CN110563478B - Fiber-reinforced ceramic matrix composite material and preparation method and application thereof - Google Patents
Fiber-reinforced ceramic matrix composite material and preparation method and application thereof Download PDFInfo
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- C04B35/71—Ceramic products containing macroscopic reinforcing agents
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- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/82—Asbestos; Glass; Fused silica
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- F27—FURNACES; KILNS; OVENS; RETORTS
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Abstract
The invention relates to a fiber reinforced ceramic matrix composite material and a preparation method and application thereof. The preparation method comprises the steps of (1) preparing glue solution for impregnating the fiber preform, (2) vacuum impregnation, (3) curing, (4) drying and sintering and (5) densification, and the following steps are also included between the steps (2) and (3): carrying out ultrasonic vibration on a system comprising the fiber preform and a glue solution for impregnation after vacuum impregnation; and (ii) introducing compressed gas into the environment of the system after the ultrasonic vibration is finished, and pressurizing to ensure that the pressure of the environment of the system reaches 1-4MPa and the maintaining time is 1-24 h. The fiber reinforced ceramic matrix composite with the thickness of more than 50mm and still having higher density, more excellent tensile strength and interlaminar shear strength can be prepared by the preparation method.
Description
Technical Field
The invention relates to the technical field of fiber reinforced ceramic matrix composite materials, in particular to a fiber reinforced ceramic matrix composite material and a preparation method and application thereof.
Background
The fiber reinforced ceramic matrix composite material has excellent thermal property and mechanical property. The preparation technology of the composite material is mastered in European and American countries such as America, Germany and the like, and the composite material is used for key parts such as a combustion chamber of an aerospace engine, a hot end part of a tail nozzle, a thermal protection structural part of an aircraft and the like. However, in China, the technical development of the composite material is slow, a mature manufacturing process is not formed, and even a plurality of technical details cannot be broken through.
At present, the preparation process of fiber reinforced ceramic matrix composite materials which is widely applied in China is a sol-gel method, namely, three-dimensional fabrics are soaked into sol, gel is filled in pores of the fiber fabrics by inducing sol reaction, and the composite materials are obtained by drying and sintering; the composite material is densified through multiple dipping cycles to obtain a final product. However, in the densification process, the impregnation difficulty of the sol particles is increased, the distribution uniformity of the sol particles in the fabric is gradually reduced, the sol particles are more difficult to enter the fabric closer to the interior of the fabric, and the density of the interior is relatively low, so that the reliability of the performance of the composite material is severely restricted. In order to solve the problem of high difficulty in dipping the sol particles, in the prior art, the dipping is assisted by a vacuumizing method in the dipping process, so that the problem of uneven dipping is solved to a great extent. However, when the thickness of the woven fabric is 50mm or more, the problem of unevenness of the composite material still remains. Therefore, the current sol-gel method is suitable for preparing the small-thickness fiber reinforced ceramic matrix composite material, and the large-thickness fiber reinforced ceramic matrix composite material cannot be prepared.
For example, in patent application publication No. CN109293385A, the whole fabric preform is immersed in an immersion tank containing silica sol during immersion, then the immersion tank is sealed and vacuumized until the vacuum degree is-0.06 to-0.1 MPa, the vacuum degree is maintained for 60 to 120min after the target vacuum degree is reached, after the pressure maintaining is finished, an air inlet valve of the immersion tank is opened to return to normal pressure, and the fabric is taken out. Although the method can obtain the fiber reinforced ceramic matrix composite material with excellent mechanical property and ablation resistance, the thickness of the composite material is not more than 20 mm.
For example, the preparation method disclosed in chinese patent application publication No. CN108911776A is an improvement of the fiber preform, and a vacuum impregnation method is used in the impregnation stage. The method can obtain the fiber reinforced ceramic matrix composite material with better heat insulation performance and scour resistance, but the thickness of the composite material is not more than 30 mm.
For example, chinese patent application publication No. CN101880172A discloses a method for manufacturing a preform, in which a "gapped pipe" is used to create a gap in the preform, and the preform is immersed by vacuum assisted transfer molding for multiple times after drying. Although the method can obtain the fiber reinforced ceramic matrix composite material with better mechanical property and fracture toughness, the thickness of the composite material still has a larger difference with the thickness requirement of a large-thickness composite material product.
Therefore, how to provide a preparation process of a fiber reinforced ceramic matrix composite with large thickness becomes a technical problem to be solved at present.
Disclosure of Invention
Aiming at the defects or shortcomings in the prior art, the invention aims to solve the technical problems that: provides a preparation process of a large-thickness fiber reinforced ceramic matrix composite.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of a fiber reinforced ceramic matrix composite comprises the steps of (1) preparing glue solution for impregnating a fiber preform, (2) vacuum impregnation, (3) curing, (4) drying and sintering, and (5) densification, and the preparation method further comprises the following steps between the steps (2) and (3):
carrying out ultrasonic vibration on a system comprising the fiber preform and a glue solution for impregnation after finishing vacuum impregnation, wherein the ultrasonic power is 50-1000W, the ultrasonic frequency is 20-40KHz, and the ultrasonic energy transmission rate is as follows: 0.1-3w/g, and the ultrasonic time is 0.5-8 h; and
(ii) introducing compressed gas into the environment of the system after the ultrasonic vibration is finished, and pressurizing to ensure that the pressure of the environment of the system reaches 1-4MPa and the maintaining time is 1-24 h.
