Alumina-quartz hybrid woven fabric reinforced ceramic matrix composite and method of making the same
By developing a method for preparing ceramic matrix composites reinforced with alumina-quartz hybrid woven fabric, the problems of decreased mechanical properties of quartz fibers at high temperatures and poor ablation resistance of alumina fibers have been solved. This method achieves excellent comprehensive performance of the material at high temperatures, making it suitable for load-bearing and heat-resistant components of hypersonic vehicles.
Patent Information
- Application Number
- CN202311796693.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-25
- Publication Date
- 2026-01-09
- Estimated Expiration
- 2043-12-25
AI Technical Summary
Quartz fibers are prone to precipitating cristobalite phase at high temperatures, which leads to fiber embrittlement and a decrease in mechanical properties. Alumina fibers, on the other hand, have poor ablation resistance and are expensive, limiting their application in high-temperature environments.
A ceramic matrix composite material with excellent comprehensive performance was prepared by using alumina-quartz hybrid woven fabric to reinforce the core layer and quartz fiber woven fabric to the surface layer. The core layer uses alumina fiber-quartz fiber hybrid woven fabric and the surface layer uses quartz fiber fabric. The composite material is connected by needle punching and stitching, combined with silica sol impregnation, drying curing and sintering process.
In high-temperature environments, the material possesses both the ablation resistance of quartz fiber and the high-temperature mechanical properties of alumina fiber, reducing density and manufacturing costs, making it suitable for load-bearing and heat-resistant components of hypersonic aircraft.
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Figure BDA0004627919040000111
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of thermal protection materials of aerospace vehicles, and particularly relates to an alumina-quartz mixed woven fabric reinforced ceramic matrix composite material and a preparation method thereof. BACKGROUND
[0002] In the flight process, a hypersonic vehicle will bear the action of thermal loads such as high temperature, high pressure, strong scouring and high heat flow. In order to ensure the normal work of the vehicle structure material, a high-temperature resistant thermal protection material needs to be used to protect the aerospace vehicle. According to the difference of force and thermal environment, different protection materials are usually used for different parts of the vehicle. The nose cone, wing leading edge and other parts with serious aerodynamic heating generally use ceramic matrix composite materials for thermal protection.
[0003] Quartz fiber has good chemical stability, heat shock resistance, ablation resistance, is easy to weave and has excellent dielectric properties, and has great application prospect in the field of aerospace wave-transparent materials. Quartz fiber reinforced quartz-based (SiO 2f / SiO2) composite material has the advantages of high strength, high temperature resistance, heat shock resistance and good electrical properties. In addition, due to the high mass fraction of SiO2 (≥99.9%) in the material, the viscosity after melting is large, and it has good ablation performance and excellent force, thermal and electrical comprehensive performance. It is the most mature and most widely used ceramic-based wave-transparent composite material at home and abroad. However, quartz fiber is a glassy material, which is in a thermodynamically unstable state, and is easy to precipitate cristobalite phase at high temperature. The precipitated cristobalite has a large volume effect during temperature fluctuation, which leads to fiber embrittlement and causes the mechanical properties of the composite material to decrease significantly, which seriously restricts the use of SiO 2f / SiO2 composite material at high temperature.
[0004] Continuous alumina fiber is a new type of high-performance oxide ceramic fiber with better high-temperature performance than quartz fiber and glass fiber, and has excellent creep resistance and thermal shock resistance. Continuous alumina fiber reinforced ceramic matrix composite material has the characteristics of high strength, excellent temperature resistance and oxidation resistance, and the mechanical properties and temperature resistance are obviously superior to SiO 2f / SiO2 system, and is one of the ideal high-temperature bearing materials. However, alumina fiber has a large linear expansion coefficient, poor ablation resistance, and is more expensive than quartz fiber, which limits the application of alumina fiber reinforced oxide composite material in ablation and heat protection materials. SUMMARY
[0005] The present application solves the technical problem of providing an alumina-quartz mixed woven fabric reinforced ceramic matrix composite material and a preparation method thereof, taking the alumina fiber-quartz fiber mixed layer as the core layer and the quartz layer as the surface layer, avoiding the mechanical property decline of the quartz fiber under high temperature conditions, solving the problems of poor ablation resistance and relatively high density of the alumina fiber, and having a wide application prospect in the field of load-bearing and heat-proof components of hypersonic aircraft.
