CN115448741B - 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
- Publication number
- CN115448741B CN115448741B CN202210963117.4A CN202210963117A CN115448741B CN 115448741 B CN115448741 B CN 115448741B CN 202210963117 A CN202210963117 A CN 202210963117A CN 115448741 B CN115448741 B CN 115448741B
- Authority
- CN
- China
- Prior art keywords
- slurry
- preform
- fabric
- sol
- viscosity
- 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
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 94
- 239000002131 composite material Substances 0.000 title claims abstract description 87
- 239000011159 matrix material Substances 0.000 title claims abstract description 80
- 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 69
- 239000007788 liquid Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000011226 reinforced ceramic Substances 0.000 title claims abstract description 34
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 22
- 230000008569 process Effects 0.000 title claims abstract description 21
- 239000004744 fabric Substances 0.000 claims abstract description 97
- 239000002002 slurry Substances 0.000 claims abstract description 72
- 238000001035 drying Methods 0.000 claims abstract description 53
- 238000005245 sintering Methods 0.000 claims abstract description 47
- 238000005470 impregnation Methods 0.000 claims abstract description 42
- 238000010438 heat treatment Methods 0.000 claims abstract description 41
- 238000003756 stirring Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 239000012141 concentrate Substances 0.000 claims abstract description 14
- 238000009941 weaving Methods 0.000 claims abstract description 13
- 238000007598 dipping method Methods 0.000 claims abstract description 7
- 239000000080 wetting agent Substances 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 16
- 238000001816 cooling Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 12
- 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
- 238000004140 cleaning Methods 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 9
- 229910052863 mullite Inorganic materials 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 8
- 239000010453 quartz Substances 0.000 claims description 7
- 238000005406 washing Methods 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
- 230000005653 Brownian motion process Effects 0.000 claims description 2
- 238000005537 brownian motion Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims description 2
- 238000009940 knitting Methods 0.000 claims description 2
- 239000012466 permeate Substances 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000013329 compounding Methods 0.000 abstract description 3
- 238000000280 densification Methods 0.000 abstract description 3
- 230000014759 maintenance of location Effects 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract description 3
- 230000001502 supplementing effect Effects 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000012780 transparent material Substances 0.000 description 2
- 238000009954 braiding Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011153 ceramic matrix composite Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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
-
- 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
- C04B35/622—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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
-
- 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
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
-
- 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
- C04B2235/606—Drying
-
- 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
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
-
- 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
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
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 wetting agent; vacuum-pressing impregnation is carried out; concentrating under reduced pressure at constant liquid level: maintaining the vacuum degree in the dipping device, stirring and heating the device to a certain temperature to concentrate the low-viscosity slurry, and simultaneously, continuously supplementing and injecting the low-viscosity slurry from the lower part of the device, so that the liquid level of the slurry in the device is maintained constant, and the slurry in the preform and the slurry outside the preform are continuously subjected to replacement of water and matrix components, so that the matrix content in the preform is gradually increased; performing in-situ gel reaction; drying and sintering; and (5) carrying out impregnation densification for a plurality of times according to actual needs. The invention can effectively reduce the times of impregnation 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, heat and electric performance, is used as a structural material, a heat protection material, a wave-transparent material and other structural function integrated materials, and is widely applied to various fields. Continuous alumina fibers are commonly referred to as Nextel550/610/720 from 3M company in the United states, S-1920F/G from Sumitomo Japan, and other 550/610/720 type fibers (i.e., fibers having a composition and properties comparable to those of Nextel550/610/720 fibers) which are woven or co-woven into a three-dimensional preform web having a specific multi-scale structure, and then compounded with a sol or a mixture thereof to finally obtain the target composite material.
At present, the composite technology of the prefabricated fabric reinforced ceramic matrix composite material generally comprises an impregnation-in-situ gel method and an impregnation-drying method, wherein the impregnation-in-situ gel technology depends on sol to perform gel reaction under a certain condition so that the sol immersed in the prefabricated fabric generates a three-dimensional network structure and is reserved in situ; the dipping-drying process realizes the improvement of the density of the composite material by the principle of retaining matrix components by capillary force among fiber tows. The viscosity of the slurry used in the above process must be low, typically less than 50mpa.s, because the low viscosity slurry has good flowability to ensure adequate impregnation of the slurry into the preform web. However, low viscosity slurries generally have a relatively low solids content, and the composite materials are desirably dense, with conventional compounding techniques requiring impregnation cycles of not less than 10 times, and multiple sinters substantially reducing the strength of the fibers, thereby reducing the mechanical properties of the composite materials. Some sizing agents with low viscosity and high solid content, such as high-concentration silica sol, are generally poor in stability and extremely easy to cause physical and chemical changes, sol particles exist in an agglomerated state, are not easy to fully impregnate inside fiber bundle filaments, and finally affect the mechanical properties of the composite material.
Under the technical background, how to uniformly impregnate the composite material by adopting the low-viscosity slurry can also avoid the problems of too many impregnation times and poor composite material performance caused by low solid content of the slurry, and is a problem to be solved in the prior art of the preparation process of the composite material.
