CN111978092B - Preparation method of fiber-reinforced ceramic matrix composite - Google Patents

Preparation method of fiber-reinforced ceramic matrix composite Download PDF

Info

Publication number
CN111978092B
CN111978092B CN202010902472.1A CN202010902472A CN111978092B CN 111978092 B CN111978092 B CN 111978092B CN 202010902472 A CN202010902472 A CN 202010902472A CN 111978092 B CN111978092 B CN 111978092B
Authority
CN
China
Prior art keywords
ultrasonic
fiber
fiber preform
powder
sol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202010902472.1A
Other languages
Chinese (zh)
Other versions
CN111978092A (en
Inventor
孙志强
张剑
吴涛
杨小波
慈吉良
吕毅
张昊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Aerospace Research Institute of Materials and Processing Technology
Original Assignee
Aerospace Research Institute of Materials and Processing Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Aerospace Research Institute of Materials and Processing Technology filed Critical Aerospace Research Institute of Materials and Processing Technology
Priority to CN202010902472.1A priority Critical patent/CN111978092B/en
Publication of CN111978092A publication Critical patent/CN111978092A/en
Application granted granted Critical
Publication of CN111978092B publication Critical patent/CN111978092B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C04B35/82—Asbestos; Glass; Fused silica
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/185—Mullite 3Al2O3-2SiO2
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/624—Sol-gel processing
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/616—Liquid infiltration of green bodies or pre-forms

Abstract

The invention relates to a preparation method of a fiber reinforced ceramic matrix composite, which comprises the step of impregnating a fiber preform with glue solution, wherein during impregnation, ultrasonic treatment is carried out according to the following conditions: thickness of the fiber preform is d1The ultrasonic frequency is 20-40Hz, the ultrasonic energy delivery efficiency is 0-5w/g, and the ultrasonic time is 10-30 min; thickness of the fiber preform is d2The ultrasonic frequency is 25-45Hz, the ultrasonic energy delivery efficiency is 5-10w/g, and the ultrasonic time is 30-40 min; thickness of the fiber preform is d3When in use, the ultrasonic frequency is 30-50Hz, the ultrasonic energy delivery efficiency is 10-20w/g, and the ultrasonic time is 40-50 min; thickness of the fiber preform is d4The ultrasonic frequency is 35-55Hz, the ultrasonic energy transmission efficiency is 20-30w/g, and the ultrasonic time is 60-90 min. The method enables the application of the ultrasonic treatment process to be more extensive.