[0006] To solve the above problems, the first aspect of the present application provides an alumina-quartz mixed woven fabric reinforced ceramic matrix composite material, comprising a reinforcing material and a ceramic matrix; the reinforcing material comprises a core layer fabric and surface layer fabrics arranged on the upper and lower surfaces of the core layer fabric; the core layer fabric is an alumina fiber-quartz fiber mixed woven fabric; the surface layer fabric is a quartz fiber fabric; and the ceramic matrix is silicon dioxide.
[0007] Preferably, in the core layer fabric, the mass ratio of the alumina fiber to the quartz fiber is 1:0.5-4.
[0008] Preferably, the total volume ratio of the core layer fabric to the surface layer fabrics on the upper and lower surfaces is 1:0.5-5.
[0009] Preferably, the core layer fabric is one or more of the following: a mixed fiber woven alumina-quartz mixed woven fabric obtained by mixing alumina fiber bundles and quartz fiber bundles, an alumina-quartz mixed woven fabric woven by alumina fibers and quartz fibers, and a fabric obtained by superimposing and needling the combination of alumina cloth and quartz cloth.
[0010] Preferably, the surface layer fabric and the core layer fabric are connected by needling and sewing.
[0011] The second aspect of the present application provides a preparation method of the above-mentioned alumina-quartz mixed woven fabric reinforced ceramic matrix composite material, comprising the following steps:
[0012] S1. Preparing the reinforcing material;
[0013] S2. Impregnating the reinforcing material with silicon sol;
[0014] S3. Drying and curing the reinforcing material impregnated with silicon sol to obtain an alumina-quartz mixed woven fabric reinforced ceramic matrix composite material blank;
[0015] S4. Sintering the alumina-quartz mixed woven fabric reinforced ceramic matrix composite material blank to obtain the alumina-quartz mixed woven fabric reinforced ceramic matrix composite material.
[0016] Preferably, step S2 specifically comprises the following steps: placing the reinforcing material in a vacuum impregnation device, vacuumizing the vacuum impregnation device, and then sucking in silicon sol with a density of 1.1-1.5 g / cm3.3 The silica sol is kept under vacuum for 2-24 hours;
[0017] In step S3, the curing temperature is 100-250℃, and the curing time is 24-100h;
[0018] In step S4, the sintering atmosphere is one or a mixture of nitrogen, ammonia, and argon, or a vacuum environment; the sintering temperature is 300-900℃; and the sintering time is 1-3 hours.
[0019] Preferably, the method further includes removing the wetting agent from the reinforcing material before step S2;
[0020] The removal of the wetting agent from the reinforcing material specifically includes the following steps: placing the reinforcing material in a sealed container, evacuating the container, then drawing in the cleaning solvent and immersing the reinforcing material, treating it at 20-100℃ and 0-5MPa for 4-20 hours, and then drying the treated reinforcing material at 20-200℃ for 10-25 hours.
[0021] Preferably, the method further includes repeating steps S2, S3, and S4 5-10 times after step S4 to perform cyclic densification of the composite material.
[0022] It also includes: during the cyclic densification process of the composite material, performing 3-5 processing steps to make the surface layer of the processed alumina-quartz woven reinforced ceramic matrix composite material a quartz fiber / quartz matrix composite material layer.
[0023] Preferably, the process further includes, after the composite material is cyclically densified, surface sealing of the obtained alumina-quartz woven reinforced ceramic matrix composite material, wherein the surface sealing is performed using a mixture of one or two of quartz powder or quartz-quartz composite material powder and silica sol at a mass ratio of 1:(0.2-5).