Disclosure of Invention
Aiming at the problems of poor performance, complicated procedures, high cost and the like of the alumina fiber reinforced ceramic matrix composite material prepared by the prior art, the invention provides a novel preparation process which can effectively reduce the times of impregnation and sintering in the compounding process and improve the strength retention rate of fibers so as to improve the mechanical property of the composite material; meanwhile, the novel process can reduce the usage amount of ceramic slurry and 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, the preparation method comprising the following steps:
(1) Weaving a fiber preform fabric: weaving or mixedly weaving continuous alumina fibers into a three-dimensional preform fabric with a certain structure;
(2) Removing the soaking agent: removing the organic impregnating compound on the fiber surface of the preform fabric;
(3) Vacuum-pressing impregnation: placing the prefabricated body fabric in an impregnating device, vacuumizing, injecting low-viscosity slurry from the lower part to enable the slurry to permeate the prefabricated body fabric, then pressurizing the device with gas to promote impregnation, and finally repeatedly vacuumizing and pressurizing the impregnation;
(4) Concentrating under reduced pressure at constant liquid level: maintaining the vacuum degree in the impregnating device, stirring and heating the impregnating device to a certain temperature to concentrate the low-viscosity slurry, and simultaneously, continuously and complementarily injecting the low-viscosity slurry from the lower part of the impregnating device, so that the liquid level of the slurry in the impregnating device is maintained constant, the slurry in the preform fabric and the external slurry are continuously subjected to water and matrix component replacement, and the content of matrix components in the preform fabric is gradually increased;
(5) In situ gel reaction: when the slurry reaches a certain viscosity, stopping vacuumizing, stirring and replenishing the slurry, and increasing the overall temperature of the impregnating device, so that the high-viscosity slurry undergoes an in-situ gel reaction, and the matrix component is remained in the preform fabric;
(6) And (3) drying: taking out the gel-containing preform fabric, then drying at constant temperature and humidity, and then thoroughly drying;
(7) Sintering: sintering the composite material obtained in the step (6) for a certain time at a certain temperature, and naturally cooling to obtain the alumina fiber reinforced ceramic matrix composite material.
Further, the above method may further include step (8) of dip densification for a plurality of times: if necessary, the alumina fiber reinforced ceramic matrix composite is subjected to impregnation-concentration-gel-drying-sintering for a plurality of times, so that the ceramic density reaches the requirement.
Preferably, the step (1) is performed as follows:
the continuous alumina fibers include Nextel550/610/720 from 3M company, sumitomo S-1920F/G, and other 550/610/720 type fibers (i.e., fibers having a composition and performance comparable to those of Nextel 550/610/720).
The structure of the preform fabric comprises a 2.5D structure, a three-dimensional structure, a needling structure and a sewing structure; the composition of the preform fiber comprises pure alumina fiber or alumina fiber/quartz fiber mixed knitting.
Preferably, in the step (2), the method for removing the wetting agent comprises sintering, acetone cleaning and water cleaning. The sintering temperature is 500-800 ℃; the temperature of the acetone cleaning is 50-56 ℃; the temperature of the water washing is 60-90 ℃.
Preferably, the vacuum degree of the step (3) vacuumized is about-0.1 MPa; the air extraction time is 3-10h, so that the inside of the fiber bundle filaments is fully exhausted;
the viscosity of the low-viscosity slurry is less than 100mpa.s and is generally controlled below 50 mpa.s;
the low-viscosity slurry is sol or a mixture of 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 gelling reaction in step (5) is 80-100 ℃.
Preferably, in the step (6), the constant temperature variable humidity drying temperature 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 moisturizing for 24 hours at 90% humidity, it is kept for 24 hours at 80% humidity, then it is kept for 24 hours at 70% humidity, and finally it is kept 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 of step (8) are densified, if not necessary, and may not be performed.
An alumina fiber reinforced ceramic matrix composite is prepared by the method.
Preferably, the alumina fiber reinforced ceramic matrix composite has a room temperature tensile strength greater than 100MPa.
The alumina fiber reinforced ceramic matrix composite can be used as a structural material and a structural function integrated material such as a thermal protection material, a wave-transparent material and the like.
The invention provides a brand new compound technology, namely a constant liquid level concentration-in-situ gel technology. After the low-viscosity slurry impregnates the preform, the slurry system is subjected to constant liquid level reduced pressure distillation, the concentration of the slurry is slowly increased, water and matrix components are continuously replaced between the inner slurry and the outer slurry of the fabric of the preform, so that the matrix content in the fabric is continuously increased, and finally, the high-concentration slurry is gelled and solidified through heating. The meaning of constant liquid level concentration is that the low-viscosity slurry continuously supplemented in the concentration process can ensure that the slurry in the concentration process always has small particle size particles with a certain proportion, thereby being beneficial to fully impregnating sol particles in fiber bundles and being beneficial to the overall stability of the slurry. The number of impregnation cycles required by the constant liquid level concentration-in-situ gel process is not more than 5, the preparation period of the composite material is greatly shortened, the reduction of sintering times improves the strength retention rate of fibers, and the performance of the composite material is improved by 30%. Meanwhile, the usage amount of the ceramic slurry is reduced to 25-35% of the original usage 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 gel process used in the invention can obviously shorten the preparation period of the composite material, and the composite 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 in the invention can reduce the use amount of the slurry to 25-35% of the original use amount, and greatly reduce the preparation cost of the composite material.
(3) The constant liquid level concentration-in-situ gel process used in the invention is applicable to various ceramic matrix forms, and comprises sol or a mixture of sol and ceramic powder.
(4) The constant liquid level concentration-in-situ gel process used in the invention has small damage to fiber, and the mechanical strength of the prepared composite material can be improved by more than 30%.
Drawings
FIG. 1 is a flow chart of the present invention for preparing an alumina fiber reinforced ceramic matrix composite.
