal material choice for chemical processing and high-temperature corrosion environments. In the field of electronics and communications, magnesium aluminate spinel has unique advantages in the manufacture of microwave wave-transparent devices and isolator devices due to its low dielectric constant and low dielectric loss. In addition, its transparency also makes it useful for the manufacture of certain optical devices, such as windows and lenses at high temperatures, especially in applications that require the material to have high transmittance in the infrared and ultraviolet ranges.
[0004] Alumina continuous fiber (ALC) is an excellent composite material component known for its high tensile strength and low volume saturation weight ratio, usually existing in the form of continuous fibers, providing better mechanical properties and corrosion resistance compared to carbon fiber materials. This fiber has an amorphous structure with very few internal voids, making it an ideal choice for manufacturing efficient thermoset composites. In addition to excellent mechanical properties and corrosion resistance, ALC also exhibits excellent high-temperature resistance, maintaining structural and functional stability in extreme high-temperature environments of 1000 to 1200°C. In addition, alumina fiber also has good wave-transparent performance, especially suitable for high-temperature wave-transparent application scenarios such as high-temperature sensors and communication equipment. These characteristics make ALC widely used in the aviation, military, automotive manufacturing and other industries, showing broad application potential.
[0005] There are also different synthetic processes for the preparation of composite materials. CN107805064A relates to a method for preparing an alumina fiber reinforced alumina ceramic matrix composite material, which adopts a prepreg forming technology to realize the preparation of the composite material through the impregnation of alumina fibers in alumina slurry, molding and high temperature sintering. CN117682883A describes a method for preparing a fiber reinforced high temperature resistant magnesium aluminate spinel aerogel, which prepares a magnesium aluminate spinel sol by sol-gel technology, and composites the fiber felt with the sol by impregnation method, and then performs aging, drying and heat treatment to obtain the final product.
[0006] However, these existing technologies still have certain limitations. The high temperature sintering process of an alumina fiber reinforced alumina ceramic matrix composite material can cause damage to the microstructure of the material. Especially for alumina fiber materials, high temperature environment can cause rapid decline in mechanical properties, thereby affecting the performance of the material in extreme high temperature environment. While the aerogel technology improves the thermal insulation performance of the material, the wave transmission performance and chemical stability in ultra-high temperature and extreme dynamic environment (such as supersonic conditions) still need to be enhanced. In addition, the aerogel needs to be dried using supercritical fluid technology during preparation, which has high equipment cost, long time consumption, complex operation, and requires a large amount of organic solvent for aging, which is not environmentally friendly. Moreover, the material is mainly used for industrial kiln insulation structure, so the mechanical properties of the composite material are low. SUMMARY
[0007] Therefore, the present application provides a method for preparing a high-performance alumina fiber reinforced ceramic matrix composite material, which uses a new type of magnesium aluminate spinel aqueous sol as a precursor to reduce the sintering temperature of the composite material forming, and obtains an alumina fiber reinforced magnesium aluminate spinel ceramic matrix composite material.