Preferably, the glue solution comprises a sol;
preferably, the sol is selected from any one or more of silica sol, alumina sol, mullite sol.
Preferably, the glue solution for impregnation further comprises ceramic powder;
preferably, the ceramic powder is selected from any one or more of glass powder, alumina powder, mullite powder, zirconia powder, boron nitride powder and silicon nitride powder;
more preferably, the ceramic powder has the following gradation:
the powder with the particle size less than 100nm accounts for 5-15%, the powder with the particle size of 100nm-200nm accounts for 70-80%, and the powder with the particle size greater than 200nm accounts for 5-15%;
preferably, the mass ratio of the ceramic powder to the sol is (3-4): 2.
preferably, the fiber preform is made of a three-dimensional fiber fabric selected from any one or more of a quartz fiber fabric, an alumina fiber fabric, a mullite fiber fabric, a carbon fiber fabric, a silicon nitride fiber fabric, and a silicon boron nitrogen fiber fabric;
preferably, the thickness of the fiber preform is greater than or equal to 50 mm.
Preferably, the step (2) is performed as follows: placing the fiber preform in a dipping tool, vacuumizing, injecting glue solution into the dipping tool, and enabling the glue solution to sink through the fiber preform;
preferably, the vacuum degree of the vacuum pumping is 0.01-0.1 MPa.
Preferably, in step (3), the curing is carried out at 50 to 90 ℃.
Preferably, in step (4), the drying is performed as follows: firstly, carrying out primary drying under the conditions of constant temperature and constant humidity, wherein the temperature is 30-60 ℃, the humidity is 50-100%, and then carrying out secondary conventional drying, wherein the temperature is 50-250 ℃; and/or
The sintering is carried out at the temperature of 1000 ℃ and 1300 ℃ for 1-3 h.
Preferably, said step (5) is carried out by cycling steps (2) to (4) a number of times until the material density reaches 60-90% of the theoretical density.
A fiber reinforced ceramic matrix composite prepared by any one of the above preparation methods;
the fiber reinforced ceramic matrix composite material has one or more of the following characteristics:
the thickness is more than or equal to 50 mm;
the normal temperature tensile strength is 80-130 MPa;
the interlaminar shear strength is 3-10 MPa.
The fiber reinforced ceramic matrix composite is applied to civil high-temperature furnace linings or aviation weapon hot end components.
Advantageous effects
The technical scheme of the invention has the following advantages:
the preparation method provided by the invention improves the existing sol-gel method: firstly, carry out ultrasonic vibration to the system that contains fibre preform and glue solution after accomplishing vacuum impregnation, the ultrasonic wave can promote the brownian motion of micelle, promotes the micelle and breaks through the separation of fibre silk bundle, realizes combined material's even flooding to can prepare the combined material of large thickness. In addition, the introduction of ultrasonic waves can break residual micro-pores among the fiber monofilaments, which is beneficial to improving the density of the composite material; and secondly, pressurizing a system containing the fiber preform and the glue solution after ultrasonic vibration, further compressing air holes in the fabric, and reducing the volume fraction of the air holes to the lowest. Through detection, the fiber reinforced ceramic matrix composite with the thickness of more than 50mm and still having higher density, more excellent tensile strength and interlaminar shear strength can be prepared by using the preparation method provided by the invention.
The preparation method provided by the invention has the advantages of simple and convenient process, low requirements on fiber weaving performance, and good densification effect without improving the structure of the fiber preform.
The preparation method provided by the invention also discloses a great deal of technical details, and the preparation process is explained in detail, so that the preparation method is a feasible production and preparation process of the fiber reinforced ceramic matrix composite.
Drawings
FIG. 1 is a schematic flow diagram of a preparation method provided by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In a first aspect, the present invention provides a method of making a fiber reinforced ceramic matrix composite. The method improves the existing sol-gel method: firstly, carry out ultrasonic vibration to the system that contains fibre preform and glue solution after accomplishing vacuum impregnation, the ultrasonic wave can promote the brownian motion of micelle, promotes the micelle and breaks through the separation of fibre silk bundle, realizes combined material's even flooding to can prepare the combined material of large thickness. In addition, the introduction of ultrasonic waves can break residual micro-pores among the fiber monofilaments, which is beneficial to improving the density of the composite material; and secondly, pressurizing a system containing the fiber preform and the glue solution after ultrasonic vibration, further compressing air holes in the fabric, and reducing the volume fraction of the air holes to the lowest.