Fig. 2 is a schematic diagram of tooling equipment 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 in connection with the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a preparation method of an alumina fiber reinforced ceramic matrix composite, as shown in figure 1, comprising the following steps:
(1) Woven fiber three-dimensional preform fabric: weaving the Nextel550/610/720 or S-1920F/G or other 550/610/720 continuous alumina fibers into an alumina fiber or alumina/quartz fiber mixed-woven prefabricated body fabric with a 2.5D structure or a three-dimensional structure or a needle structure or a sewing structure;
(2) Removing the soaking agent: sintering the organic impregnating compound on the surface of the prefabricated body fabric at 500-800 ℃, or washing with acetone at 50-60 ℃ or washing with water at 60-90 ℃;
(3) Vacuum-pressing impregnation: placing the prefabricated body fabric in a vacuum impregnation device, vacuumizing the device, wherein the vacuum degree is about-0.1 MPa, and the vacuumizing time is 3-10h. The sol or the mixture of sol and ceramic powder is injected from below into the preform web. The device is pressurized with gas to facilitate impregnation. Finally, repeatedly vacuumizing and pressurizing;
(4) Concentrating under reduced pressure at constant liquid level: maintaining the vacuum degree in the dipping device, stirring and heating the device to 40-60 ℃ to concentrate the low-viscosity slurry, and simultaneously, continuously supplementing and injecting the low-viscosity slurry from the lower part of the device, so that the liquid level of the slurry in the device is maintained constant, and the slurry in the preform and the slurry outside the preform are continuously subjected to replacement of water and matrix components, so that the matrix content in the preform is gradually increased;
(5) Gel reaction: when the slurry reaches a certain viscosity, stopping vacuumizing, stirring and replenishing the slurry, and increasing the temperature of the impregnating device to 80-100 ℃ to enable the high-viscosity slurry to undergo a gel reaction, wherein matrix components are remained in the preform;
(6) And (3) drying: taking out the gel-containing preform, drying at 40-50deg.C with constant temperature and humidity decreasing from 90% to 60%, and conventional drying at 80-200deg.C for 5-12 hr;
(7) Sintering: sintering the composite material at 600-1200 ℃ for 0.5-3h, and naturally cooling;
(8) Immersing again for densification: and (3) carrying out multiple times of dipping, concentrating, gelling, drying and sintering on the alumina fiber reinforced ceramic matrix composite material to obtain the composite material with normal-temperature tensile strength of more than 100MPa.
Fig. 2 is a schematic view of a tooling device, i.e. an impregnating apparatus, used in the present invention. The working principle of the device is as follows:
1. the vacuum pump is started and vacuumized, so that the internal pressure of the tank body is minus 0.1MPa. The purpose is to exhaust the gas inside the fabric, facilitating the immersion of the low viscosity sol.
2. And starting a liquid inlet pump, and injecting the low-viscosity sol into the tank body from the liquid inlet. When the liquid level reaches the control floating ball, the liquid inlet pump automatically stops working.
3. The gas cylinder is opened, so that high-pressure air is pumped into the tank body from the upper part of the tank body, and the gas cylinder is closed after pressure maintaining is carried out for a certain time. The aim is to expel air bubbles inside the fabric as much as possible.
4. And (3) discharging pressure, starting a vacuum pump and a stirrer, and heating steam to heat the outer wall of the tank body. The reduced pressure concentration was started and the volatilized vapor was discharged from the vacuum pump outlet. The purpose is that the low-viscosity sol in the tank body is concentrated, the solid content of the sol is improved, and at the moment, the low-viscosity sol in the fabric is replaced with the high-viscosity sol in the tank body under the driving force of Brownian motion, so that the solid content of the sol in the fabric is consistent, and the solid content of the sol in the fabric is improved. Therefore, after the gel, more sol particles are reserved in the fabric, and the composite material has the advantages of high density, short preparation period and high performance.
5. Along with the reduction of the liquid level of the sol, the liquid level control floating ball can control the switch, so that the liquid inlet pump is started, and low-viscosity slurry is supplemented into the tank body, thereby realizing constant liquid level concentration. The purpose is that: the meaning of constant liquid level concentration is that the low-viscosity slurry continuously supplemented in the concentration process can ensure that the slurry in the concentration process always has small particle size particles with a certain proportion, thereby being beneficial to fully impregnating sol particles in fiber bundles and being beneficial to the overall stability of the slurry.
6. When the sol in the tank reaches a certain viscosity, all the equipment is stopped.
Example 1
Firstly, weaving S-1920 continuous alumina fibers into a 2.5D structure prefabricated body fabric; then, the organic impregnating compound on the surface of the preform fiber is removed by sintering at 600 ℃; subsequently, the preform web was placed in a vacuum impregnation apparatus, evacuated to a vacuum degree of-0.1 MPa and an evacuation time of 3 hours. Subsequently, a low-viscosity alumina/silica mixed sol is injected from the lower part, and the preform fabric is penetrated through and repeatedly pumped and pressed; then, maintaining the vacuum degree in the impregnating device, stirring and heating the device to 40 ℃ to continuously concentrate the sol, and simultaneously continuously injecting the low-viscosity sol from the lower part of the device, so as to maintain the constant liquid level, and continuously replacing water and matrix components in and out of the fabric to gradually increase the matrix content in the fabric; after the sol in the device reaches a certain viscosity, stopping vacuumizing, stirring and replenishing slurry, and heating the whole impregnating device to 80 ℃ to enable the high-concentration sol to undergo a gel reaction, so that matrix components are reserved in the preform fabric; taking out the gel-containing preform, drying at 45 ℃ with constant temperature and humidity reduced from 90% to 60%, and then gradually heating and drying at 80-200 ℃ for 12h; finally, sintering the composite material at 900 ℃ for 1h, and naturally cooling; finally, the alumina fiber reinforced ceramic matrix composite is subjected to impregnation, gel drying and sintering for a plurality of times, and the normal-temperature tensile strength of the composite is more than 110MPa.
