CN115448741A - Method for preparing alumina fiber reinforced ceramic matrix composite based on constant liquid level concentration-in-situ gel process and application thereof - Google Patents
Method for preparing alumina fiber reinforced ceramic matrix composite based on constant liquid level concentration-in-situ gel process and application thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 95
- 239000002131 composite material Substances 0.000 title claims abstract description 89
- 239000011159 matrix material Substances 0.000 title claims abstract description 79
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000007788 liquid Substances 0.000 title claims abstract description 41
- 239000011226 reinforced ceramic Substances 0.000 title claims abstract description 33
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 21
- 239000004744 fabric Substances 0.000 claims abstract description 112
- 239000002002 slurry Substances 0.000 claims abstract description 71
- 238000001035 drying Methods 0.000 claims abstract description 52
- 238000005245 sintering Methods 0.000 claims abstract description 49
- 238000005470 impregnation Methods 0.000 claims abstract description 44
- 238000007598 dipping method Methods 0.000 claims abstract description 41
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 238000009941 weaving Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- 238000003825 pressing Methods 0.000 claims abstract description 17
- 239000012141 concentrate Substances 0.000 claims abstract description 15
- 238000000280 densification Methods 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 22
- 150000001875 compounds Chemical class 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 15
- 230000001502 supplementing effect Effects 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 238000005086 pumping Methods 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000000919 ceramic Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052863 mullite Inorganic materials 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000010453 quartz Substances 0.000 claims description 7
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 6
- 238000009958 sewing Methods 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 239000012780 transparent material Substances 0.000 claims description 2
- 239000000080 wetting agent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000003054 catalyst Substances 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 230000014759 maintenance of location Effects 0.000 abstract description 3
- 238000013329 compounding Methods 0.000 abstract description 2
- 230000003247 decreasing effect Effects 0.000 description 12
- 230000000717 retained effect Effects 0.000 description 9
- 239000002245 particle Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000001879 gelation Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 230000005653 Brownian motion process Effects 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005537 brownian motion Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011153 ceramic matrix composite Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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Abstract
The invention relates to a method for preparing an alumina fiber reinforced ceramic matrix composite based on a constant liquid level concentration-in-situ gel process and application thereof. The preparation method comprises the following steps: weaving a fiber preform fabric; removing the impregnating agent; vacuum-pressing impregnation is carried out; carrying out constant liquid level reduced pressure concentration: maintaining the vacuum degree in the dipping device, stirring and heating the device to a certain temperature to concentrate low-viscosity slurry, and continuously replenishing and injecting the low-viscosity slurry from the lower part of the device, so that the slurry liquid level in the device is maintained to be constant, and the slurry in the prefabricated body and the external slurry are continuously replaced by water and matrix components, so that the matrix content in the prefabricated body is gradually increased; carrying out in-situ gel reaction; drying and sintering; and (4) carrying out multiple times of impregnation densification according to actual needs. The invention can effectively reduce the times of dipping and sintering in the compounding process and improve the strength retention rate of the fiber, thereby improving the mechanical property of the composite material and reducing the preparation cost of the composite material.
Description
Technical Field
The invention relates to the technical field of ceramic matrix composite materials, in particular to a method for preparing an alumina fiber reinforced ceramic matrix composite material based on a constant liquid level concentration-in-situ gel process and application thereof.
Background
The continuous alumina fiber reinforced ceramic matrix composite has excellent force, thermal and electrical properties, and can be widely applied to various fields as a structural material, a thermal protection material, a wave-transparent material and other structural function integrated materials. The continuous alumina fiber generally refers to Nextel550/610/720 of American 3M company, S-1920F/G of Japanese Sumitomo company and other 550/610/720 type fibers (i.e. fibers with the composition and the performance equivalent to those of the Nextel550/610/720 fibers), and the fibers are woven or mixed and woven to form a three-dimensional prefabricated fabric with a specific multi-scale structure, and then the three-dimensional prefabricated fabric is compounded with sol or a mixture thereof and the like to finally obtain the target composite material.
At present, a composite process of a prefabricated fabric reinforced ceramic matrix composite material generally comprises a dipping-in-situ gel method and a dipping-drying method, wherein the dipping-in-situ gel process depends on sol to generate a gel reaction under a certain condition, so that the sol dipped into the prefabricated fabric generates a three-dimensional network structure and is retained in situ; the impregnation-drying process is to realize the increase of the density of the composite material by the principle that the capillary force between fiber tows retains the components of the matrix. The viscosity of the slurry used in the above process must be low, typically less than 50mpa.s, because low viscosity slurries have good flow properties to ensure adequate impregnation of the slurry into the preform fabric. However, low viscosity slurries generally have a relatively low solid content, and when the composite material is required to reach an ideal density, the number of impregnation cycles required by the conventional composite process is usually not less than 10, and multiple sintering can greatly reduce the strength of the fibers, thereby reducing the mechanical properties of the composite material. Some slurry with low viscosity and high solid content, such as high-concentration silica sol, has poor stability, is easy to generate physical and chemical changes, and the sol particles exist in an agglomerated state, so that the slurry is not easy to be fully impregnated in fiber bundles, and finally the mechanical property of the composite material is influenced.