[0024] Compared with the prior art, the present invention has the following advantages:
[0025] The alumina-quartz hybrid woven ceramic matrix composite of the present invention uses an alumina fiber-quartz fiber hybrid woven fabric in the core layer, so that the composite material has the characteristics of quartz fiber / quartz matrix composite material such as ablation resistance, good heat resistance and low emissivity in high temperature environment, as well as the excellent high temperature mechanical properties of alumina fiber. The use of quartz fiber fabric in the surface layer can give full play to the ablation resistance of quartz fiber / quartz matrix composite material, ensure the integrity of alumina fiber under ablation conditions, and make the composite material have a high strength retention rate. Moreover, compared with alumina fiber / quartz matrix composite material, the use of quartz fiber fabric in the surface layer can significantly reduce the density and manufacturing cost of the composite material.
[0026] The alumina-quartz mixed woven fabric reinforced ceramic matrix composite material of the present application solves the problems of poor ablation resistance and relatively high density of alumina fiber while avoiding the mechanical property decline of quartz fiber under high temperature conditions, and is a load-heat integrated material with excellent comprehensive performance, which has a wide application prospect in the field of load-heat integrated components of hypersonic aircraft. DETAILED DESCRIPTION
[0027] The technical solutions of the present application will be described clearly and completely below in combination with the embodiments of the present application. Obviously, the described embodiments are only some of the embodiments of the present application, but not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.
[0028] For the thermal protection material of space aircraft, quartz fiber reinforced quartz matrix composite material has the advantages of high strength, high temperature resistance, thermal shock resistance, good electrical performance and good ablation performance, but quartz fiber is easy to precipitate cristobalite phase at high temperature, which leads to fiber embrittlement and causes the mechanical properties of the composite material to decrease significantly. The high temperature performance of alumina fiber is better than that of quartz fiber, and alumina fiber has excellent creep resistance and thermal shock resistance, but the linear expansion coefficient of alumina fiber is large, the ablation resistance is poor, and the price is high compared with quartz fiber.
[0029] Therefore, the first aspect of the embodiments of the present application provides an alumina-quartz mixed woven fabric reinforced ceramic matrix composite material, which comprises a reinforcing material and a ceramic matrix; the reinforcing material comprises a core layer fabric and a surface layer fabric arranged on the upper and lower surfaces of the core layer fabric; the core layer fabric is an alumina fiber-quartz fiber mixed woven fabric; the surface layer fabric is a quartz fiber fabric; and the ceramic matrix is silicon dioxide.
[0030] The alumina-quartz mixed woven fabric reinforced ceramic matrix composite material of the embodiments of the present application uses alumina fiber-quartz fiber mixed woven fabric in the core layer, so that the composite material has the characteristics of good ablation resistance, good heat resistance and low radiation coefficient of quartz fiber / quartz matrix composite material under high temperature environment, and also has excellent high temperature mechanical properties of alumina fiber; the quartz fiber fabric is used in the surface layer, which can fully exert the ablation resistance characteristics of quartz fiber / quartz matrix composite material, ensure the integrity of alumina fiber under ablation conditions, make the composite material have a high strength retention rate, and compared with alumina fiber / quartz matrix composite material, the use of quartz fiber fabric in the surface layer can significantly reduce the density and preparation cost of the composite material.
[0031] In some embodiments, the mass ratio of alumina fibers to quartz fibers in the core fabric can be adjusted in a wide range. Preferably, the mass ratio of alumina fibers to quartz fibers is 1:0.5-4. With the increase of the content of alumina fibers, the high-temperature performance, creep resistance and thermal shock resistance of the composite material are improved, but the ablation resistance is reduced. With the increase of the content of quartz fibers, the ablation resistance of the composite material is improved, but the high-temperature mechanical properties are reduced. When the mass ratio is used, the composite material produced has lower production cost while having excellent high-temperature performance, creep resistance, thermal shock resistance, high-temperature mechanical properties and ablation resistance.