Specifically, referring to FIG. 1, the method for preparing a fiber reinforced ceramic matrix composite according to the present invention comprises the following steps:
preparing glue solution for dipping the fiber preform;
vacuum dipping the fiber preform into the glue solution;
carrying out ultrasonic vibration on the system which is subjected to vacuum impregnation and contains the fiber preform and the impregnation glue solution;
introducing compressed gas into the environment where the system is located after the ultrasonic vibration is finished to pressurize;
curing the pressurized material;
drying and sintering the cured material in sequence;
and (3) densifying the sintered material.
In addition, the invention optimizes the specific technical parameters in the two steps of ultrasonic vibration and pressurization. The better technical conditions of ultrasonic vibration are as follows: the ultrasonic power when ultrasonic vibration is carried out is controlled to be 50-1000W, for example, 50W, 100W, 150W, 200W, 250W, 300W, 350W, 400W, 450W, 500W, 550W, 600W, 650W, 700W, 750W, 800W, 850W, 900W, 950W, 1000W, the ultrasonic frequency is 20-40KHz, for example, 20KHz, 30KHz, 40KHz, the ultrasonic energy delivery rate: 0.1 to 3w/g, for example, 0.1w/g, 0.5w/g, 1w/g, 1.5w/g, 2w/g, 2.5w/g, 3w/g, and the ultrasonic time is 0.5 to 8 hours, for example, 0.5 hour, 1 hour, 1.5 hour, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours, 5.5 hours, 8 hours. More preferably, the ultrasonic power is 100-. Most preferably, the ultrasonic power is 500-. The ultrasonic waves emitted by larger ultrasonic power and frequency can better promote the Brownian motion of colloidal particles and better promote the colloidal particles to break through the obstruction of fiber tows, so that the impregnation effect of the composite material is more uniform, and simultaneously, the residual micropores between the fiber monofilaments can be crushed, thereby being beneficial to improving the density of the composite material. However, the inventors have found in their studies that the ultrasound power and frequency continue to increase without the expected improvement. When the ultrasonic power exceeds 1000W and/or the ultrasonic frequency is 40KHz, the number of air holes in the composite material is increased, so that the impregnation density of the composite material is low, the temperature of the sol is increased quickly, the stability of the sol is reduced, and the operation process is not facilitated. Therefore, the ultrasonic frequency is controlled to be 50-1000W, the ultrasonic frequency is controlled to be 20-40KHz, the ultrasonic energy delivery rate is as follows: 0.1-3w/g, and the ultrasonic time is controlled to be 0.5-8 h.
The preferable pressurizing technical conditions are as follows: the pressure of the environment of the system is 1-4MPa, for example, 1MPa, 2MPa, 3MPa and 4MPa, and the pressure is maintained for 1-24h, for example, 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h, 10h, 11h, 12h, 13h, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h, 23h and 24 h. Too large pressure not only improves the compactness of the material to a small extent, but also greatly improves the risk of actual operation.
In addition, the invention not only optimizes the technical parameters of the ultrasonic vibration step and the pressurizing step, but also optimizes the technical details of the other steps, and the method specifically comprises the following steps:
in some preferred embodiments, the glue solution comprises a sol. Preferably, the sol is selected from any one or more of silica sol, alumina sol, mullite sol.
In some preferred embodiments, the impregnation cement further comprises ceramic powder. Preferably, the ceramic powder is selected from any one or more of glass powder, alumina powder, mullite powder, zirconia powder, boron nitride powder and silicon nitride powder. More preferably, the ceramic powder has the following gradation: the powder with a particle size of less than 100nm accounts for 5-15%, the powder with a particle size of 100nm-200nm accounts for 70-80%, and the powder with a particle size of more than 200nm accounts for 5-15%. The grain diameter of the ceramic powder is less than 100nm, the viscosity of the slurry is greatly improved, and the doping amount is difficult to ensure. The ceramic powder has a particle size of more than 200nm, and the activity of the powder is too low to form a high-strength matrix after sintering. The ceramic powder with a certain grain size grading can ensure that the viscosity of the dipping material is not too high and the activity is relatively high under the condition of fully ensuring the solid content of the powder. For the proportioning relation of the ceramic powder and the sol, the invention preferably selects the mass ratio of the ceramic powder to the sol as (3-4): 2. the ceramic powder accounts for too much, the viscosity of the glue solution is large, and the glue solution is difficult to enter the braided fabric.
In some preferred embodiments, the fiber preform is made of a three-dimensional fiber fabric selected from any one or more of a quartz fiber fabric, an alumina fiber fabric, a mullite fiber fabric, a carbon fiber fabric, a silicon nitride fiber fabric, and a silicon boron nitrogen fiber fabric. Preferably, the thickness of the fiber preform is greater than or equal to 50 mm.
In some preferred embodiments, the step (2) is performed as follows: and placing the fiber preform in a dipping tool, vacuumizing, injecting glue solution into the dipping tool, and enabling the glue solution to sink over the fiber preform. The degree of vacuum of the evacuation is preferably 0.01 to 0.1MPa, and may be, for example, 0.01MPa, 0.02MPa, 0.03MPa, 0.04MPa, 0.05MPa, 0.06MPa, 0.07MPa, 0.08MPa, 0.09MPa, or 0.1 MPa.