Under the technical background, how to realize uniform impregnation of the composite material by adopting low-viscosity slurry and simultaneously avoid the problems of too many impregnation times and poor composite material performance caused by low solid content of the slurry are the problems to be solved urgently in the prior composite material preparation process technology.
Disclosure of Invention
Aiming at the problems of poor performance, complicated working procedures, high cost and the like of the alumina fiber reinforced ceramic matrix composite prepared by the prior art, the invention provides a novel preparation process which can effectively reduce the times of impregnation and sintering in the composite process and improve the strength retention rate of fibers, thereby improving the mechanical property of the composite; meanwhile, the new process can reduce the use amount of the ceramic slurry and reduce the preparation cost of the composite material.
In order to solve the technical problems, the invention provides the following technical scheme:
a method for preparing an alumina fiber reinforced ceramic matrix composite based on a constant liquid level concentration-in-situ gel process comprises the following steps:
(1) Weaving a fiber preform fabric: weaving or co-weaving continuous alumina fiber into a three-dimensional prefabricated fabric with a certain structure;
(2) Removing the impregnating agent: removing the organic impregnating compound on the fiber surface of the prefabricated fabric;
(3) Vacuum-pressing impregnation: placing the prefabricated fabric in a dipping device, vacuumizing, injecting low-viscosity slurry from the lower part to enable the slurry to submerge the prefabricated fabric, then pressurizing the device by gas to promote dipping, and finally repeatedly vacuumizing and pressurizing for dipping;
(4) Constant liquid level and reduced pressure concentration: maintaining the vacuum degree in the dipping device, stirring and heating the dipping device to a certain temperature to concentrate low-viscosity slurry, and continuously replenishing and injecting the low-viscosity slurry from the lower part of the dipping device, so that the slurry liquid level in the dipping device is maintained constant, and the slurry in the prefabricated fabric and the external slurry are continuously subjected to water and matrix component replacement to gradually increase the content of the matrix component in the prefabricated fabric;
(5) In-situ gel reaction: when the slurry reaches a certain viscosity, stopping vacuumizing, stirring and supplementing the slurry, and increasing the overall temperature of the dipping device to enable the high-viscosity slurry to generate in-situ gel reaction, and the matrix component to be retained in the prefabricated fabric;
(6) And (3) drying: taking out the gel-containing prefabricated fabric, drying at constant temperature and variable humidity, and then completely drying;
(7) And (3) sintering: and (5) sintering the composite material obtained in the step (6) at a certain temperature for a certain time, and naturally cooling to obtain the alumina fiber reinforced ceramic matrix composite material.
Further, the method may further include a step (8) of impregnating and densifying the steel sheet for a plurality of times: if necessary, the alumina fiber reinforced ceramic matrix composite material is subjected to dipping, concentration, gelling, drying and sintering for multiple times, so that the density of the ceramic reaches the requirement.
Preferably, the step (1) is performed as follows:
the continuous alumina fiber comprises Nextel550/610/720 of 3M company in the United states, S-1920F/G of Sumitomo company in Japan and other 550/610/720 type fibers (i.e. fibers with composition and performance equivalent to the Nextel550/610/720 fibers).
The structure of the prefabricated fabric comprises a 2.5D structure, a three-dimensional structure, a needling structure and a sewing structure; the composition of the prefabricated body fiber comprises pure alumina fiber or alumina fiber/quartz fiber mixed weaving.
Preferably, in the step (2), the method for removing the wetting agent includes sintering, acetone cleaning and water washing. The sintering temperature is 500-800 ℃; the temperature for cleaning the acetone is 50-56 ℃; the temperature of the water washing is 60-90 ℃.
Preferably, the vacuum degree of the vacuum pumping in the step (3) is about-0.1 MPa; the air extraction time is 3-10h, so that the inside of the fiber bundle is fully exhausted;
the viscosity of the low-viscosity slurry is less than 100mpa.s, and is generally controlled below 50mpa.s;
the low-viscosity slurry is sol or a mixture of the sol and ceramic powder;
the sol comprises at least one of alumina sol, silica sol, mullite sol and mixed sol; the ceramic powder comprises at least one of alumina powder and mullite powder.
Preferably, in the step (4), the heating temperature is 40-60 ℃.
Preferably, the temperature of the in-situ gelation reaction in the step (5) is 80 to 100 ℃.
Preferably, in the step (6), the temperature of the constant-temperature humidity-changing drying is 40-50 ℃, and the humidity is 60-90% of saturated steam humidity;
the application process of the variable humidity comprises the following steps: after being moisturized for 24 hours at 90% humidity, the liquid is maintained for 24 hours at 80% humidity, then maintained for 24 hours at 70% humidity, and finally maintained for 24 hours at 60% humidity.