[0032] In some embodiments, the volume ratio of the core fabric to the surface fabric can be adjusted in a wide range. Preferably, the total volume ratio of the core fabric to the surface fabric of the upper and lower surfaces is 1:0.5-5. The higher the volume content of the core fabric, the higher the content of alumina fibers, and the higher-temperature performance, creep resistance and thermal shock resistance of the composite material are improved, but the ablation resistance is reduced. The higher the volume content of the surface fabric, the higher the ablation resistance of the composite material, but the high-temperature mechanical properties are reduced. When the volume ratio is used, the integrity of the alumina fibers under ablation conditions can be ensured, so that the composite material has a high strength retention rate, and the composite material produced has excellent high-temperature performance, creep resistance, thermal shock resistance, high-temperature mechanical properties and ablation resistance.
[0033] In some embodiments, the alumina fiber-quartz fiber mixed fabric used in the core fabric can be one or a combination of several of the following fiber cloths.
[0034] The first is an alumina-quartz mixed fabric woven by mixing alumina fiber bundles and quartz fiber bundles, i.e., hybridization within the fiber bundle. Alumina fiber bundles and quartz fiber bundles with a low number of filaments are cabled and twisted according to a selected ratio to obtain alumina-quartz hybrid fibers, and the alumina-quartz hybrid fibers are woven into an alumina-quartz mixed fabric. Specifically, the alumina-quartz hybrid fibers can be prepared by cabling and twisting (2-10) times to obtain (10-100) twists.
[0035] The second is an alumina-quartz mixed fabric woven by alumina fibers and quartz fibers, i.e., hybridization within the cloth layer. Alumina fibers and quartz fibers are woven into an alumina-quartz mixed fabric according to a selected mass ratio.
[0036] The third is a combination of alumina cloth and quartz cloth, i.e., hybridization between cloth layers. For example, a combination of 3 layers of alumina cloth and 3 layers of quartz cloth.
[0037] Specifically, the hybrid fabric can be woven by using a single hybrid fabric in a fiber bundle, a single hybrid fabric in a fabric layer, a single hybrid fabric in a fabric layer, or a combination of two or three hybrid fabrics, such as a combination of 3 layers of hybrid fabric in a fiber bundle and 3 layers of hybrid fabric in a fabric layer, a combination of 2 layers of hybrid fabric in a fiber bundle, 2 layers of hybrid fabric in a fabric layer, 1 layer of aluminum oxide fabric, and 1 layer of quartz fabric. The hybrid fabrics in each layer can be connected by needling.
[0038] In some embodiments, the surface layer fabric and the core layer fabric are connected by needling.
[0039] The second aspect of the embodiment of the present application provides a preparation method of the above-mentioned aluminum oxide-quartz hybrid fabric reinforced ceramic matrix composite material, comprising:
[0040] S1. preparing the reinforcing material;
[0041] S2. impregnating the reinforcing material with silica sol;
[0042] S3. drying and curing the reinforcing material impregnated with silica sol to obtain an aluminum oxide-quartz hybrid fabric reinforced ceramic matrix composite material blank;
[0043] S4. sintering the aluminum oxide-quartz hybrid fabric reinforced ceramic matrix composite material blank to obtain the aluminum oxide-quartz hybrid fabric reinforced ceramic matrix composite material.
[0044] In some embodiments, step S1 comprises:
[0045] S101. preparing a core layer fabric;
[0046] S102. preparing a surface layer fabric and connecting the surface layer fabric and the core layer fabric.
[0047] Specifically, the surface layer fabric can be prepared by directly stacking a quartz fabric on the core layer fabric and needling and sewing to obtain the reinforcing material.
[0048] In some embodiments, the method further comprises, before step S2, removing the impregnating agent on the reinforcing material.
[0049] Preferably, the removing of the infiltrant on the reinforcing material comprises the following steps: placing the reinforcing material in a sealed container, vacuumizing the container, then absorbing the cleaning solvent and immersing the reinforcing material, treating the reinforcing material at 20-100℃ and 0-5MPa for 4-20h, and then drying the treated reinforcing material at 20-200℃ for 10-25h. Through the above cleaning process, the infiltrant on the surface of the fiber can be removed, which is beneficial to the full infiltration of the resin to the fiber.