In some preferred embodiments, in step (3), the curing is performed at 50 to 90 ℃ (e.g., may be 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃).
In some preferred embodiments, in step (4), the drying is performed according to the following method: first drying under constant temperature and humidity conditions of 30-60 deg.C, such as 30 deg.C, 35 deg.C, 40 deg.C, 45 deg.C, 50 deg.C, 55 deg.C, 60 deg.C, and humidity conditions (relative humidity) of 50-100%, such as 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 100%, and then performing second conventional drying under temperature conditions of 50-250 deg.C, such as 50 deg.C, 55 deg.C, 60 deg.C, 65 deg.C, 70 deg.C, 75 deg.C, 85 deg.C, 95 deg.C, 100 deg.C, 150 deg.C, 200 deg.C, and 250 deg.C.
In some preferred embodiments, the sintering is performed under conditions of a sintering temperature of 1000 ℃ to 1300 ℃, for example, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃, 1250 ℃, 1300 ℃, and a sintering time of 1 to 3 hours, for example, 1 hour, 1.5 hours, 2 hours, 2.5 hours, and 3 hours.
In some preferred embodiments, densification is achieved by multiple cycles of the vacuum impregnation described above-the ultrasonic vibration described above-the pressurization described above-the curing described above-the drying described above-the sintering described above, until the material density reaches 60-90% of the theoretical density.
Most fully, the preparation method provided by the invention comprises the following steps:
preparing glue solution for dipping the fiber preform;
vacuum dipping the fiber preform into the glue solution;
carrying out ultrasonic vibration on the system which is subjected to vacuum impregnation and contains the fiber preform and the impregnation glue solution;
introducing compressed gas into the environment where the system is located after the ultrasonic vibration is finished to pressurize;
curing the pressurized material;
drying and sintering the cured material in sequence;
and (3) densifying the sintered material.
The ultrasonic power is controlled to be 50-1000W when ultrasonic vibration is carried out, the ultrasonic frequency is controlled to be 20-40KHz, and the ultrasonic energy delivery rate is as follows: 0.1-3W/g, the ultrasonic time is 0.5-8h, more preferably, the ultrasonic power is 300-. Most preferably, the ultrasonic power is 600- & lt1000 & gtW, and the ultrasonic time is 1-2 h. The pressurizing technical conditions are as follows: the pressure of the environment of the system reaches 1-4MPa by introducing compressed gas, and the system is maintained for 1-24h under the pressure condition.
The glue solution comprises a sol. Preferably, the sol is selected from any one or more of silica sol, alumina sol, mullite sol.
The glue solution for impregnation also comprises ceramic powder. The ceramic powder is selected from any one or more of glass powder, alumina powder, mullite powder, zirconia powder, boron nitride powder and silicon nitride powder. The ceramic powder has the following grading: the powder with a particle size of less than 100nm accounts for 5-15%, the powder with a particle size of 100nm-200nm accounts for 70-80%, and the powder with a particle size of more than 200nm accounts for 5-15%. For the proportioning relation of the ceramic powder and the sol, the mass ratio of the ceramic powder to the sol is (3-4): 2.
the fiber preform is a three-dimensional fiber fabric, and the three-dimensional fiber fabric is any one or more of a quartz fiber fabric, an alumina fiber fabric, a mullite fiber fabric, a carbon fiber fabric, a silicon nitride fiber fabric and a silicon boron nitrogen fiber fabric. The thickness of the fiber preform is more than or equal to 50 mm.
The step (2) is carried out according to the following method: and placing the fiber preform in a dipping tool, vacuumizing, injecting glue solution into the dipping tool, and enabling the glue solution to sink over the fiber preform. Preferably, the vacuum degree of the vacuum pumping is 0.01-0.1 MPa.
In step (3), the curing is carried out at 50 to 90 ℃.
In the step (4), the drying is performed as follows: first drying under constant temperature and humidity conditions (30-60 deg.C and humidity (relative humidity) of 50-100%), and then performing second conventional drying at 50-250 deg.C.
When sintering is carried out, the sintering temperature condition is 1000-1300 ℃, and the sintering time condition is 1-3 h.
Densification was achieved by multiple cycles of the above-mentioned vacuum impregnation-the above-mentioned ultrasonic vibration-the above-mentioned pressurization-the above-mentioned curing-the above-mentioned drying-the above-mentioned sintering until the material density reached 60-90% of the theoretical density.
The preparation method provided by the invention has the following advantages:
the preparation method provided by the invention improves the existing sol-gel method: firstly, carry out ultrasonic vibration to the system that contains fibre preform and glue solution after accomplishing vacuum impregnation, the ultrasonic wave can promote the brownian motion of micelle, promotes the micelle and breaks through the separation of fibre silk bundle, realizes combined material's even flooding to can prepare the combined material of large thickness. In addition, the introduction of ultrasonic waves can break residual micro-pores among the fiber monofilaments, which is beneficial to improving the density of the composite material; and secondly, pressurizing a system containing the fiber preform and the glue solution after ultrasonic vibration, further compressing air holes in the fabric, and reducing the volume fraction of the air holes to the lowest. Through detection, the fiber reinforced ceramic matrix composite with the thickness of more than 50mm and still having higher density, more excellent tensile strength and interlaminar shear strength can be prepared by using the preparation method provided by the invention.