Preferably, in the step (7), the sintering temperature is 600-1200 ℃, and the sintering time is 0.5-3h.
Preferably, the multiple impregnation cycles in step (8) are densified, if not necessary, and may not be performed.
An alumina fiber reinforced ceramic matrix composite material is prepared by the method.
Preferably, the tensile strength of the alumina fiber reinforced ceramic matrix composite material at normal temperature is more than 100MPa.
The alumina fiber reinforced ceramic matrix composite material can be used as a structural material, a thermal protection material, a wave-transmitting material and other structural and functional integrated materials.
The invention provides a brand-new composite process technology, namely a constant liquid level concentration-in-situ gelation process. After the low-viscosity slurry is used for dipping the prefabricated body, constant liquid level reduced pressure distillation is carried out on a slurry system, the concentration of the slurry is slowly improved, water and matrix components are continuously replaced between the slurry inside and outside the fabric of the prefabricated body, the matrix content inside the fabric is continuously improved, and finally the high-concentration slurry is initiated to be gelled and solidified through temperature rise. The constant liquid level concentration means that the low-viscosity slurry continuously supplemented in the concentration process can enable the slurry in the concentration process to always have small-particle-size particles in a certain proportion, so that the sol particles are favorably fully impregnated in the fiber bundle filaments, and the overall stability of the slurry is also favorably realized. The dipping cycle times required by the constant liquid level concentration-in-situ gel process are not more than 5, the preparation period of the composite material is greatly shortened, the strength retention rate of the fiber is improved by reducing the sintering times, and the performance of the composite material is improved by 30%. Meanwhile, the use amount of the ceramic slurry is reduced to 25-35% of the original use amount, and the preparation cost of the composite material is reduced.
Specifically, the technical scheme of the invention has the following advantages:
(1) The constant liquid level concentration-in-situ gelation process used by the invention can obviously shorten the preparation period of the composite material, and the compounding times are reduced from more than or equal to 10 times to less than or equal to 5 times.
(2) The constant liquid level concentration-in-situ gel process used by the invention can reduce the use amount of the slurry to 25-35% of the original use amount, thereby greatly reducing the preparation cost of the composite material.
(3) The constant liquid level concentration-in-situ gel process used by the invention is applicable to various ceramic matrix forms, and covers sol or a mixture of sol and ceramic powder.
(4) The constant liquid level concentration-in-situ gelation process used in the invention has small damage to fibers, and the mechanical strength of the prepared composite material can be improved by more than 30 percent.
Drawings
FIG. 1 is a flow chart illustrating the preparation of an alumina fiber reinforced ceramic matrix composite in accordance with the present invention.
Fig. 2 is a schematic view of tooling used in 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 an alumina fiber reinforced ceramic matrix composite, as shown in figure 1, the preparation method comprises the following steps:
(1) Weaving a fiber three-dimensional prefabricated fabric: weaving Nextel550/610/720 or S-1920F/G or other 550/610/720 type continuous alumina fibers into alumina fibers or alumina/quartz fiber mixed woven prefabricated fabrics with a 2.5D structure or a three-dimensional structure or a needle-punched structure or a sewing structure;
(2) Removing the impregnating agent: sintering the organic impregnating compound on the surface of the prefabricated fabric at 500-800 ℃, or cleaning the organic impregnating compound by acetone at 50-60 ℃ or washing the organic impregnating compound by water at 60-90 ℃;
(3) Vacuum-pressing impregnation: and putting the prefabricated fabric into a vacuum impregnation device, and vacuumizing the device, wherein the vacuum degree is about-0.1 MPa, and the air-extracting time is 3-10h. The sol or the mixture of sol and ceramic powder is poured from below over the preform fabric. The apparatus is gas pressurized to facilitate impregnation. Finally, repeatedly vacuumizing and pressing;
(4) Constant liquid level decompression concentration: maintaining the vacuum degree in the impregnation device, stirring and heating the device to 40-60 ℃ to concentrate low-viscosity slurry, and continuously replenishing and injecting the low-viscosity slurry from the lower part of the device, so that the slurry liquid level in the device is maintained to be constant, and the slurry in the prefabricated body and the external slurry are continuously subjected to water and matrix component replacement, so that the matrix content in the prefabricated body is gradually increased;
(5) And (3) gel reaction: stopping vacuumizing, stirring and supplementing the slurry after the slurry reaches a certain viscosity, and increasing the temperature of the dipping device to 80-100 ℃ to enable the high-viscosity slurry to have a gel reaction, and the matrix components are remained in the prefabricated body;
(6) And (3) drying: taking out the gel-containing preform, drying at constant temperature and humidity of 40-50 deg.C and humidity decreasing from 90% to 60%, and drying at 80-200 deg.C for 5-12 hr;
(7) And (3) sintering: sintering the composite material at 600-1200 ℃ for 0.5-3h, and naturally cooling;
(8) And (3) impregnation and densification again: the alumina fiber reinforced ceramic matrix composite is subjected to dipping, concentration, gelling, drying and sintering for multiple times, and the normal-temperature tensile strength of the obtained composite is more than 100MPa.
Fig. 2 is a schematic view of a tooling apparatus, i.e., a dipping apparatus, used in the present invention. The working principle of the device is as follows:
1. starting a vacuum pump, and vacuumizing to ensure that the internal pressure of the tank body is-0.1 MPa. The purpose is to exhaust the gas in the fabric and facilitate the immersion of low viscosity sol.
2. And starting a liquid inlet pump, and injecting the low-viscosity sol into the tank body from a liquid inlet. When the liquid level reaches the position of the control floating ball, the liquid inlet pump automatically stops working.
3. And opening the gas cylinder to drive high-pressure air into the tank body from the upper part of the tank body, and closing the gas cylinder after maintaining the pressure for a certain time. The aim is to evacuate the air bubbles inside the fabric as much as possible.
4. And releasing the pressure, starting a vacuum pump and a stirrer, and heating the outer wall of the tank body by heating steam. Vacuum concentration is started, and the volatilized steam is discharged from the outlet of the vacuum pump. The method aims to concentrate the low-viscosity sol in the tank body and improve the solid content of the sol, and at the moment, the low-viscosity sol in the fabric and the high-viscosity sol in the tank body are replaced under the driving force of Brownian motion, so that the solid contents of the sol in the fabric and the sol in the fabric are consistent, and the solid content of the sol in the fabric is improved. Therefore, after the gel is formed, more sol particles are reserved in the fabric, the density of the composite material is increased quickly, the preparation period is short, and the performance is high.
5. Along with the reduction of the sol liquid level, the liquid level control floating ball can control the switch, so that the liquid inlet pump is started to supplement low-viscosity slurry into the tank body, and the constant liquid level concentration is realized. The purpose is as follows: the constant liquid level concentration means that the low-viscosity slurry continuously supplemented in the concentration process can enable the slurry in the concentration process to always have small-particle-size particles in a certain proportion, so that the sol particles are favorably fully impregnated in the fiber bundle filaments, and the overall stability of the slurry is also favorably realized.
6. And stopping all the devices when the sol in the tank body reaches a certain viscosity.
Example 1
Firstly, weaving S-1920 continuous alumina fibers into 2.5D structure preform fabrics; then, removing the organic impregnating compound on the surface of the prefabricated body fiber by sintering at 600 ℃; and then, placing the prefabricated fabric in a vacuum impregnation device, and vacuumizing for 3h, wherein the vacuum degree is-0.1 MPa. Then, injecting the low-viscosity alumina/silica mixed sol from the lower part to submerge the prefabricated fabric, and repeatedly pumping and pressing; then, maintaining the vacuum degree in the dipping device, stirring and heating the device to 40 ℃ to continuously concentrate the sol, and continuously injecting the low-viscosity sol from the lower part of the device, thereby maintaining the height of the liquid level to be constant, and continuously replacing water and matrix components inside and outside the fabric, so that the matrix content in the fabric is gradually increased; stopping vacuumizing, stirring and supplementing slurry when the sol in the device reaches a certain viscosity, and integrally heating the impregnation device to 80 ℃ to enable the high-concentration sol to carry out gel reaction, so that the matrix components are retained in the prefabricated fabric; taking out the gel-containing preform, drying at a constant temperature and a variable humidity, wherein the temperature is 45 ℃ and the humidity is decreased from 90% to 60%, and gradually increasing the temperature at 80-200 ℃ for drying for 12h; finally, sintering the composite material at 900 ℃ for 1h, and naturally cooling; and finally, carrying out impregnation, gelling, drying and sintering on the alumina fiber reinforced ceramic matrix composite for multiple times to obtain the composite with the normal-temperature tensile strength of more than 110MPa.
Example 2
Firstly, weaving Nextel 610 continuous alumina fibers into a three-way orthogonal structure preform fabric; then, removing the organic impregnating compound on the surface of the prefabricated body fiber by sintering at 600 ℃; and then, placing the prefabricated fabric in a vacuum impregnation device, and vacuumizing for 10h, wherein the vacuum degree is-0.1 MPa. Then, injecting low-viscosity alumina sol from the lower part to submerge the prefabricated fabric, and repeatedly pumping air and pressing; then, maintaining the vacuum degree in the dipping device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and continuously injecting the low-viscosity sol from the lower part of the device, thereby maintaining the height of the liquid level to be constant, and continuously replacing water and matrix components inside and outside the fabric, so that the matrix content in the fabric is gradually increased; stopping vacuumizing, stirring and supplementing slurry when the sol in the device reaches a certain viscosity, and integrally heating the impregnation device to 90 ℃ to enable the high-concentration sol to carry out gel reaction, so that the matrix components are retained in the prefabricated fabric; taking out the gel-containing preform, drying at a constant temperature and humidity of 40 ℃ and with humidity decreasing from 90% to 60%, and gradually heating and drying at 80-200 ℃ for 12h; finally, sintering the composite material at 1000 ℃ for 1h, and naturally cooling; and finally, carrying out dipping, gelling, drying and sintering on the alumina fiber reinforced ceramic matrix composite for multiple times to obtain the composite with the normal-temperature tensile strength of more than 240MPa.
Example 3
Firstly, weaving domestic 720-type continuous alumina fibers into a three-way orthogonal structure preform fabric; then, removing the organic impregnating compound on the surface of the prefabricated body fiber by sintering at 600 ℃; and then, placing the prefabricated fabric in a vacuum impregnation device, and vacuumizing for 3h, wherein the vacuum degree is-0.1 MPa. Then, injecting low-viscosity alumina sol from the lower part to submerge the prefabricated fabric, and repeatedly exhausting and pressing; then, maintaining the vacuum degree in the dipping device, stirring and heating the device to 60 ℃ to continuously concentrate the sol, and continuously injecting the low-viscosity sol from the lower part of the device, thereby maintaining the constant height of the liquid level, and continuously replacing water and matrix components inside and outside the fabric, so that the matrix content in the fabric is gradually increased; stopping vacuumizing, stirring and supplementing slurry when the sol in the device reaches a certain viscosity, and integrally heating the impregnation device to 100 ℃ to enable the high-concentration sol to carry out gel reaction, so that the matrix components are retained in the prefabricated fabric; taking out the gel-containing preform, drying at a constant temperature and a variable humidity, wherein the temperature is 45 ℃ and the humidity is decreased from 90% to 60%, and gradually increasing the temperature at 80-200 ℃ for drying for 5h; finally, sintering the composite material at 1200 ℃ for 1h, and naturally cooling; and finally, carrying out dipping, gelling, drying and sintering on the alumina fiber reinforced ceramic matrix composite for multiple times to obtain the composite with the normal-temperature tensile strength of more than 150MPa.
Example 4
Firstly, mixing and weaving domestic 550 type continuous alumina fiber and quartz fiber into 2.5D structure prefabricated fabric; then, cleaning and removing the organic impregnating compound on the surfaces of the prefabricated fibers by acetone at 50 ℃; and then, placing the prefabricated fabric in a vacuum impregnation device, and vacuumizing for 3h, wherein the vacuum degree is-0.1 MPa. Then, injecting the low-viscosity alumina/silica mixed sol from the lower part to submerge the prefabricated fabric, and repeatedly pumping and pressing; then, maintaining the vacuum degree in the dipping device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and continuously injecting the low-viscosity sol from the lower part of the device, thereby maintaining the height of the liquid level to be constant, and continuously replacing water and matrix components inside and outside the fabric, so that the matrix content in the fabric is gradually increased; stopping vacuumizing, stirring and supplementing slurry when the sol in the device reaches a certain viscosity, and integrally heating the impregnation device to 80 ℃ to enable the high-concentration sol to carry out gel reaction, so that the matrix components are retained in the prefabricated fabric; taking out the gel-containing preform, drying at constant temperature and humidity of 45 deg.C and humidity decreasing from 90% to 60%, and gradually heating at 80-200 deg.C for 7 hr; finally, sintering the composite material at 600 ℃ for 1h, and naturally cooling; and finally, carrying out impregnation, gelling, drying and sintering on the alumina fiber reinforced ceramic matrix composite for multiple times to obtain the composite with the normal-temperature tensile strength of more than 100MPa.
Example 5
Firstly, weaving domestic 720-type continuous alumina fibers into a three-way orthogonal structure preform fabric; then, removing the organic impregnating compound on the surface of the prefabricated fabric by washing at 60 ℃; and then, placing the prefabricated fabric in a vacuum impregnation device, and vacuumizing for 3h, wherein the vacuum degree is-0.1 MPa. Then, injecting low-viscosity alumina sol from the lower part to submerge the prefabricated fabric, and repeatedly pumping air and pressing; then, maintaining the vacuum degree in the dipping device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and continuously injecting the low-viscosity sol from the lower part of the device, thereby maintaining the height of the liquid level to be constant, and continuously replacing water and matrix components inside and outside the fabric, so that the matrix content in the fabric is gradually increased; when the sol in the device reaches a certain viscosity, stopping vacuumizing, stirring and supplementing slurry, and integrally heating the dipping device to 90 ℃ to enable high-concentration sol to carry out gel reaction, so that the matrix components are kept in the prefabricated fabric; taking out the gel-containing preform, drying at constant temperature and humidity of 45 deg.C and humidity decreasing from 90% to 60%, and gradually heating at 80-200 deg.C for drying for 12 hr; finally, sintering the composite material at 1200 ℃ for 1h, and naturally cooling; and finally, the alumina fiber reinforced ceramic matrix composite is subjected to dipping, gelling, drying and sintering for multiple times to obtain the composite with the normal-temperature tensile strength of more than 150MPa.
Example 6
Firstly, weaving Nextel 720 continuous alumina fibers into a three-way orthogonal structure preform fabric; then, removing the organic impregnating compound on the surface of the prefabricated fabric through washing at 60 ℃; and then, placing the prefabricated fabric in a vacuum impregnation device, and vacuumizing for 3h, wherein the vacuum degree is-0.1 MPa. Then, injecting low-viscosity mullite sol from the lower part to submerge the prefabricated fabric, and repeatedly pumping air and pressing; then, maintaining the vacuum degree in the dipping device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and continuously injecting the low-viscosity sol from the lower part of the device, thereby maintaining the height of the liquid level to be constant, and continuously replacing water and matrix components inside and outside the fabric, so that the matrix content in the fabric is gradually increased; stopping vacuumizing, stirring and supplementing slurry when the sol in the device reaches a certain viscosity, and integrally heating the impregnation device to 90 ℃ to enable the high-concentration sol to carry out gel reaction, so that the matrix components are retained in the prefabricated fabric; taking out the gel-containing preform, drying at a constant temperature and humidity of 50 ℃ and with humidity decreasing from 90% to 60%, and gradually heating and drying at 80-200 ℃ for 12h; finally, sintering the composite material at 1200 ℃ for 1h, and naturally cooling; and finally, carrying out dipping, gelling, drying and sintering on the alumina fiber reinforced ceramic matrix composite for multiple times to obtain the composite with the normal-temperature tensile strength of more than 180MPa.
Example 7
Firstly, weaving Nextel 720 continuous alumina fibers into a three-way orthogonal structure preform fabric; then, removing the organic impregnating compound on the surface of the prefabricated fabric through washing at 60 ℃; and then, placing the prefabricated fabric in a vacuum impregnation device, and vacuumizing for 3h, wherein the vacuum degree is-0.1 MPa. Then, injecting the mixture of the low-viscosity alumina sol and the mullite sol from the lower part to submerge the prefabricated fabric, and repeatedly pumping and pressing; then, maintaining the vacuum degree in the dipping device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and continuously injecting the low-viscosity sol from the lower part of the device, thereby maintaining the height of the liquid level to be constant, and continuously replacing water and matrix components inside and outside the fabric, so that the matrix content in the fabric is gradually increased; stopping vacuumizing, stirring and supplementing slurry when the sol in the device reaches a certain viscosity, and integrally heating the impregnation device to 90 ℃ to enable the high-concentration sol to carry out gel reaction, so that the matrix components are retained in the prefabricated fabric; taking out the gel-containing preform, drying at constant temperature and humidity of 45 deg.C and humidity decreasing from 90% to 60%, and gradually heating at 80-200 deg.C for drying for 8 hr; finally, sintering the composite material at 1200 ℃ for 1h, and naturally cooling; and finally, carrying out impregnation, gelling, drying and sintering on the alumina fiber reinforced ceramic matrix composite for multiple times to obtain the composite with the normal-temperature tensile strength of more than 160MPa.
Example 8
Firstly, weaving Nextel 720 continuous alumina fibers into a three-way orthogonal structure preform fabric; then, cleaning and removing the organic impregnating compound on the surface of the prefabricated fabric by acetone at 50 ℃; and then, placing the prefabricated fabric in a vacuum impregnation device, and vacuumizing for 3h, wherein the vacuum degree is-0.1 MPa. Then, injecting the mixture of the low-viscosity mullite sol and the alumina powder from the lower part to submerge the prefabricated fabric, and repeatedly pumping and pressing; then, maintaining the vacuum degree in the dipping device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and continuously injecting the low-viscosity sol from the lower part of the device, thereby maintaining the constant height of the liquid level, and continuously replacing water and matrix components inside and outside the fabric, so that the matrix content in the fabric is gradually increased; stopping vacuumizing, stirring and supplementing slurry when the sol in the device reaches a certain viscosity, and integrally heating the impregnation device to 80 ℃ to enable the high-concentration sol to carry out gel reaction, so that the matrix components are retained in the prefabricated fabric; taking out the gel-containing preform, drying at constant temperature and humidity of 45 deg.C and humidity decreasing from 90% to 60%, and gradually heating at 80-200 deg.C for drying for 12 hr; finally, sintering the composite material at 1200 ℃ for 1h, and naturally cooling; and finally, carrying out impregnation, gelling, drying and sintering on the alumina fiber reinforced ceramic matrix composite for multiple times to obtain the composite with the normal-temperature tensile strength of more than 150MPa.
Example 9
Firstly, nextel 720 continuous alumina fiber of American 3M company is woven into a three-way orthogonal structure preform fabric; then, cleaning and removing the organic impregnating compound on the surface of the prefabricated fabric by acetone at 50 ℃; and then, placing the prefabricated fabric in a vacuum impregnation device, and vacuumizing for 3h, wherein the vacuum degree is-0.1 MPa. Then, injecting the mixture of the low-viscosity mullite sol and the alumina powder from the lower part to submerge the prefabricated fabric, and repeatedly pumping and pressing; then, maintaining the vacuum degree in the dipping device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and continuously injecting the low-viscosity sol from the lower part of the device, thereby maintaining the height of the liquid level to be constant, and continuously replacing water and matrix components inside and outside the fabric, so that the matrix content in the fabric is gradually increased; when the sol in the device reaches a certain viscosity, stopping vacuumizing, stirring and supplementing slurry, and integrally heating the dipping device to 80 ℃ to enable high-concentration sol to carry out gel reaction, so that the matrix components are kept in the prefabricated fabric; taking out the gel-containing preform, drying at constant temperature and humidity of 45 deg.C and humidity decreasing from 90% to 60%, and gradually heating at 80-200 deg.C for drying for 12 hr; finally, sintering the composite material at 1050 ℃ for 1h, and naturally cooling; and finally, carrying out dipping, gelling, drying and sintering on the alumina fiber reinforced ceramic matrix composite for multiple times to obtain the composite with the normal-temperature tensile strength of more than 140MPa.
Example 10
Firstly, mixing and weaving domestic 550 type continuous alumina fiber and quartz fiber into 2.5D structure prefabricated fabric; then, cleaning and removing the organic impregnating compound on the surface of the prefabricated body fiber by acetone at 50 ℃; and then, placing the prefabricated fabric in a vacuum impregnation device, and vacuumizing for 3h, wherein the vacuum degree is-0.1 MPa. Then, injecting low-viscosity silica sol from the lower part to submerge the prefabricated fabric, and repeatedly pumping air and pressing; then, maintaining the vacuum degree in the dipping device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and continuously injecting the low-viscosity sol from the lower part of the device, thereby maintaining the height of the liquid level to be constant, and continuously replacing water and matrix components inside and outside the fabric, so that the matrix content in the fabric is gradually increased; when the sol in the device reaches a certain viscosity, stopping vacuumizing, stirring and supplementing slurry, and integrally heating the dipping device to 80 ℃ to enable high-concentration sol to carry out gel reaction, so that the matrix components are kept in the prefabricated fabric; taking out the gel-containing preform, drying at a constant temperature and a variable humidity, wherein the temperature is 45 ℃ and the humidity is decreased from 90% to 60%, and gradually increasing the temperature at 80-200 ℃ for drying for 12h; finally, sintering the composite material at 800 ℃ for 1h, and naturally cooling; and finally, carrying out impregnation, gelling, drying and sintering on the alumina fiber reinforced ceramic matrix composite for multiple times to obtain the composite with the normal-temperature tensile strength of more than 110MPa.
Comparative example 1 (conventional dip-in situ gel method, compare mainly with example 10)
Firstly, mixing and weaving domestic 550 type continuous alumina fiber and quartz fiber into 2.5D structure prefabricated fabric; then, cleaning and removing the organic impregnating compound on the surface of the prefabricated body fiber by acetone at 50 ℃; and then, placing the prefabricated fabric in a vacuum impregnation device, and vacuumizing for 3h, wherein the vacuum degree is-0.1 MPa. Then, injecting low-viscosity silica sol from the lower part to submerge the prefabricated fabric, and repeatedly exhausting and pressing; heating the whole dipping device to 90 ℃ to enable the sol to generate a gel reaction, so that the matrix components are kept in the prefabricated fabric; taking out the gel-containing preform, drying at constant temperature and humidity of 45 deg.C and humidity decreasing from 90% to 60%, and gradually heating at 80-200 deg.C for drying for 12 hr; finally, sintering the composite material at 800 ℃ for 1h, and naturally cooling; the alumina fiber reinforced ceramic matrix composite is subjected to dipping, gelling, drying and sintering for multiple times, and the normal-temperature tensile strength of the obtained composite is about 90MPa. It is worth noting that in the scheme, the time period is more than 40 days, and the preparation cost of the single square meter composite material is more than 10 ten thousand yuan.
Comparative example 2 (conventional dip-drying method, compare mainly with example 10)
Firstly, co-weaving domestic 550 type continuous alumina fiber and quartz fiber into 2.5D structure prefabricated fabric; then, cleaning and removing the organic impregnating compound on the surface of the prefabricated body fiber by acetone at 50 ℃; and then, placing the prefabricated fabric in a vacuum impregnation device, and vacuumizing for 3h, wherein the vacuum degree is-0.1 MPa. Then, injecting low-viscosity silica sol from the lower part to submerge the prefabricated fabric, and repeatedly pumping air and pressing; secondly, taking out the wet fabric, and then immediately carrying out gradual temperature rise drying at 50-200 ℃ in an oven, wherein the drying time is 15h; thirdly, sintering the composite material at 600 ℃ for 1h, and naturally cooling; the alumina fiber reinforced ceramic matrix composite is subjected to dipping, drying and sintering for multiple times to obtain the composite with the normal-temperature tensile strength of about 90MPa. It is worth noting that in the scheme, the time period is more than 35 days, and the preparation cost of the single square meter composite material is more than 10 ten thousand yuan.
The total time required for the composite impregnation, the cost of the slurry required to make a single square meter of flat board, and the tensile strength of the ceramic material produced were recorded for each of the examples and comparative examples above and are shown in table 1.
TABLE 1
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 should 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 (10)
1. A preparation method of a continuous alumina fiber reinforced ceramic matrix composite is characterized by comprising the following steps:
(1) Weaving or co-weaving continuous alumina fiber into a three-dimensional prefabricated fabric with a certain structure;
(2) Removing the organic impregnating compound on the fiber surface of the prefabricated fabric;
(3) Placing the prefabricated fabric in a dipping device, after vacuumizing, injecting low-viscosity slurry from the lower part to ensure that the slurry is submerged in the prefabricated fabric, then pressurizing the device with gas to promote dipping, and finally repeatedly carrying out vacuum-pressing dipping;
(4) Maintaining the vacuum degree in the impregnation device, stirring and heating the impregnation device to a certain temperature to concentrate low-viscosity slurry, and continuously replenishing and injecting the low-viscosity slurry from the lower part of the impregnation device, so that the slurry liquid level in the impregnation device is maintained constant, and the slurry in the prefabricated fabric and the external slurry continuously perform water and matrix component replacement, so that the content of the matrix component in the prefabricated fabric is gradually increased, and constant liquid level decompression concentration is realized;
(5) After the slurry reaches a certain viscosity, stopping vacuumizing, stirring and supplementing the slurry, and increasing the overall temperature of the dipping device to enable the high-viscosity slurry to generate in-situ gel reaction, and the matrix components to be remained in the prefabricated fabric;
(6) Taking out the gel-containing prefabricated fabric, drying at constant temperature and variable humidity, and then completely drying;
(7) And (4) sintering the composite material obtained in the step (6) at a certain temperature for a certain time, and naturally cooling to obtain the alumina fiber reinforced ceramic matrix composite material.
2. The preparation method according to claim 1, wherein the alumina fiber reinforced ceramic matrix composite material is subjected to the steps (3) to (7) of impregnation-concentration-gelling-drying-sintering for a plurality of times of impregnation densification according to actual needs, so that the ceramic density meets the requirement.
3. The method according to claim 1, wherein the continuous alumina fiber in step (1) comprises Nextel550/610/720, S-1920F/G and other 550/610/720 type fibers; the structure of the prefabricated fabric comprises a 2.5D structure, a three-dimensional structure, a needling structure and a sewing structure; the composition of the prefabricated body fiber comprises pure alumina fiber or alumina fiber/quartz fiber mixed weaving.
4. The manufacturing method according to claim 1, wherein in the step (2), the method for removing the wetting agent comprises sintering, acetone cleaning, water washing; the sintering temperature is 500-800 ℃; the temperature for cleaning the acetone is 50-56 ℃; the temperature of the water washing is 60-90 ℃.
5. The method for preparing the catalyst according to claim 1, wherein the degree of vacuum of the vacuum pumping in the step (3) is-0.1 MPa; the air extraction time is 3-10h, so that the inside of the fiber bundle is fully exhausted; the viscosity of the low viscosity slurry is less than 100mpa.s; the low-viscosity slurry is sol or a mixture of the sol and ceramic powder; the sol comprises alumina sol, silica sol, mullite sol and mixed sol; the powder comprises alumina powder and mullite powder.
6. The method according to claim 1, wherein the temperature of heating in the step (4) is 40 to 60 ℃; the temperature of the in-situ gel reaction in the step (5) is 80-100 ℃; the sintering temperature in the step (7) is 600-1200 ℃, and the sintering time is 0.5-3h.
7. The method according to claim 1, wherein the temperature of the constant temperature-humidity drying in the step (6) is 40 to 50 ℃ and the humidity is 60 to 90% of saturated steam humidity; the application process of the variable humidity comprises the following steps: after the moisture is preserved for 24 hours under the humidity of 90%, the moisture is preserved for 24 hours under the humidity of 80%, then the moisture is preserved for 24 hours under the humidity of 70%, and finally the moisture is preserved for 24 hours under the humidity of 60%; and then carrying out conventional drying at the temperature of 80-200 ℃ for 5-12h.
8. An alumina fiber reinforced ceramic matrix composite produced by the production method according to any one of claims 1 to 7.
9. The alumina fiber reinforced ceramic matrix composite according to claim 8, wherein the composite has an ambient tensile strength greater than 100MPa.
10. Use of the composite material according to claim 8 or 9 as a structural material and as a thermal protection material, wave-transparent material.
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