Description

Preparation method of fiber-reinforced ceramic matrix composite
Technical Field
The invention relates to the technical field of fiber reinforced ceramic matrix composite materials, and relates to a preparation method of a fiber reinforced ceramic matrix composite material.
Background
The fiber reinforced ceramic matrix composite has the advantages of high temperature resistance, oxidation resistance, wear resistance, corrosion resistance and the like of ceramic materials, and has excellent external impact load resistance due to the reinforcing and toughening effects of the fibers. The fiber reinforced ceramic matrix composite is more and more widely applied in the fields of advanced aircraft engine hot end parts, advanced aircraft thermal protection systems and the like by virtue of good high-temperature stability and high-temperature mechanical properties. 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, for the composite preparation of the large-thickness three-dimensional fabric, the common process method is insufficient, and the uniformity is difficult to realize.
The ultrasonic dipping and sol-gel process is a novel process, and can obviously improve the thickness of the composite material prepared uniformly.
Disclosure of Invention
Technical problem to be solved
The inventors have found that the ultrasound parameter requirements for different thicknesses are different. The invention aims to provide a preparation process of a ceramic matrix composite material suitable for fiber preforms with different thicknesses.
(II) technical scheme
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 step of impregnating a fiber preform with glue solution, and during impregnation, ultrasonic treatment is carried out according to the following conditions:
thickness of the fiber preform is d1When d is greater than1Less than 20mm, and the process conditions of ultrasonic treatment are as follows: the ultrasonic frequency is 20-40Hz, the ultrasonic energy delivery efficiency is 0-5w/g, and the ultrasonic time is 10-30 min;
thickness of the fiber preform is d2When d is more than or equal to 20mm2Less than 30mm, and the process conditions of ultrasonic treatment are as follows: the ultrasonic frequency is 25-45Hz, the ultrasonic energy delivery efficiency is 5-10w/g, and the ultrasonic time is 30-40 min;
thickness of the fiber preform is d3When d is more than or equal to 30mm3Less than 50mm, and the process conditions of ultrasonic treatment are as follows: the ultrasonic frequency is 30-50Hz, the ultrasonic energy delivery efficiency is 10-20w/g, and the ultrasonic time is 40-50 min;
thickness of the fiber preform is d4When d is greater than4More than 50mm, and the process conditions of ultrasonic treatment are as follows: the ultrasonic frequency is 35-55Hz, the ultrasonic energy transmission efficiency is 20-30w/g, and the ultrasonic time is 60-90 min.
Preferably, the fiber preform is a flat plate-shaped structure;
preferably, the fiber preform is a flat plate-shaped structure formed by stacking three-dimensional fiber fabric plies.
Preferably, the fiber type in the fiber preform is selected from any one or more of quartz fiber, alumina fiber, mullite fiber, carbon fiber, silicon nitride fiber, and silicon boron nitrogen fiber.
Preferably, the glue solution comprises sol and/or ceramic powder;
preferably, the glue solution comprises ceramic powder and sol, and the mass ratio of the ceramic powder to the sol is (1-10): 2.
preferably, the sol is selected from any one or more of silica sol, alumina sol, mullite sol; and/or
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.
Preferably, 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%.
Preferably, the method comprises:
providing glue solution;
dipping the fiber preform by using glue solution;
a step of curing;
a step of drying; and
and (4) sintering.
Preferably, the impregnation mode is vacuum impregnation, and the impregnation is preferably carried out in a vacuum environment with the vacuum degree of 0.01-0.1 MPa;
curing at 50-90 deg.C;
drying was carried out 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
Sintering at 1000-1300 deg.C for 1-3 h.
Preferably, the method further comprises the step of densifying;
preferably, the material density is brought to 65-95% of the theoretical density by densification.
Preferably, said densifying is achieved by cycling said impregnating, said curing, said drying and said sintering.
(III) advantageous effects
The technical scheme of the invention has the following advantages:
the invention provides a method and a rule for changing technological parameters of ultrasonic treatment. The process parameter change method is mainly used for corresponding to the change of ultrasonic frequency, energy transmission efficiency and ultrasonic time after the thickness of the prefabricated body is changed, so that the application of the ultrasonic treatment process is wider and more important. Through detection, the density of the composite material can reach more than 65%.
The method provided by the invention can be used for dipping by using the glue solution containing high ceramic powder content, so that the compactness of the composite material is improved to a certain extent. In addition, even if the glue solution with high ceramic powder content is used for impregnation, the invention can still obtain uniform impregnation effect.