[0008] To achieve the above-mentioned purposes, the technical scheme of the present application is as follows:
[0009] A method for preparing a high-performance alumina fiber reinforced ceramic matrix composite material, comprising the following steps:
[0010] 1) Preparing an alumina fiber fabric: preparing continuous alumina fibers and weaving them into an alumina fiber fabric, and cleaning the alumina fiber fabric with an organic solvent;
[0011] 2) Preparation of magnesium-aluminum spinel aqueous sol: magnesium source and aluminum source are dissolved in organic solvent at the same time, stirred uniformly for 10-60 min, and the pH value is adjusted to 9-10 by using ammonia water, and a transparent sol solution is formed by controllable hydrolysis. The sol solution is placed in a flask, and a rotary evaporator is installed. The temperature of the rotary evaporator is set at 40-60℃, and the rotation rate is set at 40-60 r / min. After the organic solvent is removed by rotary evaporation, deionized water is added at 20% of the volume of the organic solvent, and a stable magnesium-aluminum spinel aqueous sol is obtained;
[0012] 3) Preparation of composite material: the magnesium-aluminum spinel aqueous sol is brushed on the alumina fiber fabric, and after the surface is dried, the pre-impregnated fabric is stacked and hot-pressed, and then placed in a muffle furnace for sintering at a temperature of 700-900℃ for 1-3 h. After cooling to 25℃, the initial alumina fiber ceramic composite material is obtained. The alumina fiber ceramic composite material is placed in a vacuum assisted impregnation device for vacuum assisted impregnation. After the impregnation is completed, the vacuum assisted impregnation device containing the alumina fiber ceramic composite material is placed in an oven for drying. The sintering-vacuum assisted impregnation-drying steps are repeated, and finally the final alumina fiber ceramic matrix composite material is obtained after sintering again.
[0013] Further, the structure of the woven alumina fiber fabric in step 1) is a two-dimensional layered structure, and the fiber volume content of the fabric is (45±2) %.
[0014] Further, the cleaning method of the organic solvent in step 1) is: using acetone for ultrasonic assisted cleaning for 10 min, and repeating the cleaning for 3-5 times.
[0015] Further, the magnesium source in step 2) is one or more combinations of magnesium acetate, magnesium ethoxide, anhydrous magnesium chloride, magnesium chloride hexahydrate, magnesium acetate tetrahydrate, and magnesium sulfate. The aluminum source is one or more combinations of aluminum isopropoxide, anhydrous aluminum chloride, aluminum chloride hexahydrate, aluminum nitrate hexahydrate, aluminum hydroxide, and aluminum sec-butoxide.
[0016] Further, the organic solvent in step 2) is one or more combinations of anhydrous methanol, anhydrous ethanol, n-propanol, isopropyl alcohol, N,N-dimethylformamide (DMF), and N,N-dimethylacetamide (DMA).
[0017] Further, the molar ratio of the magnesium source to the aluminum source in step 2) is 1:1.8-2.2, and the mass ratio of the total mass of the magnesium source and the aluminum source to the mass of the organic solvent is 1:60-100.
[0018] Further, the pressure given by the vacuum assisted impregnation in step 3) is 3-7 MPa, and the pressure holding time at 25℃ is 24-96 h.
[0019] Further, the temperature of the oven drying in step 3) is 100-140℃, and the drying time is 24-72h.
[0020] Further, step 3) repeats the sintering-vacuum assisted impregnation-drying step 3-7 times.
[0021] The present application has the following advantages:
[0022] (1) The present application ensures the uniformity of the reaction and the appropriate concentration of the solution by precisely controlling the appropriate molar ratio of magnesium and aluminum and the volume of the solvent, thereby forming a uniform precursor sol. Controlling the rotary evaporation temperature and rotation rate allows the solvent to evaporate uniformly, preventing overheating decomposition and improving production efficiency. The aqueous sol generally has good dispersibility, which can ensure the uniformity of the material during subsequent molding and sintering, and the aqueous sol is environmentally friendly and does not release harmful gases during the molding process, which is green and environmentally friendly, and more conducive to large-scale production. Using