The preparation method provided by the invention has the advantages of simple and convenient process, low requirements on fiber weaving performance, and good densification effect without improving the structure of the fiber preform.
The preparation method provided by the invention also discloses a great deal of technical details, and the preparation process is explained in detail, so that the preparation method is a feasible production and preparation process of the fiber reinforced ceramic matrix composite.
In a second aspect, the present invention provides a fiber reinforced ceramic matrix composite material made by the method of the present invention. The fiber reinforced ceramic matrix composite material has one or more of the following characteristics: the thickness is more than or equal to 50 mm; the normal temperature tensile strength is 80-130 MPa; the interlaminar shear strength is 3-10 MPa. The density of the composite material obtained by using the alumina fiber braided fabric and soaking silica sol according to the preparation method provided by the invention reaches 2.0g/cm3. The fiber reinforced ceramic matrix composite provided by the invention can be applied to civil high-temperature furnace linings or aviation weapon hot end components.
The following are examples of the present invention.
Example 1
Firstly, a fiber preform made of quartz fiber fabric and having a thickness of 50mm is placed in a dipping tool, and an ultrasonic device is arranged in the dipping tool and used for carrying out ultrasonic vibration. And vacuumizing the tool by 0.1MPa, pumping the silica sol into the tool, and finishing the glue feeding after the slurry passes through the fabric. Then, start ultrasonic device, carry out ultrasonic vibration to fibre preform and glue solution in the frock, the inside gas pocket that persists of broken and the exclusion fabric, ultrasonic power is 50W, ultrasonic frequency 20KHz, ultrasonic energy transfer rate: 0.1w/g and the ultrasonic time is 0.5 h. And then, introducing compressed air into the tool to enable the inside of the tool to have 1MPa of air pressure, wherein the pressing time is 1 h. And then, placing the whole tool in an oven at 50 ℃ to initiate the gelation reaction of the slurry in the tool, so that the slurry in the preform is solidified and left in the preform. And secondly, after taking out the fiber preform, carrying out constant-temperature constant-humidity drying at the temperature of 30 ℃ and the humidity of 50%, carrying out conventional drying at the temperature of 50 ℃, and sintering at the temperature of 1000 ℃ for 1h to obtain the composite material. Finally, the fiber reinforced composite material is subjected to vacuum impregnation, ultrasonic vibration, pressurization, curing, drying and sintering circulation, so that the density of the ceramic reaches 60% of the theoretical density.
Example 2
Firstly, a fiber preform with the thickness of 50mm, which is made of an alumina fiber fabric, is placed in a dipping tool, and an ultrasonic device is arranged in the dipping tool and is used for carrying out ultrasonic vibration. And vacuumizing the tool by 0.1MPa, pumping the silica sol into the tool, and finishing the glue feeding after the slurry passes through the fabric. Then, start ultrasonic device, carry out ultrasonic vibration to fibre preform and glue solution in the frock, the inside gas pocket that persists of broken and the exclusion fabric, ultrasonic power is 50W, ultrasonic frequency 20KHz, ultrasonic energy transfer rate: 0.1w/g and the ultrasonic time is 0.5 h. And then, introducing compressed air into the tool to enable the inside of the tool to have 1MPa of air pressure, wherein the pressing time is 1 h. And then, placing the whole tool in an oven at 50 ℃ to initiate the gelation reaction of the slurry in the tool, so that the slurry in the preform is solidified and left in the preform. And secondly, after taking out the fiber preform, carrying out constant-temperature constant-humidity drying at the temperature of 30 ℃ and the humidity of 50%, conventionally drying at the temperature of 50 ℃, and sintering at the temperature of 1200 ℃ for 1h to obtain the composite material. Finally, the fiber reinforced composite material is subjected to vacuum impregnation, ultrasonic vibration, pressurization, curing, drying and sintering circulation, so that the density of the ceramic reaches 60% of the theoretical density.
Example 3
Firstly, a fiber preform with the thickness of 50mm, which is made of an alumina fiber fabric, is placed in a dipping tool, and an ultrasonic device is arranged in the dipping tool and is used for carrying out ultrasonic vibration. And vacuumizing the tool by 0.05MPa, pumping the silica sol into the tool, and finishing the glue feeding after the slurry passes through the fabric. Then, start ultrasonic device, carry out ultrasonic vibration to fibre preform and glue solution in the frock, the inside gas pocket that persists of broken and the exclusion fabric, ultrasonic power is 100W, ultrasonic frequency 25KHz, ultrasonic energy transfer rate: 0.5w/g and the ultrasonic time is 1 h. And then, introducing compressed air into the tool to enable the inside of the tool to have 1MPa of air pressure, wherein the pressing time is 1 h. And then, placing the whole tool in an oven at 50 ℃ to initiate the gelation reaction of the slurry in the tool, so that the slurry in the preform is solidified and left in the preform. And secondly, after taking out the fiber preform, carrying out constant-temperature constant-humidity drying at the temperature of 30 ℃ and the humidity of 50%, conventionally drying at the temperature of 50 ℃, and sintering at the temperature of 1200 ℃ for 1h to obtain the composite material. Finally, the fiber reinforced composite material is subjected to vacuum impregnation, ultrasonic vibration, pressurization, curing, drying and sintering circulation, so that the density of the ceramic reaches 60% of the theoretical density.