Drawings
FIG. 1 is a schematic flow diagram of a 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.
The invention provides a preparation method of a fiber reinforced ceramic matrix composite, which comprises the step of impregnating a fiber preform with glue solution, wherein during impregnation, ultrasonic treatment is carried out according to the following conditions:
a preparation method of a fiber reinforced ceramic matrix composite comprises the step of impregnating a fiber preform with glue solution, and during impregnation, ultrasonic treatment is carried out according to the following conditions:
thickness of the fiber preform is d1When d is greater than1Less than 20mm, sonicatedThe process conditions are as follows: the ultrasonic frequency is 20-40Hz, the ultrasonic energy delivery efficiency is 0-5w/g, and the ultrasonic time is 10-30 min;
thickness of the fiber preform is d2When d is more than or equal to 20mm2Less than 30mm, and the process conditions of ultrasonic treatment are as follows: the ultrasonic frequency is 25-45Hz, the ultrasonic energy delivery efficiency is 5-10w/g, and the ultrasonic time is 30-40 min;
thickness of the fiber preform is d3When d is more than or equal to 30mm3Less than 50mm, and the process conditions of ultrasonic treatment are as follows: the ultrasonic frequency is 30-50Hz, the ultrasonic energy delivery efficiency is 10-20w/g, and the ultrasonic time is 40-50 min;
thickness of the fiber preform is d4When d is greater than4More than 50mm, and the process conditions of ultrasonic treatment are as follows: the ultrasonic frequency is 35-55Hz, the ultrasonic energy transmission efficiency is 20-30w/g, and the ultrasonic time is 60-90 min.
The invention provides a method and a rule for changing technological parameters of ultrasonic treatment. The process parameter change method is mainly used for corresponding to the change of ultrasonic frequency, energy transmission efficiency and ultrasonic time after the thickness of the prefabricated body is changed, so that the application of the ultrasonic treatment process is wider and more important. Through detection, the density of the composite material can reach more than 65%.
In some preferred embodiments, the fiber preform has a flat plate-shaped structure. Further preferably, the fiber preform is a flat plate-shaped structure formed by stacking three-dimensional fiber fabric plies.
In some preferred embodiments, the glue solution comprises a sol and/or a ceramic powder. More specifically, the glue solution comprises ceramic powder and sol, and the mass ratio of the ceramic powder to the sol is (1-10): 2, e.g. 1:1, 1:2, 3:2, 2:1, 5:2, 3:1, 7:2, 4:1, 9:2, 5: 1. The invention optimizes the ultrasonic frequency, energy transmission efficiency and ultrasonic time according to the thickness of the prefabricated body. Therefore, in the method provided by the invention, the glue solution containing high ceramic powder content can be used for impregnation, so that the compactness of the composite material is improved to a certain extent. In addition, even if the glue solution with high ceramic powder content is used for impregnation, the invention can still obtain uniform impregnation effect.
In some preferred embodiments, the fiber type in the fiber preform is selected from any one or more of quartz fiber, alumina fiber, mullite fiber, carbon fiber, silicon nitride fiber, silicon boron nitrogen fiber.
In some preferred embodiments, the sol is selected from any one or more of a silica sol, an alumina sol, a mullite sol.
In some preferred embodiments, 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%.
Referring to fig. 1, the method provided by the present invention comprises:
providing glue solution;
dipping the fiber preform by using glue solution;
a step of curing;
a step of drying; and
and (4) sintering.
In some preferred embodiments, the impregnation mode is vacuum impregnation, and more preferably, the impregnation is performed in a vacuum environment with a vacuum degree of 0.01 to 0.1 MPa.
In some preferred embodiments, curing is carried out at 50-90 ℃.
In some preferred embodiments, the drying is carried out as follows: first drying under constant temperature and humidity conditions, the temperature is 30-60 ℃, the humidity is 50-100%, and then second conventional drying is carried out, the temperature is 50-250 ℃.
In some preferred embodiments, the sintering is carried out at 1000-1300 ℃ for 1-3 hours.
In some preferred embodiments, the method further comprises the step of densifying. Preferably, the material density is brought to 65-95% of the theoretical density by densification. The densification may be achieved by cycling the impregnating, the curing, the drying, and the sintering.
The following are examples of the present invention.
Example 1
Laying layers of quartz fiber fabrics, stacking the layers to prepare a fiber preform with the thickness of 50mm, placing the fiber preform in a dipping tool, wherein an ultrasonic device is arranged in the dipping tool and used for carrying out ultrasonic treatment. And vacuumizing the tool by 0.1MPa, and pumping the silica sol into the tool to ensure that the sol liquid submerges the fiber preform.