the pre-impregnated laminate hot pressing process, multiple layers of sol-coated fiber cloth are stacked and pre-formed through the hot pressing process to form a pre-impregnated blank. By slowly heating, the grain growth process is controlled to prevent excessive grain growth and the formation of crystal defects, while ensuring uniform sintering and uniform particle size. Subsequently, the vacuum assisted impregnation process significantly improves the density and interlaminar bonding of the alumina fiber ceramic matrix composite by fully infiltrating the aqueous magnesium aluminate spinel sol in a vacuum environment. This method effectively fills the pores and micro-cracks inside the material, reduces defects and improves the mechanical strength and durability of the material. Finally, vacuum assisted impregnation ensures high performance of the composite material, making it more suitable for use in high temperature and extreme environments. Lower sintering temperature optimizes the crystal structure and particle size distribution of magnesium aluminate spinel, improving the purity, hardness, transparency and mechanical properties of the material, while also reducing the damage to alumina fibers caused by thermal stress during repeated sintering processes. Therefore, the present application not only improves the quality and performance of the composite material, but also reduces production costs, improves process controllability and consistency, making the method have significant advantages in large-scale production and industrial applications;
[0023] (2) The composite material prepared by the present application has good wave transmission performance and strong mechanical properties, is suitable for use in extreme environments such as ultra-high temperature and supersonic speed, and has high surface flatness, is suitable for secondary processing, and can be constructed in large size and environmentally friendly. Compared with the prior art, the present application introduces a composite structure of magnesium aluminate spinel and alumina fiber, which significantly improves the performance of the material in terms of high temperature stability, mechanical properties and wave transmission characteristics, especially for applications in extreme environments, which exhibits significant technical advantages and application potential. Moreover, the magnesium aluminate spinel sol used in the present application is an aqueous sol, which does not require the use of organic sol in the process of large-size parts, and is environmentally friendly. BRIEF DESCRIPTION OF DRAWINGS
[0024] Figure 1 is a preparation flow chart of a high-performance alumina fiber ceramic matrix composite material.
[0025] Figure 2 is a photo of the magnesium aluminate spinel aqueous sol precursor obtained in Example 1.
[0026] Figure 3 is an XRD pattern of the magnesium aluminate spinel ceramic obtained in Example 1.
[0027] Figure 4 is an XRD pattern of the alumina fiber reinforced ceramic matrix composite material obtained in Example 1.
[0028] Figure 5 is an SEM pattern of the alumina fiber reinforced ceramic matrix composite material obtained in Example 1.
[0029] Figure 6 is an SEM pattern of the magnesium aluminate spinel in the composite material obtained in Example 1.
[0030] Figure 7 is an SEM pattern of the magnesium aluminate spinel ceramic in the composite material obtained in Comparative Example 1.
[0031] Figure 8 is an SEM pattern of the magnesium aluminate spinel ceramic in the composite material obtained in Comparative Example 2. DETAILED DESCRIPTION
[0032] In order to enable a more detailed understanding of the features and technical content of the present application, the implementation of the present application is described in detail below in conjunction with the accompanying drawings, which are only used for reference and do not limit the present application.
[0033] I. Example
[0034] Example 1:
[0035] As shown in Figure 1 , a preparation method of a high-performance alumina fiber reinforced ceramic matrix composite material includes the following steps:
[0036] Step 1): Preparation of alumina fiber fabric: continuous alumina fibers are prepared and woven into a two-dimensional laminated structure of alumina fiber fabric, the fiber volume content of the fabric is 43%, and the alumina fiber fabric is cleaned by ultrasonic assisted acetone for 10 min, and the cleaning is repeated 3 times.