Example 4
Firstly, a fiber preform with the thickness of 50mm, which is made of an alumina fiber fabric, is placed in a dipping tool, and an ultrasonic device is arranged in the dipping tool and is used for carrying out ultrasonic vibration. And vacuumizing the tool by 0.05MPa, pumping the mullite sol into the tool, and finishing the glue feeding after the slurry passes through the fabric. Then, start ultrasonic device, carry out ultrasonic vibration to fibre preform and glue solution in the frock, the inside gas pocket that persists of broken and the exclusion fabric, ultrasonic power is 100W, ultrasonic frequency 25KHz, ultrasonic energy transfer rate: 0.5w/g and the ultrasonic time is 1 h. And then, introducing compressed air into the tool to enable the inside of the tool to have 1MPa of air pressure, wherein the pressing time is 1 h. And then, placing the whole tool in an oven at 50 ℃ to initiate the gelation reaction of the slurry in the tool, so that the slurry in the preform is solidified and left in the preform. And secondly, after taking out the fiber preform, carrying out constant-temperature constant-humidity drying at the temperature of 30 ℃ and the humidity of 50%, conventionally drying at the temperature of 50 ℃, and sintering at the temperature of 1200 ℃ for 1h to obtain the composite material. Finally, the fiber reinforced composite material is subjected to vacuum impregnation, ultrasonic vibration, pressurization, curing, drying and sintering circulation, so that the density of the ceramic reaches 60% of the theoretical density.
Example 5
Firstly, a fiber preform with the thickness of 50mm, which is made of an alumina fiber fabric, is placed in a dipping tool, and an ultrasonic device is arranged in the dipping tool and is used for carrying out ultrasonic vibration. And vacuumizing the tool by 0.05MPa, pumping the mullite sol into the tool, and finishing the glue feeding after the slurry passes through the fabric. Then, start ultrasonic device, carry out ultrasonic vibration to fibre preform and glue solution in the frock, the inside gas pocket that persists of broken and the exclusion fabric, ultrasonic power is 500W, ultrasonic frequency 30KHz, ultrasonic energy transfer rate: 1w/g and the ultrasonic time is 2 h. And then, introducing compressed air into the tool to enable the inside of the tool to have 2MPa of air pressure, wherein the pressing time is 2 h. And then, placing the whole tool in an oven at 50 ℃ to initiate the gelation reaction of the slurry in the tool, so that the slurry in the preform is solidified and left in the preform. And secondly, after taking out the fiber preform, carrying out constant-temperature constant-humidity drying at the temperature of 30 ℃ and the humidity of 50%, conventionally drying at the temperature of 50 ℃, and sintering at the temperature of 1200 ℃ for 1h to obtain the composite material. Finally, the fiber reinforced composite material is subjected to vacuum impregnation, ultrasonic vibration, pressurization, curing, drying and sintering circulation, so that the density of the ceramic reaches 60% of the theoretical density.
Example 6
Firstly, a fiber preform with the thickness of 50mm, which is made of an alumina fiber fabric, is placed in a dipping tool, and an ultrasonic device is arranged in the dipping tool and is used for carrying out ultrasonic vibration. And vacuumizing the tool by 0.05MPa, pumping the mullite sol into the tool, and finishing the glue feeding after the slurry passes through the fabric. Then, start ultrasonic device, carry out ultrasonic vibration to fibre preform and glue solution in the frock, the inside gas pocket that persists of broken and the exclusion fabric, ultrasonic power is 500W, ultrasonic frequency 30KHz, ultrasonic energy transfer rate: 1w/g and the ultrasonic time is 2 h. And then, introducing compressed air into the tool to enable the inside of the tool to have 2MPa of air pressure, wherein the pressing time is 2 h. And then, placing the whole tool in an oven at 80 ℃ to initiate the gelation reaction of the slurry in the tool, so that the slurry in the preform is solidified and left in the preform. And secondly, after taking out the fiber preform, carrying out constant-temperature constant-humidity drying at the temperature of 30 ℃ and the humidity of 50%, carrying out conventional drying at the temperature of 50 ℃, and sintering at 1250 ℃ for 2h to obtain the composite material. Finally, the fiber reinforced composite material is subjected to vacuum impregnation, ultrasonic vibration, pressurization, curing, drying and sintering circulation, so that the density of the ceramic reaches 80% of the theoretical density.
Example 7
Firstly, a fiber preform with the thickness of 50mm, which is made of an alumina fiber fabric, is placed in a dipping tool, and an ultrasonic device is arranged in the dipping tool and is used for carrying out ultrasonic vibration. And vacuumizing the tool by 0.05MPa, pumping the mullite sol into the tool, and finishing the glue feeding after the slurry passes through the fabric. Then, start ultrasonic device, carry out ultrasonic vibration to fibre preform and glue solution in the frock, the inside gas pocket that persists of broken and the exclusion fabric, ultrasonic power is 500W, ultrasonic frequency 30KHz, ultrasonic energy transfer rate: 1.5w/g and the ultrasonic time is 2 h. And then, introducing compressed air into the tool to enable the inside of the tool to have 2MPa of air pressure, wherein the pressing time is 2 h. And then, placing the whole tool in an oven at 80 ℃ to initiate the gelation reaction of the slurry in the tool, so that the slurry in the preform is solidified and left in the preform. And secondly, after taking out the fiber preform, carrying out constant-temperature constant-humidity drying at 50 ℃ and 70% of humidity, conventionally drying at 80 ℃, and sintering at 1300 ℃ for 3h to obtain the composite material. Finally, the fiber reinforced composite material is subjected to vacuum impregnation, ultrasonic vibration, pressurization, curing, drying and sintering circulation, so that the density of the ceramic reaches 85% of the theoretical density.
Example 8
Firstly, a fiber preform with the thickness of 50mm, which is made of an alumina fiber fabric, is placed in a dipping tool, and an ultrasonic device is arranged in the dipping tool and is used for carrying out ultrasonic vibration. The tool is vacuumized by 0.05MPa, the mixed slurry of mullite sol and glass powder (the glass powder used in the embodiment has the following grading that the powder with the particle size of less than 100nm accounts for 5 percent, the powder with the particle size of 100nm-200nm accounts for 80 percent, and the powder with the particle size of more than 200nm accounts for 15 percent) is pumped into the tool, and the slurry is pumped into the tool after passing through the fabric. Then, start ultrasonic device, carry out ultrasonic vibration to fibre preform and glue solution in the frock, the inside gas pocket that persists of broken and the exclusion fabric, ultrasonic power is 500W, ultrasonic frequency 30KHz, ultrasonic energy transfer rate: 2w/g and the ultrasonic time is 2 h. And then, introducing compressed air into the tool to enable the inside of the tool to have 2MPa of air pressure, wherein the pressing time is 2 h. And then, placing the whole tool in an oven at 80 ℃ to initiate the gelation reaction of the slurry in the tool, so that the slurry in the preform is solidified and left in the preform. And secondly, after taking out the fiber preform, carrying out constant-temperature constant-humidity drying at 50 ℃ and the humidity of 70 percent, conventionally drying at 80 ℃, and sintering at 1250 ℃ for 3h to obtain the composite material. Finally, the fiber reinforced composite material is subjected to vacuum impregnation, ultrasonic vibration, pressurization, curing, drying and sintering circulation, so that the density of the ceramic reaches 85% of the theoretical density.
Example 9
Firstly, a fiber preform made of an alumina fiber fabric and having a thickness of 70mm is placed in a dipping tool, and an ultrasonic device is arranged in the dipping tool and used for carrying out ultrasonic vibration. The tool is vacuumized by 0.05MPa, the mixed slurry of mullite sol and glass powder (the glass powder used in the embodiment has the following grading that the powder with the particle size of less than 100nm accounts for 15%, the powder with the particle size of 100-200 nm accounts for 80%, and the powder with the particle size of more than 200nm accounts for 5%) is pumped into the tool, and the slurry is pumped into the tool after passing through the fabric. Then, start ultrasonic device, carry out ultrasonic vibration to fibre preform and glue solution in the frock, the inside gas pocket that persists of broken and the exclusion fabric, ultrasonic power is 1000W, ultrasonic frequency 40KHz, ultrasonic energy transfer rate: 3w/g and the ultrasonic time is 1 h. And then, introducing compressed air into the tool to enable the inside of the tool to have 2MPa of air pressure, wherein the pressing time is 2 h. And then, placing the whole tool in an oven at 80 ℃ to initiate the gelation reaction of the slurry in the tool, so that the slurry in the preform is solidified and left in the preform. And secondly, after taking out the fiber preform, carrying out constant-temperature constant-humidity drying at 50 ℃ and the humidity of 70 percent, conventionally drying at 80 ℃, and sintering at 1200 ℃ for 3 hours to obtain the composite material. Finally, the fiber reinforced composite material is subjected to vacuum impregnation, ultrasonic vibration, pressurization, curing, drying and sintering circulation, so that the density of the ceramic reaches 90% of the theoretical density.