And starting an ultrasonic device, and carrying out ultrasonic treatment on the fiber preform and the glue solution in the tool, wherein the ultrasonic frequency is 35Hz, the ultrasonic energy delivery rate is 20w/g, and the ultrasonic time is 65 min.
And (3) placing the whole tool in a 50 ℃ oven to initiate the gelation reaction of the slurry in the tool, so that the slurry in the prefabricated body is solidified and left in the prefabricated body.
Taking out the fiber preform, drying the fiber preform at a constant temperature and humidity of 30 ℃ and a humidity of 60%, and then drying the fiber preform at a temperature of 50 ℃ in a conventional manner.
And sintering the dried material at 1000 ℃ for 1 h.
Then, the series of steps of vacuum impregnation, ultrasonic treatment, curing, drying and sintering are repeated, so that the compactness of the composite material reaches 70%.
Example 2
Laying layers of quartz fiber fabrics, stacking the layers to prepare a fiber preform with the thickness of 55mm, placing the fiber preform in a dipping tool, wherein an ultrasonic device is arranged in the dipping tool and used for carrying out ultrasonic treatment. And vacuumizing the tool by 0.1MPa, and pumping the silica sol into the tool to ensure that the sol liquid submerges the fiber preform.
And starting an ultrasonic device, and carrying out ultrasonic treatment on the fiber preform and the glue solution in the tool, wherein the ultrasonic frequency is 50Hz, the ultrasonic energy transmission rate is 25w/g, and the ultrasonic time is 60 min.
And (3) placing the whole tool in a 60-DEG C oven to initiate the gelation reaction of the slurry in the tool, so that the slurry in the prefabricated body is solidified and left in the prefabricated body.
Taking out the fiber preform, drying the fiber preform at a constant temperature and humidity of 40 ℃ and a humidity of 50%, and then drying the fiber preform at a temperature of 60 ℃ in a conventional manner.
The dried material was sintered at 1100 ℃ for 1 h.
Then, the series of steps of vacuum impregnation, ultrasonic treatment, curing, drying and sintering are repeated, so that the compactness of the composite material reaches 65 percent.
Example 3
Laying layers of quartz fiber fabrics, stacking the layers to form a fiber preform with the thickness of 60mm, placing the fiber preform in a dipping tool, and arranging an ultrasonic device in the dipping tool for ultrasonic treatment. And vacuumizing the tool by 0.01MPa, and pumping the silica sol into the tool to ensure that the sol liquid submerges the fiber preform.
And starting an ultrasonic device, and carrying out ultrasonic treatment on the fiber preform and the glue solution in the tool, wherein the ultrasonic frequency is 55Hz, the ultrasonic energy transmission rate is 30w/g, and the ultrasonic time is 65 min.
And (3) placing the whole tool in a 60-DEG C oven to initiate the gelation reaction of the slurry in the tool, so that the slurry in the prefabricated body is solidified and left in the prefabricated body.
Taking out the fiber preform, drying the fiber preform at a constant temperature and humidity of 50 ℃ and at a humidity of 50%, and then drying the fiber preform at a temperature of 60 ℃ in a conventional manner.
The dried material was sintered at 1100 ℃ for 1 h.
Then, the series of steps of vacuum impregnation, ultrasonic treatment, curing, drying and sintering are repeated, so that the compactness of the composite material reaches 70%.
Example 4
Laying layers of the alumina fiber fabric to be stacked to prepare a fiber preform with the thickness of 60mm, placing the fiber preform in a dipping tool, wherein an ultrasonic device is arranged in the dipping tool and used for carrying out ultrasonic treatment. Vacuumizing the tool by 0.05MPa, and pumping glue solution (comprising mullite sol and glass powder, wherein the mass ratio of the mullite sol to the glass powder is 1:1, and the used glass powder has the following grading that powder with the particle size of less than 100nm accounts for 15%, powder with the particle size of 100-200 nm accounts for 80%, and powder with the particle size of more than 200nm accounts for 5%) into the tool to ensure that the glue solution submerges the fiber preform.
And starting an ultrasonic device, and carrying out ultrasonic treatment on the fiber preform and the glue solution in the tool, wherein the ultrasonic frequency is 55Hz, the ultrasonic energy transmission rate is 30w/g, and the ultrasonic time is 60 min.
And (3) 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 prefabricated body is solidified and left in the prefabricated body.
Taking out the fiber preform, drying the fiber preform at a constant temperature and humidity of 50 ℃ and a humidity of 60%, and then drying the fiber preform at a temperature of 100 ℃ in a conventional manner.
And sintering the dried material at 1200 ℃ for 1 h.
Then, the series of steps of vacuum impregnation, ultrasonic treatment, curing, drying and sintering are repeated, so that the compactness of the composite material reaches 95%.
Example 5