Example 2
First, braiding a Nextel 610 continuous alumina fiber into a three-way orthogonal structure preform fabric; then, the organic impregnating compound on the surface of the preform fiber is removed by sintering at 600 ℃; subsequently, the preform web was placed in a vacuum impregnation apparatus, evacuated to a vacuum degree of-0.1 MPa and evacuated for 10 hours. Subsequently, a low-viscosity alumina sol is injected from the lower part, and the preform fabric is penetrated through and repeatedly pumped and pressed; then, maintaining the vacuum degree in the impregnating device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and simultaneously continuously injecting the low-viscosity sol from the lower part of the device, so as to maintain the constant liquid level, and continuously replacing water and matrix components in and out of the fabric to gradually increase the matrix content in the fabric; after the sol in the device reaches a certain viscosity, stopping vacuumizing, stirring and replenishing slurry, and heating the whole impregnating device to 90 ℃ to enable the high-concentration sol to undergo a gel reaction, so that matrix components are reserved in the preform fabric; taking out the gel-containing preform, drying at 40 ℃ with constant temperature and humidity reduced from 90% to 60%, and then gradually heating and drying at 80-200 ℃ for 12h; finally, sintering the composite material at 1000 ℃ for 1h, and naturally cooling; finally, the alumina fiber reinforced ceramic matrix composite is subjected to impregnation, gel drying and sintering for a plurality of times, and the normal-temperature tensile strength of the composite is more than 240MPa.
Example 3
Firstly, weaving domestic 720-type continuous alumina fibers into a three-way orthogonal structure prefabricated body fabric; then, the organic impregnating compound on the surface of the preform fiber is removed by sintering at 600 ℃; subsequently, the preform web was placed in a vacuum impregnation apparatus, evacuated to a vacuum degree of-0.1 MPa and an evacuation time of 3 hours. Subsequently, a low-viscosity alumina sol is injected from the lower part, and the preform fabric is penetrated through and repeatedly pumped and pressed; then, maintaining the vacuum degree in the impregnating device, stirring and heating the device to 60 ℃ to continuously concentrate the sol, and simultaneously continuously injecting the low-viscosity sol from the lower part of the device, so as to maintain the constant liquid level, and continuously replacing water and matrix components in and out of the fabric to gradually increase the matrix content in the fabric; after the sol in the device reaches a certain viscosity, stopping vacuumizing, stirring and replenishing slurry, and heating the whole impregnating device to 100 ℃ to enable the high-concentration sol to undergo a gel reaction, so that matrix components are reserved in the preform fabric; taking out the gel-containing preform, drying at 45 ℃ with constant temperature and humidity reduced from 90% to 60%, and then gradually heating and drying at 80-200 ℃ for 5h; finally, sintering the composite material at 1200 ℃ for 1h, and naturally cooling; finally, the alumina fiber reinforced ceramic matrix composite is subjected to impregnation, gel drying and sintering for a plurality of times, and the normal-temperature tensile strength of the composite is more than 150MPa.
Example 4
Firstly, mixing domestic 550 type continuous alumina fiber and quartz fiber to form a 2.5D structure preform fabric; then, cleaning and removing the organic impregnating compound on the surface of the preform fiber by acetone at 50 ℃; subsequently, the preform web was placed in a vacuum impregnation apparatus, evacuated to a vacuum degree of-0.1 MPa and an evacuation time of 3 hours. Subsequently, a low-viscosity alumina/silica mixed sol is injected from the lower part, and the preform fabric is penetrated through and repeatedly pumped and pressed; then, maintaining the vacuum degree in the impregnating device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and simultaneously continuously injecting the low-viscosity sol from the lower part of the device, so as to maintain the constant liquid level, and continuously replacing water and matrix components in and out of the fabric to gradually increase the matrix content in the fabric; after the sol in the device reaches a certain viscosity, stopping vacuumizing, stirring and replenishing slurry, and heating the whole impregnating device to 80 ℃ to enable the high-concentration sol to undergo a gel reaction, so that matrix components are reserved in the preform fabric; taking out the gel-containing preform, drying at 45 ℃ with constant temperature and humidity reduced from 90% to 60%, and then gradually heating and drying at 80-200 ℃ for 7h; finally, sintering the composite material at 600 ℃ for 1h, and naturally cooling; finally, the alumina fiber reinforced ceramic matrix composite is subjected to impregnation, gel drying and sintering for a plurality of times, and the normal-temperature tensile strength of the composite is more than 100MPa.
Example 5
Firstly, weaving domestic 720-type continuous alumina fibers into a three-way orthogonal structure prefabricated body fabric; then, the organic impregnating compound on the surface of the prefabricated body fabric is removed by washing with water at 60 ℃; subsequently, the preform web was placed in a vacuum impregnation apparatus, evacuated to a vacuum degree of-0.1 MPa and an evacuation time of 3 hours. Subsequently, a low-viscosity alumina sol is injected from the lower part, and the preform fabric is penetrated through and repeatedly pumped and pressed; then, maintaining the vacuum degree in the impregnating device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and simultaneously continuously injecting the low-viscosity sol from the lower part of the device, so as to maintain the constant liquid level, and continuously replacing water and matrix components in and out of the fabric to gradually increase the matrix content in the fabric; after the sol in the device reaches a certain viscosity, stopping vacuumizing, stirring and replenishing slurry, and heating the whole impregnating device to 90 ℃ to enable the high-concentration sol to undergo a gel reaction, so that matrix components are reserved in the preform fabric; taking out the gel-containing preform, drying at 45 ℃ with constant temperature and humidity reduced from 90% to 60%, and then gradually heating and drying at 80-200 ℃ for 12h; finally, sintering the composite material at 1200 ℃ for 1h, and naturally cooling; finally, the alumina fiber reinforced ceramic matrix composite is subjected to impregnation, gel drying and sintering for a plurality of times, and the normal-temperature tensile strength of the composite is more than 150MPa.