Example 10
Firstly, a fiber preform with the thickness of 50mm, which is made of an alumina fiber fabric, is placed in a dipping tool, and an ultrasonic device is arranged in the dipping tool and is used for carrying out ultrasonic vibration. And vacuumizing the tool by 0.05MPa, pumping the mullite sol into the tool, and finishing the glue feeding after the slurry passes through the fabric. Then, start ultrasonic device, carry out ultrasonic vibration to fibre preform and glue solution in the frock, the inside gas pocket that persists of broken and the exclusion fabric, ultrasonic power is 1500W, ultrasonic frequency 50KHz, ultrasonic energy transfer rate: 4w/g and the ultrasonic time is 2 h. The stability of the mullite sol under the ultrasonic condition is greatly reduced, and the mullite sol can not be used continuously after one-time impregnation. And then, introducing compressed air into the tool to enable the inside of the tool to have 2MPa of air pressure, wherein the pressing time is 2 h. And then, placing the whole tool in an oven at 80 ℃ to initiate the gelation reaction of the slurry in the tool, so that the slurry in the preform is solidified and left in the preform. And secondly, after taking out the fiber preform, carrying out constant-temperature constant-humidity drying at 50 ℃ and 70% of humidity, conventionally drying at 80 ℃, and sintering at 1300 ℃ for 3h to obtain the composite material. Finally, the fiber reinforced composite material is subjected to vacuum impregnation, ultrasonic vibration, pressurization, curing, drying and sintering circulation, so that the density of the ceramic reaches 85% of the theoretical density.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A preparation method of a fiber reinforced ceramic matrix composite, which comprises the steps of (1) preparing glue solution for impregnating a fiber preform, (2) vacuum impregnation, (3) curing, (4) drying and sintering, and (5) densification, and is characterized by further comprising the following steps between the step (2) and the step (3):
carrying out ultrasonic vibration on a system comprising the fiber preform and a glue solution for impregnation after finishing vacuum impregnation, wherein the ultrasonic power is 50-1000W, the ultrasonic frequency is 20-40KHz, and the ultrasonic energy transmission rate is as follows: 0.1-3w/g, and the ultrasonic time is 2-8 h; and
(ii) introducing compressed gas into the environment of the system after the ultrasonic vibration is finished to pressurize, so that the pressure of the environment of the system reaches 1-4MPa, and the maintaining time is 1-24 h;
wherein the thickness of the fiber preform is more than or equal to 50 mm;
the glue solution comprises sol and ceramic powder;
the mass ratio of the ceramic powder to the sol is (3-4): 2;
the ceramic powder has the following grading:
the powder with the particle size less than 100nm accounts for 5-15%, the powder with the particle size of 100nm-200nm accounts for 70-80%, and the powder with the particle size greater than 200nm accounts for 5-15%;
the step (5) is realized by repeatedly circulating the steps (2) to (4) until the density of the material reaches 60 to 90 percent of the theoretical density.
2. The production method according to claim 1,
the sol is selected from any one or more of silica sol, alumina sol and mullite sol.
3. The production method according to claim 2,
the ceramic powder is selected from any one or more of alumina powder, mullite powder, zirconia powder, boron nitride powder and silicon nitride powder.
4. The production method according to claim 1,
the fiber preform is made of three-dimensional fiber fabric, and the three-dimensional fiber fabric is selected from any one or more of quartz fiber fabric, alumina fiber fabric, mullite fiber fabric, carbon fiber fabric, silicon nitride fiber fabric and silicon boron nitrogen fiber fabric.
5. The production method according to claim 1,
the step (2) is carried out according to the following method: placing the fiber preform in a dipping tool, vacuumizing, injecting glue solution into the dipping tool, and enabling the glue solution to sink through the fiber preform;
the vacuum degree of the vacuum pumping is 0.01-0.1 MPa.
6. The production method according to claim 1,
in step (3), the curing is carried out at 50 to 90 ℃.
7. The production method according to claim 1,
in the step (4), the drying is performed as follows: firstly, carrying out primary drying under the conditions of constant temperature and constant humidity, wherein the temperature is 30-60 ℃, the humidity is 50-100%, and then carrying out secondary conventional drying, wherein the temperature is 50-250 ℃; and/or
The sintering is carried out at the temperature of 1000 ℃ and 1300 ℃ for 1-3 h.
8. A fiber reinforced ceramic matrix composite characterized in that,
prepared by the preparation method of any one of claims 1 to 7;
the fiber reinforced ceramic matrix composite material has one or more of the following characteristics:
the thickness is more than or equal to 50 mm;
the normal temperature tensile strength is 80-130 MPa;
the interlaminar shear strength is 3-10 MPa.
9. Use of the fiber reinforced ceramic matrix composite according to claim 8 in civil high temperature furnace linings or hot end components for aeroweapons.
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| CN111978092B (en) * | 2020-09-01 | 2022-04-29 | 航天特种材料及工艺技术研究所 | Preparation method of fiber-reinforced ceramic matrix composite |
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| CN115894056A (en) * | 2022-07-11 | 2023-04-04 | 东华大学 | Preparation method and forming device of three-dimensional alumina fiber reinforced zirconia ceramic composite material |
| CN115286371A (en) * | 2022-07-27 | 2022-11-04 | 航天特种材料及工艺技术研究所 | SiO (silicon dioxide) 2f /SiO 2 Composite material and preparation method thereof |
| CN115636682A (en) * | 2022-11-02 | 2023-01-24 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of alumina fiber-based rigid heat insulation material |
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