Laying layers of the alumina fiber fabric to be stacked to prepare a fiber preform with the thickness of 60mm, placing the fiber preform in a dipping tool, wherein an ultrasonic device is arranged in the dipping tool and used for carrying out ultrasonic treatment. Vacuumizing the tool by 0.01MPa, and pumping glue solution (comprising mullite sol and glass powder, wherein the mass ratio of the mullite sol to the glass powder is 3:1, and the used glass powder has the following grading that powder with the particle size of less than 100nm accounts for 15%, powder with the particle size of 100-200 nm accounts for 80%, and powder with the particle size of more than 200nm accounts for 5%) into the tool to ensure that the glue solution submerges the fiber preform.
And starting an ultrasonic device, and carrying out ultrasonic treatment on the fiber preform and the glue solution in the tool, wherein the ultrasonic frequency is 55Hz, the ultrasonic energy transmission rate is 30w/g, and the ultrasonic time is 90 min.
And (3) 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 prefabricated body is solidified and left in the prefabricated body.
Taking out the fiber preform, drying the fiber preform at a constant temperature and humidity of 70 ℃ and a humidity of 60%, and then drying the fiber preform at a temperature of 120 ℃ in a conventional manner.
And sintering the dried material at 1200 ℃ for 1.5 h.
Then, the series of steps of vacuum impregnation, ultrasonic treatment, curing, drying and sintering are repeated, so that the compactness of the composite material reaches 95%.
Example 6
Laying layers of quartz fiber fabrics, stacking the layers to prepare a fiber preform with the thickness of 30mm, placing the fiber preform in a dipping tool, wherein an ultrasonic device is arranged in the dipping tool and used for carrying out ultrasonic treatment. And vacuumizing the tool by 0.1MPa, and pumping the silica sol into the tool to ensure that the sol liquid submerges the fiber preform.
And starting an ultrasonic device, and carrying out ultrasonic treatment on the fiber preform and the glue solution in the tool, wherein the ultrasonic frequency is 30Hz, the ultrasonic energy transmission rate is 15w/g, and the ultrasonic time is 40 min.
And (3) placing the whole tool in a 50 ℃ oven to initiate the gelation reaction of the slurry in the tool, so that the slurry in the prefabricated body is solidified and left in the prefabricated body.
Taking out the fiber preform, drying the fiber preform at a constant temperature and humidity of 30 ℃ and a humidity of 60%, and then drying the fiber preform at a temperature of 50 ℃ in a conventional manner.
And sintering the dried material at 1000 ℃ for 1 h.
Then, the series of steps of vacuum impregnation, ultrasonic treatment, curing, drying and sintering are repeated, so that the compactness of the composite material reaches 80 percent.
Example 7
Laying layers of quartz fiber fabrics, stacking the layers to prepare a fiber preform with the thickness of 20mm, placing the fiber preform in a dipping tool, wherein an ultrasonic device is arranged in the dipping tool and used for carrying out ultrasonic treatment. And vacuumizing the tool by 0.1MPa, and pumping the silica sol into the tool to ensure that the sol liquid submerges the fiber preform.
And starting an ultrasonic device, and carrying out ultrasonic treatment on the fiber preform and the glue solution in the tool, wherein the ultrasonic frequency is 25Hz, the ultrasonic energy transmission rate is 5w/g, and the ultrasonic time is 30 min.
And (3) placing the whole tool in a 50 ℃ oven to initiate the gelation reaction of the slurry in the tool, so that the slurry in the prefabricated body is solidified and left in the prefabricated body.
Taking out the fiber preform, drying the fiber preform at a constant temperature and humidity of 30 ℃ and a humidity of 60%, and then drying the fiber preform at a temperature of 50 ℃ in a conventional manner.
And sintering the dried material at 1000 ℃ for 1 h.
Then, the series of steps of vacuum impregnation, ultrasonic treatment, curing, drying and sintering are repeated, so that the compactness of the composite material reaches 85%.
Example 8
Laying layers of quartz fiber fabrics, stacking the layers to form a fiber preform with the thickness of 10mm, placing the fiber preform in a dipping tool, and arranging an ultrasonic device in the dipping tool for ultrasonic treatment. And vacuumizing the tool by 0.1MPa, and pumping the silica sol into the tool to ensure that the sol liquid submerges the fiber preform.
And starting an ultrasonic device, and carrying out ultrasonic treatment on the fiber preform and the glue solution in the tool, wherein the ultrasonic frequency is 20Hz, the ultrasonic energy transmission rate is 1w/g, and the ultrasonic time is 15 min.
And (3) placing the whole tool in a 50 ℃ oven to initiate the gelation reaction of the slurry in the tool, so that the slurry in the prefabricated body is solidified and left in the prefabricated body.
Taking out the fiber preform, drying the fiber preform at a constant temperature and humidity of 30 ℃ and a humidity of 60%, and then drying the fiber preform at a temperature of 50 ℃ in a conventional manner.
And sintering the dried material at 1000 ℃ for 1 h.
Then, the series of steps of vacuum impregnation, ultrasonic treatment, curing, drying and sintering are repeated, so that the compactness of the composite material reaches 85%.
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 (5)