Example 6
Firstly, weaving Nextel 720 continuous alumina fibers into a three-way orthogonal structure prefabricated body fabric; then, the organic impregnating compound on the surface of the prefabricated body fabric is removed by washing at 60 ℃; subsequently, the preform web was placed in a vacuum impregnation apparatus, evacuated to a vacuum degree of-0.1 MPa and an evacuation time of 3 hours. Then, the mullite sol with low viscosity is injected from the lower part, and the mullite sol is poured over the prefabricated body fabric and is repeatedly pumped and pressed; then, maintaining the vacuum degree in the impregnating device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and simultaneously continuously injecting the low-viscosity sol from the lower part of the device, so as to maintain the constant liquid level, and continuously replacing water and matrix components in and out of the fabric to gradually increase the matrix content in the fabric; after the sol in the device reaches a certain viscosity, stopping vacuumizing, stirring and replenishing slurry, and heating the whole impregnating device to 90 ℃ to enable the high-concentration sol to undergo a gel reaction, so that matrix components are reserved in the preform fabric; taking out the gel-containing preform, drying at 50 ℃ with constant temperature and humidity reduced from 90% to 60%, and then gradually heating and drying at 80-200 ℃ for 12h; finally, sintering the composite material at 1200 ℃ for 1h, and naturally cooling; finally, the alumina fiber reinforced ceramic matrix composite is subjected to impregnation, gel drying and sintering for a plurality of times, and the normal-temperature tensile strength of the composite is more than 180MPa.
Example 7
Firstly, weaving Nextel 720 continuous alumina fibers into a three-way orthogonal structure prefabricated body fabric; then, the organic impregnating compound on the surface of the prefabricated body fabric is removed by washing at 60 ℃; subsequently, the preform web was placed in a vacuum impregnation apparatus, evacuated to a vacuum degree of-0.1 MPa and an evacuation time of 3 hours. Subsequently, a mixture of a low-viscosity alumina sol and a mullite sol is injected from the lower part, and the mixture is repeatedly pumped and pressed through the prefabricated fabric; then, maintaining the vacuum degree in the impregnating device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and simultaneously continuously injecting the low-viscosity sol from the lower part of the device, so as to maintain the constant liquid level, and continuously replacing water and matrix components in and out of the fabric to gradually increase the matrix content in the fabric; after the sol in the device reaches a certain viscosity, stopping vacuumizing, stirring and replenishing slurry, and heating the whole impregnating device to 90 ℃ to enable the high-concentration sol to undergo a gel reaction, so that matrix components are reserved in the preform fabric; taking out the gel-containing preform, drying at 45 ℃ with constant temperature and humidity reduced from 90% to 60%, and then gradually heating and drying at 80-200 ℃ for 8 hours; finally, sintering the composite material at 1200 ℃ for 1h, and naturally cooling; finally, the alumina fiber reinforced ceramic matrix composite is subjected to impregnation, gel drying and sintering for a plurality of times, and the normal-temperature tensile strength of the composite is more than 160MPa.
Example 8
Firstly, weaving Nextel 720 continuous alumina fibers into a three-way orthogonal structure prefabricated body fabric; then, the organic impregnating compound on the surface of the prefabricated body fabric is cleaned and removed by acetone at 50 ℃; subsequently, the preform web was placed in a vacuum impregnation apparatus, evacuated to a vacuum degree of-0.1 MPa and an evacuation time of 3 hours. Subsequently, the mixture of mullite sol/alumina powder with low viscosity is injected from the lower part, and the mixture is repeatedly pumped and pressed through the prefabricated body fabric; then, maintaining the vacuum degree in the impregnating device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and simultaneously continuously injecting the low-viscosity sol from the lower part of the device, so as to maintain the constant liquid level, and continuously replacing water and matrix components in and out of the fabric to gradually increase the matrix content in the fabric; after the sol in the device reaches a certain viscosity, stopping vacuumizing, stirring and replenishing slurry, and heating the whole impregnating device to 80 ℃ to enable the high-concentration sol to undergo a gel reaction, so that matrix components are reserved in the preform fabric; taking out the gel-containing preform, drying at 45 ℃ with constant temperature and humidity reduced from 90% to 60%, and then gradually heating and drying at 80-200 ℃ for 12h; finally, sintering the composite material at 1200 ℃ for 1h, and naturally cooling; finally, the alumina fiber reinforced ceramic matrix composite is subjected to impregnation, gel drying and sintering for a plurality of times, and the normal-temperature tensile strength of the composite is more than 150MPa.
Example 9
First, a Nextel 720 continuous alumina fiber from 3M company of America was woven into a three-way orthogonal structure preform fabric; then, the organic impregnating compound on the surface of the prefabricated body fabric is cleaned and removed by acetone at 50 ℃; subsequently, the preform web was placed in a vacuum impregnation apparatus, evacuated to a vacuum degree of-0.1 MPa and an evacuation time of 3 hours. Subsequently, the mixture of mullite sol/alumina powder with low viscosity is injected from the lower part, and the mixture is repeatedly pumped and pressed through the prefabricated body fabric; then, maintaining the vacuum degree in the impregnating device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and simultaneously continuously injecting the low-viscosity sol from the lower part of the device, so as to maintain the constant liquid level, and continuously replacing water and matrix components in and out of the fabric to gradually increase the matrix content in the fabric; after the sol in the device reaches a certain viscosity, stopping vacuumizing, stirring and replenishing slurry, and heating the whole impregnating device to 80 ℃ to enable the high-concentration sol to undergo a gel reaction, so that matrix components are reserved in the preform fabric; taking out the gel-containing preform, drying at 45 ℃ with constant temperature and humidity reduced from 90% to 60%, and then gradually heating and drying at 80-200 ℃ for 12h; finally, sintering the composite material at 1050 ℃ for 1h, and naturally cooling; finally, the alumina fiber reinforced ceramic matrix composite is subjected to impregnation, gel drying and sintering for a plurality of times, and the normal-temperature tensile strength of the composite is more than 140MPa.