[0037] Step 2): Preparation of magnesium aluminate spinel aqueous sol: 0.1424 g magnesium acetate, 0.4084 g aluminum isopropoxide, 30 ml n-propanol were mixed, stirred uniformly, the stirring time was 10 min, and the pH value was adjusted to 9, a transparent sol solution was formed by controllable hydrolysis, the sol solution was placed in a flask, a rotary evaporator was installed, the temperature of the rotary evaporator was set at 40 °C, the rotation rate was set at 40 r / min, after the organic solvent was removed by rotary evaporation, 6 ml deionized water was added, and after the water was added, rotary evaporation was continued until the sol state was obtained, and a stable magnesium aluminate spinel aqueous sol was obtained;
[0038] Step 3): Preparation of composite material: the magnesium aluminate spinel aqueous sol was brushed on the alumina fiber fabric, and after the surface was dried, the prepreg was laminated and hot-pressed, and then was placed in a muffle furnace and sintered at a rate of 5 °C / min to 800 °C, sintered for 3 h, and cooled to 25 °C to obtain an initial alumina fiber ceramic composite material. The alumina fiber ceramic composite material was vacuum-assisted impregnated, placed in a vacuum-assisted impregnation device, and a pressure of 6 MPa was applied to the vacuum impregnation device, and the pressure was maintained at 25 °C for 72 h to further promote the impregnation of the precursor; the vacuum impregnation device containing the composite material was transferred to a 120 °C oven for drying for 72 h, and the composite material was formed and cured. The sintering-vacuum-assisted impregnation-drying steps were repeated 5 times, and finally sintered at a rate of 5 °C / min to 800 °C for 3 h to prepare an alumina fiber reinforced magnesium aluminate spinel composite material with excellent performance. As shown in the figure, the prepared material has a density of 2.37 g / cm Figures 2-6 3 , porosity of 28.9%, and bending strength of 254.90 ± 13.94 MPa.
[0039] Example 2:
[0040] The preparation method of the high-performance alumina fiber reinforced ceramic matrix composite material described in Example 1 was used, except that in step 1), 0.1424 g of magnesium acetate was replaced by 0.114 g of magnesium ethoxide. At the same time, the temperature of the rotary evaporator in step 2) was replaced by 60 °C. The prepared material has a density of 2.35 g / cm 3 , porosity of 29.1%, and bending strength of 254.91 ± 15.31 MPa.
[0041] Example 3:
[0042] The preparation method of the high-performance alumina fiber reinforced ceramic matrix composite material described in Example 1 was used, except that in step (1), 0.4084 g of aluminum isopropoxide was replaced by 0.267 g of anhydrous aluminum chloride, and 30 ml of n-propanol was replaced by n-propanol + DMF (1:1) solution. The prepared material has a density of 2.29 g / cm 3 , porosity 29.8%, flexural strength: 249.82 ± 14.27 MPa.
[0043] Example 4:
[0044] The preparation method of high-performance alumina fiber reinforced ceramic matrix composite material as described in Example 1, except that in the sintering-vacuum assisted impregnation-drying step, the vacuum assisted impregnation pressure holding time is changed to 24h. The composite density of the composite material is slightly lower than that of Example 3. The prepared material has a density of 2.23g / cm 3 , porosity 31.4%, flexural strength: 231.54 ± 13.89 MPa.
[0045] Example 5:
[0046] Step 1): Preparation of alumina fiber fabric: continuous alumina fibers are prepared and woven into a two-dimensional layered structure of alumina fiber fabric, the fiber volume content of the fabric is 43%, and the alumina fiber fabric is cleaned by ultrasonic assisted with acetone for 10min, and the cleaning is repeated for 3 times.
[0047] Step 2): Preparation of magnesium aluminate spinel aqueous sol: 0.1424g magnesium acetate, 0.3676g aluminum isopropoxide, 30ml n-propanol are mixed, stirred uniformly for 10min, and the pH value is adjusted to 9, a transparent sol solution is formed by controllable hydrolysis, the sol solution is placed in a flask, a rotary evaporator is filled, the temperature of the rotary evaporator is set at 40℃, the rotation rate is set at 40r / min, 6ml water is added after the removal of organic solvents by rotary evaporation, and the sol state is continued to be rotary evaporated after the addition of water to obtain a stable magnesium aluminate spinel aqueous sol;
[0048] Step 3): Preparation of composite material: the magnesium aluminate spinel aqueous sol is brushed on the alumina fiber fabric, and after surface drying, the prepreg stack is hot pressed, and then placed in a muffle furnace, gradually heated to 700℃ at a rate of 5℃ / min, sintered for 1h, and cooled to 25℃ to obtain the initial alumina fiber ceramic composite material, vacuum assisted impregnation is carried out on the alumina fiber ceramic composite material, placed in a vacuum assisted impregnation device, a pressure of 3MPa is given to the vacuum impregnation device, and the pressure is maintained for 24h at 25℃ to further promote the impregnation of the precursor; the vacuum impregnation device containing the composite material is transferred to a 100℃ oven for drying for 24h, and the forming and curing operation of the composite material is carried out, the sintering-vacuum assisted impregnation-drying step is repeated for 3 times, and finally sintered at a rate of 5℃ / min to 700℃ for 1h to prepare an excellent magnesium aluminate spinel composite material reinforced by alumina fiber. The prepared material has a density of 2.13g / cm 3 , porosity 33.2%, flexural strength: 223.73 ± 14.52 MPa.