1. A preparation method of a fiber reinforced ceramic matrix composite comprises the step of impregnating a fiber preform with glue solution, and is characterized in that during impregnation, ultrasonic treatment is carried out according to the following conditions:
thickness of the fiber preform is d1When d is greater than1Less than 20mm, and the process conditions of ultrasonic treatment are as follows: the ultrasonic frequency is 20-40Hz, the ultrasonic energy delivery efficiency is 0-5w/g, and the ultrasonic time is 10-30 min;
thickness of the fiber preform is d2When d is more than or equal to 20mm2Less than 30mm, and the process conditions of ultrasonic treatment are as follows: the ultrasonic frequency is 25-45Hz, the ultrasonic energy delivery efficiency is 5-10w/g, and the ultrasonic time is 30-40 min;
thickness of the fiber preform is d3When d is more than or equal to 30mm3Less than 50mm, and the process conditions of ultrasonic treatment are as follows: the ultrasonic frequency is 30-50Hz, the ultrasonic energy delivery efficiency is 10-20w/g, and the ultrasonic time is 40-50 min;
thickness of the fiber preform is d4When d is greater than4More than 50mm, and the process conditions of ultrasonic treatment are as follows: the ultrasonic frequency is 35-55Hz, the ultrasonic energy conveying efficiency is 20-30w/g, and the ultrasonic time is 60-90 min;
the glue solution comprises ceramic powder and sol, and the mass ratio of the ceramic powder to the sol is (1-10): 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 fiber prefabricated body is of a flat plate structure formed by stacking three-dimensional fiber fabric layers.
2. The production method according to claim 1,
the fiber type in the fiber preform is selected from any one or more of quartz fiber, alumina fiber, mullite fiber, carbon fiber, silicon nitride fiber and silicon boron nitrogen fiber.
3. The production method according to claim 1,
the sol is selected from any one or more of silica sol, alumina sol and mullite sol;
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.
4. The production method according to any one of claims 1 to 3,
the method comprises the following steps:
providing glue solution;
dipping the fiber preform by using glue solution;
a step of curing;
a step of drying;
sintering;
and (5) densifying.
5. The production method according to claim 4,
the impregnation mode is that the impregnation is carried out in a vacuum environment with the vacuum degree of 0.01-0.1 MPa;
curing at 50-90 deg.C;
drying was carried out 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 ℃;
sintering at 1000-1300 deg.C for 1-3 h;
the density of the material is increased to 65-95% of the theoretical density by the densification;
said densifying is achieved by cycling said impregnating, said curing, said drying and said sintering.
CN202010902472.1A 2020-09-01 2020-09-01 Preparation method of fiber-reinforced ceramic matrix composite Active CN111978092B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010902472.1A CN111978092B (en) 2020-09-01 2020-09-01 Preparation method of fiber-reinforced ceramic matrix composite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010902472.1A CN111978092B (en) 2020-09-01 2020-09-01 Preparation method of fiber-reinforced ceramic matrix composite