Example 10
Firstly, mixing domestic 550 type continuous alumina fiber and quartz fiber to form a 2.5D structure preform fabric; then, cleaning and removing the organic impregnating compound on the surface of the preform fiber by acetone at 50 ℃; subsequently, the preform web was placed in a vacuum impregnation apparatus, evacuated to a vacuum degree of-0.1 MPa and an evacuation time of 3 hours. Subsequently, low-viscosity silica sol is injected from the lower part, and the preform fabric is soaked and repeatedly pumped and pressed; then, maintaining the vacuum degree in the impregnating device, stirring and heating the device to 50 ℃ to continuously concentrate the sol, and simultaneously continuously injecting the low-viscosity sol from the lower part of the device, so as to maintain the constant liquid level, and continuously replacing water and matrix components in and out of the fabric to gradually increase the matrix content in the fabric; after the sol in the device reaches a certain viscosity, stopping vacuumizing, stirring and replenishing slurry, and heating the whole impregnating device to 80 ℃ to enable the high-concentration sol to undergo a gel reaction, so that matrix components are reserved in the preform fabric; taking out the gel-containing preform, drying at 45 ℃ with constant temperature and humidity reduced from 90% to 60%, and then gradually heating and drying at 80-200 ℃ for 12h; finally, sintering the composite material at 800 ℃ for 1h, and naturally cooling; finally, the alumina fiber reinforced ceramic matrix composite is subjected to impregnation, gel drying and sintering for a plurality of times, and the normal-temperature tensile strength of the composite is more than 110MPa.
Comparative example 1 (conventional dip-in situ gel method, mainly compared with example 10)
Firstly, mixing domestic 550 type continuous alumina fiber and quartz fiber to form a 2.5D structure preform fabric; then, cleaning and removing the organic impregnating compound on the surface of the preform fiber by acetone at 50 ℃; subsequently, the preform web was placed in a vacuum impregnation apparatus, evacuated to a vacuum degree of-0.1 MPa and an evacuation time of 3 hours. Subsequently, low-viscosity silica sol is injected from the lower part, and the preform fabric is soaked and repeatedly pumped and pressed; heating the whole soaking device to 90 ℃ to enable the sol to undergo a gel reaction, so that matrix components are reserved in the preform fabric; taking out the gel-containing preform, drying at 45 ℃ with constant temperature and humidity reduced from 90% to 60%, and then gradually heating and drying at 80-200 ℃ for 12h; finally, sintering the composite material at 800 ℃ for 1h, and naturally cooling; the alumina fiber reinforced ceramic matrix composite is subjected to impregnation, gel-drying and sintering for a plurality of times, and the normal-temperature tensile strength of the composite is about 90MPa. It is worth noting that in this scheme, the time period is more than 40 days, and the preparation cost of the single flat rice composite material is more than 10 ten thousand yuan.
Comparative example 2 (conventional impregnation-drying method, mainly compared with example 10)
Firstly, mixing domestic 550 type continuous alumina fiber and quartz fiber to form a 2.5D structure preform fabric; then, cleaning and removing the organic impregnating compound on the surface of the preform fiber by acetone at 50 ℃; subsequently, the preform web was placed in a vacuum impregnation apparatus, evacuated to a vacuum degree of-0.1 MPa and an evacuation time of 3 hours. Subsequently, low-viscosity silica sol is injected from the lower part, and the preform fabric is soaked and repeatedly pumped and pressed; secondly, taking out the wet fabric, and then drying the wet fabric in an oven at the temperature of 50-200 ℃ in a gradual heating way for 15 hours; thirdly, sintering the composite material at 600 ℃ for 1h, and naturally cooling; the alumina fiber reinforced ceramic matrix composite is subjected to impregnation, drying and sintering for a plurality of times, and the normal-temperature tensile strength of the composite is about 90MPa. It is worth noting that in this solution, the time period is more than 35 days, and the preparation cost of the single flat rice composite material is more than 10 ten thousand yuan.
The total time required for the composite impregnation, the cost of the slurry required for the preparation of the single flat panel, and the tensile strength of the ceramic material obtained were recorded for each of the above examples and comparative examples, and the results are shown in table 1.
TABLE 1
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the 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 scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. The preparation method of the continuous alumina fiber reinforced ceramic matrix composite based on the constant liquid level concentration-in-situ gel process is characterized by comprising the following steps of:
(1) Weaving or mixedly weaving continuous alumina fibers into a three-dimensional preform fabric with a certain structure;
(2) Removing the organic impregnating compound on the fiber surface of the preform fabric;
(3) Placing the prefabricated body fabric in an impregnating device, vacuumizing, injecting low-viscosity slurry from the lower part to enable the slurry to permeate the prefabricated body fabric, then pressurizing the device with gas to promote impregnation, and finally repeatedly vacuumizing and pressurizing impregnation;
(4) Maintaining the vacuum degree in the dipping device, stirring and heating the dipping device to a certain temperature to concentrate the low-viscosity slurry, improving the solid content of the slurry, and simultaneously, continuously and complementarily injecting the low-viscosity slurry from the lower part of the dipping device, so that the liquid level of the slurry in the dipping device is kept constant, the low-viscosity slurry in the fabric of the preform and the external high-viscosity slurry are continuously subjected to water and matrix component replacement under the driving force of Brownian motion, the solid content of the slurry in the fabric is consistent, the content of the matrix component in the fabric of the preform is gradually improved, and the constant liquid level reduced pressure concentration is realized;
(5) When the slurry reaches a certain viscosity, stopping vacuumizing, stirring and replenishing the slurry, and increasing the overall temperature of the impregnating device, so that the high-viscosity slurry undergoes an in-situ gel reaction, and the matrix component is remained in the preform fabric;
(6) Taking out the gel-containing preform fabric, then drying at constant temperature and humidity, and then thoroughly drying;
(7) Sintering the composite material obtained in the step (6) for a certain time at a certain temperature, and naturally cooling to obtain the alumina fiber reinforced ceramic matrix composite material.
2. The method according to claim 1, wherein the alumina fiber reinforced ceramic matrix composite is impregnated and densified a plurality of times according to actual needs, i.e., the alumina fiber reinforced ceramic matrix composite is impregnated, concentrated, gel, dried and sintered in steps (3) to (7) a plurality of times, so that the ceramic density meets the requirements.
3. The method of claim 1, wherein the continuous alumina fibers of step (1) comprise Nextel550/610/720, S-1920F/G, and other 550/610/720 type fibers; the structure of the preform fabric comprises a 2.5D structure, a three-dimensional structure, a needling structure and a sewing structure; the composition of the preform fiber comprises pure alumina fiber or alumina fiber/quartz fiber mixed knitting.
4. The method according to claim 1, wherein in the step (2), the method for removing the wetting agent comprises sintering, acetone cleaning, water cleaning; the sintering temperature is 500-800 ℃; the temperature of the acetone cleaning is 50-56 ℃; the temperature of the water washing is 60-90 ℃.
5. The method according to claim 1, wherein the vacuum degree of the vacuum pumped in the step (3) is-0.1 MPa; the air extraction time is 3-10h, so that the inside of the fiber bundle filaments 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 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 heating temperature 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 constant temperature variable humidity drying in the step (6) is performed at a temperature of 40 to 50 ℃ and a saturated steam humidity of 60 to 90%; the application process of the variable humidity comprises the following steps: firstly, keeping moisture for 24 hours under 90% humidity, then keeping the moisture for 24 hours under 80% humidity, then keeping the moisture for 24 hours under 70% humidity, and finally keeping the moisture for 24 hours under 60% humidity; and then carrying out conventional drying, wherein the temperature of the conventional drying is 80-200 ℃ and the drying time is 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 of claim 8, wherein the composite has a room temperature tensile strength of greater than 100MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210963117.4A CN115448741B (en) | 2022-08-11 | 2022-08-11 | Method for preparing alumina fiber reinforced ceramic matrix composite based on constant liquid level concentration-in-situ gel process and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210963117.4A CN115448741B (en) | 2022-08-11 | 2022-08-11 | Method for preparing alumina fiber reinforced ceramic matrix composite based on constant liquid level concentration-in-situ gel process and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115448741A CN115448741A (en) | 2022-12-09 |
| CN115448741B true CN115448741B (en) | 2023-07-18 |
Family
ID=84298021
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210963117.4A Active CN115448741B (en) | 2022-08-11 | 2022-08-11 | Method for preparing alumina fiber reinforced ceramic matrix composite based on constant liquid level concentration-in-situ gel process and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115448741B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115974536B (en) * | 2023-01-17 | 2024-02-13 | 航天特种材料及工艺技术研究所 | Alumina fiber reinforced ceramic matrix composite containing lanthanum phosphate interface layer and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010215504A (en) * | 2010-05-18 | 2010-09-30 | Society Of Japanese Aerospace Co Inc | Method for manufacturing continuous fiber strengthening type composite material |
| CN102390837A (en) * | 2011-08-03 | 2012-03-28 | 南通海迅天恒纳米科技有限公司 | Preparation method of nonspherical nanometer-scale silica sol |
| CN111732107A (en) * | 2020-07-10 | 2020-10-02 | 阳江市惠尔特新材料科技有限公司 | Method for preparing high-concentration silica sol with ultra-large particle size by using water glass |
| CN112479691A (en) * | 2020-12-02 | 2021-03-12 | 中南大学 | Preparation method of high-temperature-resistant reinforced toughened Ox/Ox composite material |
| WO2022007377A1 (en) * | 2020-07-09 | 2022-01-13 | 南京航空航天大学 | Composite material enhanced by mixed woven fiber preform and preparation method therefor |
| CN114105664A (en) * | 2021-12-20 | 2022-03-01 | 航天特种材料及工艺技术研究所 | Method for preparing ceramic fiber reinforced quartz ceramic matrix composite material by low-temperature sintering and application |
Family Cites Families (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3731650A1 (en) * | 1987-09-19 | 1989-03-30 | Schott Glaswerke | METHOD FOR PRODUCING FIBER REINFORCED COMPOSITES |
| JP2673229B2 (en) * | 1988-12-14 | 1997-11-05 | 株式会社日阪製作所 | Circulation tank of batch type concentrator |
| JP4521981B2 (en) * | 2000-11-09 | 2010-08-11 | キヤノン株式会社 | Manufacturing method of fiber assembly |
| CN1252153C (en) * | 2001-12-31 | 2006-04-19 | 上海杰事杰新材料股份有限公司 | Manufacturing method of continuous fiber reinforced thermoplastic plastic |
| CN104446334B (en) * | 2014-12-15 | 2017-08-04 | 航天特种材料及工艺技术研究所 | A kind of preparation method of inexpensive charcoal-aero gel heat-insulation composite material |
| CN105198471B (en) * | 2015-11-02 | 2017-07-18 | 湖北三江航天江北机械工程有限公司 | The preparation method of the stealthy wave-penetrating composite material of graphene modified ceramic base |
| CN109455924B (en) * | 2018-12-05 | 2021-11-30 | 航天特种材料及工艺技术研究所 | Fiber-reinforced ceramic-based wave-transmitting material with frequency selective structure and preparation method thereof |