[0049] Example 6:
[0050] Step 1): Preparation of alumina fiber fabric: Continuous alumina fibers were prepared and woven into a two-dimensional layered structure of alumina fiber fabric with a fiber volume content of 45%, the alumina fiber fabric was cleaned by ultrasonic assisted acetone for 10 min, and the cleaning was repeated 4 times.
[0051] Step 2): Preparation of magnesium aluminate spinel aqueous sol: 0.1424 g of magnesium sulfate, 0.4492 g of anhydrous aluminum chloride, and 60 ml of anhydrous methanol were mixed, stirred uniformly for 30 min, and the pH value was adjusted to 9.5. A transparent sol solution was formed by controllable hydrolysis. The sol solution was placed in a flask and loaded into a rotary evaporator with a temperature setting of 50°C and a rotation rate of 50 r / min. After removing the organic solvent by rotary evaporation, 12 ml of water was added, and the sol was obtained after continuous rotary evaporation. A stable magnesium aluminate spinel aqueous sol was obtained;
[0052] Step 3): Preparation of composite material: The magnesium aluminate spinel aqueous sol was brushed on the alumina fiber fabric, and after surface drying, the pre-preg laminate was hot-pressed, then placed in a muffle furnace and gradually heated to 800°C at a rate of 5°C / min, sintered for 2h, and cooled to 25°C to obtain the initial alumina fiber ceramic composite material. The alumina fiber ceramic composite material was vacuum assisted impregnated and placed in a vacuum assisted impregnation device, and a pressure of 5 MPa was applied to the vacuum impregnation device at 25°C for 48h to further promote the impregnation of the precursor. The vacuum impregnation device containing the composite material was transferred to a 120°C oven for drying for 48h to perform the shaping and curing operation of the composite material. The sintering-vacuum assisted impregnation-drying steps were repeated 5 times, and finally sintered at 800°C at a rate of 5°C / min for 2h to prepare an alumina fiber reinforced magnesium aluminate spinel composite material with excellent performance. The prepared material has a density of 2.22 g / cm 3 , porosity of 31.3%, and bending strength of 231.25±13.35 MPa.
[0053] Example 7:
[0054] Step 1): Preparation of alumina fiber fabric: Continuous alumina fibers were prepared and woven into a two-dimensional layered structure of alumina fiber fabric with a fiber volume content of 47%, the alumina fiber fabric was cleaned by ultrasonic assisted acetone for 10 min, and the cleaning was repeated 5 times.
[0055] Step 2): Preparation of magnesium aluminate spinel aqueous sol: 0.1424 g magnesium chloride hexahydrate, 0.4084 g aluminum chloride hexahydrate, 44 ml anhydrous ethanol were mixed, stirred uniformly for 60 min, and the pH value was adjusted to 10. A transparent sol solution was formed by controllable hydrolysis. The sol solution was placed in a flask and loaded into a rotary evaporator. The temperature of the rotary evaporator was set at 60°C and the rotation rate was set at 60 r / min. After removing the organic solvent by rotary evaporation, 9 ml of water was added. After adding water, rotary evaporation was continued until the sol state was obtained, and a stable magnesium aluminate spinel aqueous sol was obtained.
[0056] Step 3): Preparation of composite material: The magnesium aluminate spinel aqueous sol was brushed on the alumina fiber fabric, and after surface drying, the pre-impregnated fabric was laminated and hot-pressed, and then placed in a muffle furnace for sintering at a rate of 5°C / min to 900°C, sintered for 3 h, and cooled to 25°C to obtain the initial alumina fiber ceramic composite material. The alumina fiber ceramic composite material was vacuum-assisted impregnated in a vacuum-assisted impregnation device, and a pressure of 7 MPa was applied to the vacuum-assisted impregnation device. The pressure was maintained at 25°C for 96 h to further promote the impregnation of the precursor. The vacuum impregnation device containing the composite material was transferred to a 140°C oven for drying for 72 h to perform the shaping and curing operation of the composite material. The sintering-vacuum-assisted impregnation-drying steps were repeated 7 times, and finally sintered at a rate of 5°C / min to 900°C for 3 h to prepare an alumina fiber reinforced magnesium aluminate spinel composite material with excellent performance. The prepared material has a density of 2.29 g / cm 3 , porosity of 29.6%, and bending strength of 212.25 ± 16.13 MPa.
[0057] II. Comparative Example
[0058] Comparative Example 1:
[0059] The preparation method of the high-performance alumina fiber reinforced ceramic matrix composite material as described in Example 1 was used, except that the sintering temperature was changed. In step 3), the sintering at a rate of 5°C / min to 800°C was changed to sintering at a rate of 5°C / min to 1200°C. The prepared material has a density of 2.31 g / cm 3 , porosity of 30.3%, and bending strength of 156.49 MPa.
[0060] As shown in Figure 7 , during high-temperature sintering, the alumina fiber reinforced magnesium aluminate spinel composite material may face changes in morphology, grain growth, and the generation of defects such as pores and micro-cracks, which will weaken the mechanical properties of the fibers and the overall performance of the composite material. In addition, the accumulation of thermal stress may cause interface micro-cracks or delamination, further affecting the structural integrity and service life of the material.
[0061] Comparative Example 2:
[0062] The preparation method of high-performance alumina fiber reinforced ceramic matrix composite material is as described in Embodiment 1, except that: in step 2), the transparent sol solution is formed by controllable hydrolysis, and then the organic solvent is replaced with water, instead of directly forming a gel with an organic solvent. The prepared material has a density of 2.36 g / cm 3 , a porosity of 27.6%, and a bending strength of 101.37 MPa.
[0063] As shown in Figure 8 , the process of using only an organic solvent to form a gel without adding water may cause problems such as difficulty in gelation, incomplete reaction, and undesirable pore structure, thereby affecting the quality and application performance of the final material.
[0064] The specific models of the devices involved above are not limited or described in detail, and the deep connection methods of the devices involved above are not described in detail, which can be understood by those skilled in the art as common knowledge.
[0065] The above only describes the preferred embodiments of the present application, and is not intended to limit the protection scope of the present application. Any modifications, equivalent replacements, and improvements made within the spirit and principles of the present application shall be included in the protection scope of the present application.
Claims
1. A method for producing a high-performance alumina fiber-reinforced ceramic matrix composite, characterized by, The method comprises the following steps: 1) preparing an alumina fiber fabric: continuous alumina fibers are prepared and woven into an alumina fiber fabric, and the alumina fiber fabric is cleaned using an organic solvent; 2) preparing a magnesium-aluminum spinel aqueous sol: a magnesium source and an aluminum source are simultaneously dissolved in an organic solvent, stirred uniformly for 10-60 min, and the pH value is adjusted to 9-10 using ammonia water, a transparent sol solution is formed through controllable hydrolysis, the sol solution is placed in a flask, a rotary evaporator is loaded, the temperature of the rotary evaporator is set to 40-60℃, the rotation rate is set to 40-60 r / min, after the organic solvent is removed through rotary evaporation, deionized water is added at 20% of the volume of the organic solvent, and a stable magnesium-aluminum spinel aqueous sol is obtained; the molar ratio of the magnesium source to the aluminum source is 1:1.8-2.2, and the mass ratio of the total mass of the magnesium source and the aluminum source to the mass of the organic solvent is 1:60-100; 3) preparing a composite material: the magnesium-aluminum spinel aqueous sol is brushed on the alumina fiber fabric, and after surface drying, the alumina fiber fabric is laminated and hot-pressed, and then placed in a muffle furnace for sintering, the temperature is 700-900℃, the sintering time is 1-3 h, the sintering temperature rising rate is 5℃ / min, and after cooling to 25℃, an initial alumina fiber ceramic composite material is obtained; the alumina fiber ceramic composite material is placed in a vacuum-assisted impregnation device for vacuum-assisted impregnation of the magnesium-aluminum spinel aqueous sol, after the impregnation is completed, the vacuum-assisted impregnation device loaded with the alumina fiber ceramic composite material is placed in an oven for drying, and the sintering-vacuum-assisted impregnation-drying steps are repeated 3-7 times, and finally, the sintering temperature for the last sintering is 700℃, 800℃ or 900℃, and the sintering temperature rising rate is 5℃ / min, to obtain a final alumina fiber reinforced ceramic matrix composite material.
2. The method for preparing a high-performance alumina fiber-reinforced ceramic matrix composite material according to claim 1, characterized in that, The structure of the woven alumina fiber fabric in step 1) is a two-dimensional laminated structure, and the fiber volume content of the fabric is (45±2)%.
3. The method for preparing a high-performance alumina fiber-reinforced ceramic matrix composite material according to claim 2, characterized in that, The cleaning method of the organic solvent in step 1) is: using acetone for ultrasonic-assisted cleaning for 10 min, and repeating the cleaning 3-5 times.
4. The method for preparing a high-performance alumina fiber-reinforced ceramic matrix composite material according to claim 3, characterized in that, The magnesium source in step 2) is one or more combinations of magnesium acetate, magnesium ethoxide, anhydrous magnesium chloride, magnesium chloride hexahydrate, magnesium acetate tetrahydrate, and magnesium sulfate, and the aluminum source is one or more combinations of aluminum isopropoxide, anhydrous aluminum chloride, aluminum chloride hexahydrate, aluminum nitrate hexahydrate, aluminum hydroxide, and aluminum sec-butoxide.
5. The method for preparing a high-performance alumina fiber-reinforced ceramic matrix composite material according to claim 4, characterized in that, The organic solvent in step 2) is one or more combinations of anhydrous methanol, anhydrous ethanol, n-propanol, isopropyl alcohol, N,N-dimethylformamide, and N,N-dimethylacetamide.
6. The method for preparing a high-performance alumina fiber-reinforced ceramic matrix composite material according to claim 5, characterized in that, The pressure given by the vacuum-assisted impregnation in step 3) is 3-7 MPa, and the pressure holding time at 25℃ is 24-96 h.
7. The method for preparing a high-performance alumina fiber-reinforced ceramic matrix composite material according to claim 6, characterized in that, The temperature for drying in the oven in step 3) is 100-140℃, and the drying time is 24-72 h.
8. The method for preparing a high-performance alumina fiber-reinforced ceramic matrix composite material according to claim 7, characterized in that, The sintering-vacuum-assisted impregnation-drying steps in step 3) are repeated 3-7 times.
Citation Information
Patent Citations
Preparation method of alumina fiber reinforced alumina ceramic-based composite material by using prepreg forming method
CN117682883A
Method for preparing fiber-reinforced high-temperature-resistant magnesium aluminum spinel aerogel
CN107805064A
Preparation method of alumina fiber reinforced ceramic composite material containing alumina interface layer
CN112250460A