[0050] In some embodiments, the cleaning solvent can be one or a mixture of several of the following organic solvents: anhydrous ethanol, acetone, etc.
[0051] In some embodiments, step S2 specifically comprises the following steps: placing the reinforcing material in a vacuum impregnation device, vacuumizing the vacuum impregnation device, then absorbing the silica sol with a density of 1.1-1.5g / cm 3 for 2-24h under vacuum condition.
[0052] In some embodiments, in step S3, the temperature of the curing is 100-250℃, and the time of the curing is 24-100h.
[0053] In some embodiments, in step S4, the atmosphere of the sintering is a mixture of one or more of the following: nitrogen, ammonia, argon, or vacuum environment, the temperature of the sintering is 300-900℃, and the time of the sintering is 1-3h.
[0054] In some embodiments, after step S4, the steps S2, S3, and S4 are repeated for 5-10 times to perform the cyclic densification of the composite material. Through the cyclic densification, the degree of densification of the obtained composite material can be improved, thereby improving the comprehensive performance of the composite material.
[0055] In some embodiments, further comprising: during the cyclic densification of the composite material, performing 3-5 times of processing to make the surface layer of the aluminum oxide-quartz hybrid woven fabric reinforced ceramic matrix composite material into a quartz fiber / quartz composite material layer.
[0056] In some embodiments, further comprising: after the cyclic densification of the composite material, performing surface sealing on the obtained aluminum oxide-quartz hybrid woven fabric reinforced ceramic matrix composite material, and the surface sealing uses a mixture of one or both of the following: quartz powder or quartz / quartz composite material powder, and silica sol with a mass ratio of 1:(0.2-5).
[0057] Example 1
[0058] The alumina-quartz hybrid woven fabric reinforced ceramic matrix composite material of the embodiment comprises a reinforcing material and a silica matrix, and the volume percentage of the reinforcing material is 40%. The reinforcing material comprises a core layer fabric and surface layer fabrics arranged on the upper and lower surfaces of the core layer fabric. The core layer fabric is an alumina-quartz hybrid woven fabric obtained by mixing alumina fiber bundles and quartz fiber bundles at a mass ratio of 1:2 and weaving the hybrid fibers, and the core layer fabric is obtained by stacking and needling the alumina-quartz hybrid woven fabric. The surface layer fabrics are quartz fiber fabrics. The volume ratio of the core layer fabric to the surface layer fabrics is 1:3.
[0059] The method for preparing the alumina-quartz hybrid woven fabric reinforced ceramic matrix composite material of the embodiment comprises the following steps.
[0060] 1. Preparing the reinforcing material:
[0061] (1) mixing and twisting (2-10) strands of alumina fiber bundles and quartz fiber bundles at a mass ratio of 1:2 and twisting (10-100) turns to obtain alumina-quartz hybrid fibers, weaving the alumina-quartz hybrid woven fabric with the hybrid fibers, and then stacking and needling the hybrid woven fabric to obtain the core layer fabric.
[0062] (2) stacking the quartz fiber fabric on the basis of the obtained core layer fabric and needling and sewing to obtain the reinforcing material, and the volume ratio of the core layer fabric to the surface layer fabric is 1:3.
[0063] 2. Placing the obtained hybrid woven fabric reinforcing material in a sealed container, vacuumizing the container, absorbing anhydrous ethanol, and immersing the fabric, treating at 50°C and 2MPa for 10 hours, then taking out the hybrid woven fabric reinforcing material from the anhydrous ethanol and placing it in an oven for drying at 100°C for 18 hours to remove the sizing agent on the surface of the hybrid woven fabric reinforcing material.
[0064] 3. Placing the hybrid woven fabric reinforcing material with the sizing agent removed into a vacuum impregnation device, vacuumizing the device, then absorbing silica sol with a density of 1.2g / cm 3 and maintaining the vacuum condition for 15 hours to allow the silica sol to fully fill the pores in the fabric preform.
[0065] 4. Placing the hybrid woven fabric reinforcing material fully impregnated with the silica sol into a curing furnace, drying and curing at 200°C under normal pressure for 48 hours to obtain an alumina-quartz hybrid woven fabric reinforced ceramic matrix composite material blank.
[0066] 5. Placing the alumina-quartz hybrid woven fabric reinforced ceramic matrix composite material blank into a sintering device, sintering at 600°C under a nitrogen atmosphere for 2 hours.
[0067] 6. Repeat the steps 3, 4 and 5 for 8 times to perform the cycle densification of the composite material, and obtain the alumina-quartz mixed woven fabric reinforced ceramic matrix composite material with high densification degree. During the cycle densification of the composite material, the composite material is processed for 5 times to ensure that the surface layer of the processed alumina-quartz mixed woven fabric reinforced ceramic matrix composite material is a quartz fiber / quartz composite material layer.
[0068] 7. Perform the surface sealing of the obtained alumina-quartz mixed woven fabric reinforced ceramic matrix composite material, and the surface sealing adopts a mixture of quartz powder and silica sol with a mass ratio of 1:3.
[0069] Example 2
[0070] The alumina-quartz mixed woven fabric reinforced ceramic matrix composite material of the present example is different from that of example 1 in that the core layer fabric is an alumina-quartz mixed woven cloth woven by alumina fibers and quartz fibers and obtained by stacking and needling. The rest of the structure, composition and example 1 are the same.
[0071] The preparation method of the alumina-quartz mixed woven fabric reinforced ceramic matrix composite material of the present example, the preparation step of the core layer fabric is: weaving the alumina-quartz mixed woven cloth with alumina fibers and quartz fibers according to the mass ratio of 1:2, and then stacking and needling the mixed woven cloth to obtain the core layer fabric. The rest of the steps are the same as example 1.
[0072] Example 3
[0073] The alumina-quartz mixed woven fabric reinforced ceramic matrix composite material of the present example is different from that of example 1 in that the core layer fabric is obtained by alternately arranging and stacking and needling the alumina cloth and the quartz cloth. The rest of the structure, composition and example 1 are the same.
[0074] The preparation method of the alumina-quartz mixed woven fabric reinforced ceramic matrix composite material of the present example, the preparation step of the core layer fabric is: stacking and needling the alumina cloth and the quartz cloth according to the mass ratio of 1:2 to obtain the core layer fabric. The rest of the steps are the same as example 1.
[0075] Example 4
[0076] The alumina-quartz mixed woven fabric reinforced ceramic matrix composite material of the present example is different from that of example 1 in that the mass ratio of the alumina fibers to the quartz fibers in the core layer fabric is 1:0.5. The rest of the structure, composition, and preparation method are the same as example 1.
[0077] Example 5
[0078] The aluminum oxide-quartz mixed woven fabric reinforced ceramic matrix composite material of the present embodiment differs from that of Example 1 in that the mass ratio of aluminum oxide fiber to quartz fiber in the core layer fabric is 1:4. The rest of the structure, composition, and preparation method are the same as those of Example 1.
[0079] Example 6
[0080] The aluminum oxide-quartz mixed woven fabric reinforced ceramic matrix composite material of the present embodiment differs from that of Example 1 in that the mass ratio of aluminum oxide fiber to quartz fiber in the core layer fabric is 1:0.2. The rest of the structure, composition, and preparation method are the same as those of Example 1.
[0081] Example 7
[0082] The aluminum oxide-quartz mixed woven fabric reinforced ceramic matrix composite material of the present embodiment differs from that of Example 1 in that the mass ratio of aluminum oxide fiber to quartz fiber in the core layer fabric is 1:6. The rest of the structure, composition, and preparation method are the same as those of Example 1.
[0083] Example 8
[0084] The aluminum oxide-quartz mixed woven fabric reinforced ceramic matrix composite material of the present embodiment differs from that of Example 1 in that the volume ratio of the core layer fabric to the surface layer fabric is 1:0.2. The rest of the structure, composition, and preparation method are the same as those of Example 1.
[0085] Example 9
[0086] The aluminum oxide-quartz mixed woven fabric reinforced ceramic matrix composite material of the present embodiment differs from that of Example 1 in that the volume ratio of the core layer fabric to the surface layer fabric is 1:5. The rest of the structure, composition, and preparation method are the same as those of Example 1.
[0087] Example 10
[0088] The aluminum oxide-quartz mixed woven fabric reinforced ceramic matrix composite material of the present embodiment differs from that of Example 1 in that the volume ratio of the core layer fabric to the surface layer fabric is 1:0.2. The rest of the structure, composition, and preparation method are the same as those of Example 1.
[0089] Example 11
[0090] The aluminum oxide-quartz mixed woven fabric reinforced ceramic matrix composite material of the present embodiment differs from that of Example 1 in that the volume ratio of the core layer fabric to the surface layer fabric is 1:8. The rest of the structure, composition, and preparation method are the same as those of Example 1.
[0091] Comparative Example 1
[0092] The comparative example is a quartz fiber reinforced quartz matrix composite material, which comprises a quartz fiber fabric reinforcing material and a silica matrix, and the volume percentage of the reinforcing material is 40%. The preparation method of the comparative example of the quartz fiber reinforced quartz matrix composite material comprises: 1. preparing a quartz fiber fabric; steps 2-7 are the same as the preparation method of example 1.
[0093] Comparative example 2
[0094] The comparative example is an alumina fiber reinforced quartz matrix composite material, which comprises an alumina fiber fabric reinforcing material and a silica matrix, and the volume percentage of the reinforcing material is 40%. The preparation method of the comparative example of the alumina fiber reinforced quartz matrix composite material comprises: 1. preparing an alumina fiber fabric; steps 2-7 are the same as the preparation method of example 1.
[0095] Comparative example 3
[0096] The comparative example is an alumina-quartz hybrid fabric reinforced ceramic matrix composite material, which comprises a reinforcing material and a silica matrix, and the volume percentage of the reinforcing material is 40%. The reinforcing material does not distinguish the core layer and the surface layer, and the whole is made of: alumina fiber bundles and quartz fiber bundles are (2-10) plied and twisted (10-100) twists according to a mass ratio of 1:2 to obtain alumina-quartz hybrid fibers, the hybrid fibers are used to weave an alumina-quartz hybrid fabric, and then the hybrid fabric is prepared by stacking and needling. The preparation method of the comparative example of the alumina fiber reinforced quartz matrix composite material comprises: 1. preparing an alumina-quartz hybrid fabric reinforcing material; steps 2-7 are the same as the preparation method of example 1, and do not include the processing steps in the cyclic densification process.
[0097] The density, strength performance, high-temperature mechanical property and ablation performance of the composite material obtained in each of the above examples and comparative examples were tested, and the test results are shown in Table 1. As can be seen from Table 1, the quartz fiber reinforced quartz matrix composite material of Comparative Example 1 has relatively low density, good strength performance and good ablation performance, but its mechanical property at high temperature decreases significantly; the alumina fiber reinforced quartz matrix composite material of Comparative Example 2 has good strength performance and good mechanical property at high temperature, but poor ablation resistance; the alumina-quartz mixed woven fabric reinforced ceramic matrix composite material of Comparative Example 3 has better ablation performance than Comparative Example 2, but is significantly worse than Comparative Example 1. In contrast, the composite materials obtained in each of the examples of the present application have better comprehensive performance than each of the comparative examples. Among them, Examples 1, 4-7 differ in the proportion of alumina fibers and quartz fibers in the core fabric, wherein the content of alumina fibers in Example 6 is too high, the high-temperature mechanical property of the composite material does not improve significantly, but the ablation performance decreases, the cost increases greatly, and the density increases significantly; the content of quartz fibers in Example 7 is too high, the ablation performance of the composite material does not improve significantly, but the high-temperature mechanical property decreases significantly, therefore, the proportion of alumina fibers and quartz fibers in Examples 1, 4 and 5 is a more preferred proportion range. Examples 1, 8-11 differ in the volume ratio of the core fabric to the surface fabric, wherein the proportion of the core fabric in Example 10 is too large, and the ablation performance decreases significantly; the proportion of the surface fabric in Example 11 is too large, and the high-temperature mechanical property decreases significantly, therefore, the volume ratio of the core fabric to the surface fabric in Examples 1, 8 and 9 is a more preferred proportion range.
[0098] Table 1
[0099]
[0100] Obviously, the above examples are merely examples for clarity and do not limit the embodiments. Based on the above description, other different forms of changes or variations can be made by those of ordinary skill in the art. All embodiments do not need to be exhausted here. The obvious changes or variations derived therefrom are still within the protection scope of the present application.
Claims
1. An alumina-quartz hybrid fabric reinforced ceramic matrix composite material, characterized in that: comprising a reinforcing material and a ceramic matrix; the reinforcing material comprises a core fabric and surface layer fabrics arranged on the upper and lower surfaces of the core fabric; the core fabric is an alumina fiber-quartz fiber hybrid fabric; the surface layer fabric is a quartz fiber fabric; the ceramic matrix is silicon dioxide; in the core fabric, the mass ratio of alumina fiber to quartz fiber is 1:0.5-4; the total volume ratio of the core fabric to the surface layer fabric on the upper and lower surfaces is 1:0.5-5; a preparation method of the alumina-quartz hybrid fabric reinforced ceramic matrix composite material, comprising: S1. preparing the reinforcing material; S2. impregnating the reinforcing material with silica sol; S3. drying and curing the reinforcing material after impregnating silica sol to obtain an alumina-quartz hybrid fabric reinforced ceramic matrix composite material; S4. sintering the alumina-quartz hybrid fabric reinforced ceramic matrix composite material to obtain the alumina-quartz hybrid fabric reinforced ceramic matrix composite material; further comprising removing the impregnating agent on the reinforcing material before step S2; removing the impregnating agent on the reinforcing material specifically comprises the following steps: placing the reinforcing material in a sealed container, vacuumizing the container, then absorbing the cleaning solvent and immersing the reinforcing material, treating at 20-100℃, 0-5MPa for 4-20h, then drying the treated reinforcing material at 20-200℃ for 10-25h; further comprising repeating steps S2, S3, S4 for 5-10 times after step S4 to perform composite material cyclic densification; further comprising: during the composite material cyclic densification process, processing 3-5 times to make the surface layer of the alumina-quartz hybrid fabric reinforced ceramic matrix composite material a quartz fiber / quartz composite material layer; further comprising: after the composite material cyclic densification, performing surface sealing on the obtained alumina-quartz hybrid fabric reinforced ceramic matrix composite material, and the surface sealing uses a mixture of one or both of quartz powder or quartz / quartz composite material powder and silica sol in a mass ratio of 1:(0.2-5).
2. The alumina-quartz hybrid fabric reinforced ceramic matrix composite material according to claim 1, characterized in that: the core fabric is one or more of the following: an alumina-quartz hybrid fabric woven by mixing alumina fiber bundles and quartz fiber bundles, an alumina-quartz hybrid fabric woven by alumina fiber and quartz fiber, and a fabric obtained by superimposing and needling a combination of alumina fabric and quartz fabric.
3. The alumina-quartz hybrid fabric reinforced ceramic matrix composite material according to claim 2, characterized in that: the surface layer fabric and the core fabric are connected by needling and sewing.
4. The alumina-quartz hybrid fabric reinforced ceramic matrix composite material according to claim 1, characterized in that: in step S3, the curing temperature is 100-250℃, and the curing time is 24-100h. Step S2 specifically comprises the following steps: placing the reinforcing material in a vacuum impregnation device, vacuumizing the vacuum impregnation device, then sucking in silica sol with a density of 1.1-1.5 g / cm 3 for 2-24 h under vacuum condition; In step S4, the atmosphere for sintering is one or more of nitrogen, ammonia, argon, or a mixture thereof, or a vacuum environment, the temperature for sintering is 300-900℃, and the time for sintering is 1-3h.
Citation Information
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Preparation method of laminated fiber fabric reinforced composite material radome
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