| FR3102701B1 (en) * | 2019-11-06 | 2022-12-23 | Arkema France | Process for impregnating a fibrous material with an optimized system for replenishing and cleaning fine particles |
| CN111005226B (en) * | 2019-12-04 | 2022-07-05 | 航天特种材料及工艺技术研究所 | Method for modifying interface of three-dimensional fabric of alumina fiber and modified three-dimensional fabric of alumina fiber prepared by method |
| CN113511879B (en) * | 2021-09-09 | 2021-11-30 | 长沙科航特种织造有限公司 | Quartz fiber reinforced quartz-based composite material and manufacturing method thereof |
| CN113956058A (en) * | 2021-11-29 | 2022-01-21 | 航天特种材料及工艺技术研究所 | Preparation method of high-performance alumina fiber ceramic matrix composite |
| CN114751718B (en) * | 2022-04-01 | 2023-04-18 | 巩义市泛锐熠辉复合材料有限公司 | Method for preparing hydrophobic silica aerogel felt under normal pressure |
-
2022
- 2022-08-11 CN CN202210963117.4A patent/CN115448741B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010215504A (en) * | 2010-05-18 | 2010-09-30 | Society Of Japanese Aerospace Co Inc | Method for manufacturing continuous fiber strengthening type composite material |
| CN102390837A (en) * | 2011-08-03 | 2012-03-28 | 南通海迅天恒纳米科技有限公司 | Preparation method of nonspherical nanometer-scale silica sol |
| WO2022007377A1 (en) * | 2020-07-09 | 2022-01-13 | 南京航空航天大学 | Composite material enhanced by mixed woven fiber preform and preparation method therefor |
| CN111732107A (en) * | 2020-07-10 | 2020-10-02 | 阳江市惠尔特新材料科技有限公司 | Method for preparing high-concentration silica sol with ultra-large particle size by using water glass |
| CN112479691A (en) * | 2020-12-02 | 2021-03-12 | 中南大学 | Preparation method of high-temperature-resistant reinforced toughened Ox/Ox composite material |
| CN114105664A (en) * | 2021-12-20 | 2022-03-01 | 航天特种材料及工艺技术研究所 | Method for preparing ceramic fiber reinforced quartz ceramic matrix composite material by low-temperature sintering and application |
Non-Patent Citations (1)
| Title |
|---|
| 先驱体浸渍-裂解法制备SiBN纤维增强SiBN陶瓷基复合材料;余娟丽;李森;吕毅;张天翔;赵英民;;复合材料学报(02);190-196 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115448741A (en) | 2022-12-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110526728B (en) | Fiber-reinforced mullite ceramic matrix composite material and preparation method thereof | |
| CN109384459B (en) | Fiber-reinforced silicon dioxide heat-insulating ceramic material and preparation method and application thereof | |
| CN115448741B (en) | Method for preparing alumina fiber reinforced ceramic matrix composite based on constant liquid level concentration-in-situ gel process and application thereof | |
| CN110078515A (en) | A kind of preparation method of graphene oxide modified carbon fiber enhancing carbon/silicon carbide ceramic matrix composite | |
| CN114409420B (en) | Alumina fiber reinforced mullite ceramic matrix composite and preparation method thereof | |
| CN108484194B (en) | Al (aluminum)2O3-SiO2Base composite material and rapid preparation method thereof | |
| CN110804274B (en) | Light heat-proof and heat-insulation composite material based on fabric reinforcement with spacing structure and preparation method thereof | |
| CN113511879B (en) | Quartz fiber reinforced quartz-based composite material and manufacturing method thereof | |
| CN109206146A (en) | Carbon fiber/nanofiber cooperates with tough ceramic matric composite and preparation method thereof | |
| CN114105664B (en) | Method for preparing ceramic fiber reinforced quartz ceramic matrix composite material by low-temperature sintering and application | |
| CN115636681B (en) | Nitride fiber reinforced silicon nitride composite material and preparation method and application thereof | |
| CN108484173A (en) | SiCf/ SiC ceramic matrix composite material and preparation method thereof | |
| CN115385709B (en) | Method for quickly compacting carbon-carbon composite material | |
| CN113800922A (en) | Silica sol dipping composite forming method for quartz fiber braided body | |
| CN114164709A (en) | Carbon fiber paper with carbon black reinforced conductive network and preparation method thereof | |
| CN115417683A (en) | Preparation method of oxide continuous filament reinforced oxide ceramic matrix composite | |
| CN116813365A (en) | High-temperature-resistant large-size carbon-carbon bearing plate and preparation method thereof | |
| CN113896554B (en) | High-density fiber reinforced quartz ceramic composite material and preparation method thereof | |
| CN105859303B (en) | A kind of carbon/carbon compound material precast body and preparation method thereof | |
| CN115849928B (en) | Injection-molded aluminum oxide fiber reinforced composite material containing lanthanum phosphate interface layer and preparation method thereof | |
| CN109337380A (en) | A kind of fiber reinforced flexible aerogel composite and preparation method thereof | |
| CN112500181B (en) | Silica short fiber mould pressing ceramic antenna window composite material and preparation method thereof | |
| CN113698220A (en) | Preparation method of fiber-reinforced silicon carbide composite material and fiber-reinforced silicon carbide composite material | |
| CN114804893B (en) | Electronic product shell based on continuous ceramic fibers and preparation method thereof | |
| CN115974536B (en) | Alumina fiber reinforced ceramic matrix composite containing lanthanum phosphate interface layer and preparation method thereof |
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 |