Publications (2)

Publication Number Publication Date
CN111978092A CN111978092A (en) 2020-11-24
CN111978092B true CN111978092B (en) 2022-04-29

Family

ID=73447116

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010902472.1A Active CN111978092B (en) 2020-09-01 2020-09-01 Preparation method of fiber-reinforced ceramic matrix composite

Country Status (1)

Country Link
CN (1) CN111978092B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113061046A (en) * 2021-03-19 2021-07-02 中建材飞渡航天科技有限公司 Preparation method and application of silicon-boron-nitrogen fiber reinforced boron nitride ceramic matrix composite material
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

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108191446A (en) * 2018-02-09 2018-06-22 青海大学 A kind of ceramic based structures Wave suction composite material of silicon carbide fibre enhancing and preparation method thereof
CN110526728A (en) * 2019-10-15 2019-12-03 航天特种材料及工艺技术研究所 A kind of fiber reinforcement does not carry out ceramic matric composite and preparation method thereof
CN110563478A (en) * 2019-10-15 2019-12-13 航天特种材料及工艺技术研究所 fiber-reinforced ceramic matrix composite material and preparation method and application thereof
US20200208035A1 (en) * 2014-05-14 2020-07-02 Aleksandar GRUJICIC Fiber and nanomaterial composite material and method for making thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04101831A (en) * 1990-08-22 1992-04-03 Nissan Motor Co Ltd Winding method for filament

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20200208035A1 (en) * 2014-05-14 2020-07-02 Aleksandar GRUJICIC Fiber and nanomaterial composite material and method for making thereof
CN108191446A (en) * 2018-02-09 2018-06-22 青海大学 A kind of ceramic based structures Wave suction composite material of silicon carbide fibre enhancing and preparation method thereof
CN110526728A (en) * 2019-10-15 2019-12-03 航天特种材料及工艺技术研究所 A kind of fiber reinforcement does not carry out ceramic matric composite and preparation method thereof
CN110563478A (en) * 2019-10-15 2019-12-13 航天特种材料及工艺技术研究所 fiber-reinforced ceramic matrix composite material and preparation method and application thereof

Also Published As

Publication number Publication date
CN111978092A (en) 2020-11-24

Similar Documents

Publication Publication Date Title
CN111978092B (en) Preparation method of fiber-reinforced ceramic matrix composite
CN110526728B (en) Fiber-reinforced mullite ceramic matrix composite material and preparation method thereof
CN110563478B (en) Fiber-reinforced ceramic matrix composite material and preparation method and application thereof
CN109384470B (en) Rapid preparation method of C/C composite material
CN107353025B (en) Preparation method of 1200-DEG C-resistant and oxidation-resistant ceramic matrix composite
CN106866151B (en) Method for preparing carbon fiber toughened zirconium boride-silicon carbide composite material by slurry injection process
CN104311090B (en) A kind of hot pressed sintering/presoma cracking process prepares the method for Cf/ZrC-SiC ultrahigh temperature ceramic composite
CN109251052B (en) C/C composite material and preparation method thereof
CN108101566B (en) Method for preparing silicon carbide ceramic matrix composite component with assistance of RTM (resin transfer molding) process
CN105254320A (en) Preparation method of continuous oxide fiber reinforced oxide ceramic based composite
CN112341235B (en) Multiphase coupling rapid densification method for ultrahigh-temperature self-healing ceramic matrix composite
CN108484194B (en) Al (aluminum)2O3-SiO2Base composite material and rapid preparation method thereof
CN111217617A (en) Ultrahigh-temperature large-scale complex carbon/carbon material component
CN112142435A (en) Wet-process-formed flexible nano heat-insulating material and preparation method thereof
CN111908932B (en) Light high-efficiency heat-proof and heat-insulating integrated heat protection material and preparation method thereof
CN112645725B (en) Ceramic matrix composite material component with step structure and preparation method thereof
CN111454071B (en) Rock wool fiber reinforced silica-based high-strength heat insulation composite material and preparation method thereof
CN109608218B (en) Self-healing ceramic matrix composite and low-temperature rapid preparation method thereof
CN108774072B (en) Rigid heat insulation tile and preparation method thereof
CN114716258B (en) Preparation method of carbon fiber reinforced boron carbide composite material
CN107602127A (en) SiC hollow sphere and preparation method thereof
CN114605161B (en) Ceramic matrix composite with high fiber volume content and preparation method thereof
CN104478460A (en) Preparation method of fiber-enhanced silicon carbide composite material
CN114853480B (en) Low-cost rapid preparation method of high-temperature wave-transparent nitride composite material radome
CN115417683A (en) Preparation method of oxide continuous filament reinforced oxide ceramic matrix composite

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant