CN116375461A - Continuous silicon carbide fiber reinforced mullite-based composite material and preparation method thereof - Google Patents
Continuous silicon carbide fiber reinforced mullite-based composite material and preparation method thereof Download PDFInfo
- Publication number
- CN116375461A CN116375461A CN202310426528.4A CN202310426528A CN116375461A CN 116375461 A CN116375461 A CN 116375461A CN 202310426528 A CN202310426528 A CN 202310426528A CN 116375461 A CN116375461 A CN 116375461A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- composite material
- mullite
- carbide fiber
- fiber reinforced
- 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.)
- Pending
Links
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 71
- 239000000835 fiber Substances 0.000 title claims abstract description 59
- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 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 title claims abstract description 47
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000011159 matrix material Substances 0.000 claims abstract description 20
- 239000004744 fabric Substances 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 17
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 238000009941 weaving Methods 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 150000007513 acids Chemical class 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 claims description 2
- 239000011203 carbon fibre reinforced carbon Substances 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 230000003014 reinforcing effect Effects 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000011153 ceramic matrix composite Substances 0.000 description 3
- 239000003365 glass fiber Substances 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 3
- 229920003257 polycarbosilane Polymers 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000011226 reinforced ceramic Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000010942 ceramic carbide Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000012783 reinforcing fiber Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/624—Sol-gel processing
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
- C04B2235/5244—Silicon carbide
-
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5252—Fibers having a specific pre-form
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/616—Liquid infiltration of green bodies or pre-forms
-
- 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
- C04B2235/6562—Heating rate
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)
- Inorganic Fibers (AREA)
Abstract
The invention relates to the technical field of composite materials, in particular to a continuous silicon carbide fiber reinforced mullite-based composite material and a preparation method thereof; the reinforcing phase of the composite material is continuous silicon carbide fiber fabric, the main phase of the matrix is mullite, and the matrix contains one or more of alumina and silica; the silicon carbide fiber fabric is a 2.5-dimensional woven piece, and the mass content of mullite in the matrix is more than 50%; the volume fraction of the fibers in the composite material is not less than 30%; the continuous silicon carbide fiber reinforced mullite-based composite material has excellent high temperature resistance and mechanical property, and the matrix raw material has low price and wide sources. The matrix components of the composite material are regulated and controlled by adjusting the preparation mode of the mullite precursor solution, so that the mechanical properties of the continuous silicon carbide fiber reinforced mullite-based composite material are controlled, the process flow is simple, the preparation method can be used for forming large-scale complex components, and industrial production and application are easy.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a continuous silicon carbide fiber reinforced mullite-based composite material and a preparation method thereof.
Background
The rapid development of modern electronic countermeasure technology makes various weapons of future wars, such as missiles, airplanes, tanks, ships and the like, face a great threat, and development and application of stealth technology have become important directions of military technical research of various countries in order to improve the survivability of military targets in national defense systems and the outburst prevention and deep striking capability of combat weapon systems. At present, silicon carbide fiber reinforced ceramic matrix composite materials are widely applied to the fields of high-temperature structural materials, high-temperature wave absorbing materials and nuclear reactors.
Silicon carbide (SiC) fiber is a ceramic fiber in which equal amounts of carbon and silicon are periodically arranged in a diamond structure, and the actual silicon carbide fiber may contain carbon and oxygen elements, etc. The silicon carbide fiber has the advantages of small diameter, high strength, high modulus, good temperature resistance, small density, stable chemical property and the like. The high-performance continuous silicon carbide fiber can meet the severe requirements of the high-performance ceramic matrix composite material: fine diameter, oxidation resistance, high temperature resistance, creep resistance and corrosion resistance; can be stably used in the air with the temperature of not lower than 1300 ℃ and in the inert atmosphere with the temperature of not lower than 1600 ℃; the strength of the fiber can reach 1960-4410 MPa, and the modulus can reach 176-400 GPa.
The continuous silicon carbide fiber reinforced ceramic matrix composite is formed by compounding high-strength silicon carbide fibers and a ceramic matrix. The reinforced fiber is equivalent to the framework of the ceramic matrix composite material and is the main component of the composite materialThe macroscopic strength of the composite material to carry the structural units is largely dependent on the strength of the reinforcing fibers. At present, the silicon carbide ceramic matrix composite material is usually made of reinforced fibers such as carbon fibers, silicon carbide fibers, glass fibers and the like. At present, silicon carbide fiber reinforced silicon carbide based composite materials are widely applied to the fields of high-temperature structural materials, high-temperature wave absorbing materials and nuclear reactors, and silicon carbide is used as a matrix material of a ceramic carbide based composite material, so that the silicon carbide fiber reinforced silicon carbide based composite material has the advantages of high melting point, high strength, high modulus and the like. However, silicon carbide ceramic substrates have some disadvantages, such as expensive Polycarbosilane (PCS) as a precursor for preparing the silicon carbide substrate and toxic xylene (xylene), which can cause environmental pollution; the polycarbosilane generates a large amount of gas in the high-temperature cracking process, so that the finally obtained composite material has more pores and is not compact; siC (SiC) f The dielectric constant of the SiC composite material is larger, and the wave absorbing performance can be affected to a certain extent. There is no disclosed preparation scheme of the continuous silicon carbide fiber reinforced mullite-based composite material.
Disclosure of Invention
The invention overcomes the defects of the prior art, and provides a continuous silicon carbide fiber reinforced mullite-based composite material.
In order to solve the technical problems, the invention adopts the following technical scheme: the reinforcing phase of the composite material is continuous silicon carbide fiber fabric, the main phase of the matrix is mullite, and the matrix contains one or more of alumina and silica; the silicon carbide fiber fabric is a 2.5-dimensional woven piece, and the mass content of mullite in the matrix is more than 50%; the fiber volume fraction in the composite material is not less than 30%.
The invention also provides a preparation method of the continuous silicon carbide fiber reinforced mullite-based composite material, which comprises the following steps:
1) Preparation of mullite precursor solution: directly selecting mullite sol as precursor solution or preparing by the following method: mixing silica sol, alumina sol and acid solution according to a specific sequence to obtain a clear solution;
2) Weaving 2.5-dimensional silicon carbide fiber fabric in a specific mode, and cutting into a block-shaped prefabricated member with a specific size;
3) Pouring the mullite precursor solution in the step 1) into a beaker, immersing the silicon carbide fiber fabric in the step 2) into the beaker, putting into a vacuum sealed container, and vacuumizing;
4) Repeating the step 3) until the quality of the mullite precursor solution is not reduced any more to obtain a silicon carbide preform;
5) Spin-drying residual liquid on the surface of the silicon carbide preform by using a spin-coating machine, and putting the residual liquid into a vacuum drying oven for drying pretreatment.
6) And 5) placing the pretreated silicon carbide preform in the step 5) into a carbon-carbon deposition furnace, and performing heat treatment at a specific temperature to obtain the continuous silicon carbide fiber reinforced mullite-based composite material.
Further, the preparation method of the mullite precursor solution in the step 1) comprises the following steps: mixing alkaline silica sol and acidic aluminum sol, and adjusting the two-phase sol to be neutral by one or more acids selected from citric acid, oxalic acid, hydrochloric acid, nitric acid, acetic acid and phosphoric acid.
Further, the weaving mode of the 2.5D silicon carbide fabric in the step 2) is as follows: the number of warp yarn bundles is 600-1000, the number of weft yarn bundles is 600-1000, warp yarns are bent, and weft yarns are straight.
Further, the weaving mode of the 2.5D silicon carbide fabric in the step 2) is as follows: 600-1000 of warp yarn bundles, 600-1000 of weft yarn bundles, straight warp yarn and bent weft yarn.
Further, the block-shaped prefabricated member cut by the continuous silicon carbide fiber fabric in the step 2) has the length of 1000-5000mm, the width of 40-60mm, the thickness of 2-4mm and the volume fraction of 30% -50% of the composite material.
Further, the vacuum degree of the vacuum pumped in the step 3) is 3-10kPa.
Further, in the step 6), the heating rate of the heat treatment is 3-20 ℃/min, the heat treatment is carried out at 500-1500 ℃, and the heat treatment atmosphere is N 2 、Ar、O 2 One or more of the air and the temperature control is adopted to cool down or naturally cool down to the room temperature.
Compared with the prior art, the invention has the following beneficial effects:
1. the continuous silicon carbide fiber reinforced mullite-based composite material has excellent high temperature resistance and mechanical property, and the matrix raw material has low price and wide sources. The matrix components of the composite material are regulated and controlled by adjusting the preparation mode of the mullite precursor solution, so that the mechanical properties of the continuous silicon carbide fiber reinforced mullite-based composite material are controlled.
2. The continuous silicon carbide fiber reinforced mullite-based composite material adopts a sol-gel-sintering process, has simple process flow, can be used for forming large-scale complex components, and is easy for industrial production and application.
3. The invention adopts the sol with specific proportion, ensures high impregnation efficiency and good fluidity of the matrix precursor in the impregnation process, and can not block the impregnation channel.
Drawings
FIG. 1 is a photograph of a 2.5D-dimensional silicon carbide fiber fabric in example 1 of the present invention.
FIG. 2 is a graph showing the fracture morphology of the composite material of example 1 of the present invention.
Description of the embodiments
The invention is further illustrated below with reference to specific examples.
Examples
The reinforced phase of the composite material is a continuous silicon carbide fiber woven piece, the weaving mode of the 2.5D silicon carbide preform is that the number of warp yarns is 600-1000, the number of weft yarns is 600-1000, and the warp yarns are straight and the weft yarns are bent. 90% of mullite in the ceramic matrix by mass; the fiber volume fraction in the composite was 45%.
The embodiment also provides a preparation method of the continuous silicon carbide fiber reinforced mullite-based composite material, which comprises the following steps:
(1) Mullite sol is selected as a precursor solution.
(2) Cutting the woven 2.5D silicon carbide preform (length 1000 mm. Times. Width 40 mm. Times. Thickness 2.5 mm) into small blocks with length 60 mm. Times. Width 40 mm. Times. Thickness 3mm, taking 5 blocks, placing into a self-assembled dipping tank, taking 5 blocks, immersing into a beaker, placing into a self-assembled vacuum sealed container, and vacuumizing to 8kPa.
(3) Repeating the step 2) until the quality of the mullite precursor solution is not reduced.
(4) Rapidly placing the glass fiber into a spin coater to throw off residual liquid on the surface, further wiping the residual liquid with weighing paper, avoiding sucking out mixed sol immersed into the prefabricated member, placing the glass fiber into a vacuum drying oven to carry out drying pretreatment, wherein the vacuum degree is 0.085MPa, the heating rate is 3 ℃/min, and the heat preservation temperature is 60 ℃/2h-80 ℃/2h-120 ℃/2h-150 ℃/1h.
(5) And (3) placing the pretreated silicon carbide preform into a vacuum sintering furnace, heating at a heating rate of 7 ℃/min, performing heat treatment at 1200 ℃ for 3 hours, and then adopting natural cooling to room temperature to finish the preparation of the composite material.
Fig. 1 is a 2.5-dimensional silicon carbide fiber fabric woven in this example, and fig. 2 is a fracture morphology of the composite material in this example. The mechanical properties of the composite material prepared in this example were tested, and the flexural strength of the composite material was 223MPa.
Examples
The reinforced phase of the composite material is continuous silicon carbide fiber fabric, the weaving mode of the 2.5D silicon carbide preform is that the number of warp yarns is 600-1000, the number of weft yarns is 600-1000, and warp yarns are bent and weft yarns are straight. The mass content of mullite in the ceramic matrix is 70%; the fiber volume fraction in the composite was 40%.
The embodiment also provides a preparation method of the continuous silicon carbide fiber reinforced mullite-based composite material, which comprises the following steps:
(1) Mixing alkaline silica sol and acidic aluminum sol, adjusting the two-phase sol to be neutral by citric acid with pH=1, and adopting a mode of dropwise adding and stirring.
(2) Cutting the woven 2.5D silicon carbide preform (length 1000 mm. Times. Width 40 mm. Times. Thickness 2.5 mm) into small blocks with length 60 mm. Times. Width 40 mm. Times. Thickness 2.5mm, immersing 5 blocks in a beaker, placing in a vacuum-tight container which is assembled by oneself, and vacuumizing to 5kPa.
(3) Repeating the step 2) until the quality of the mullite precursor solution is not reduced.
(4) Rapidly placing the solution on a spin coater to throw off the residual liquid on the surface, further wiping the residual liquid clean by using weighing paper, placing the solution in a vacuum drying oven for drying pretreatment, wherein the vacuum degree is-0.08 MPa, the heating rate is 2 ℃/min, and the heat preservation temperature is 80 ℃/2-100 ℃/2-120 ℃/2-150 ℃/1h.
(5) And (3) placing the pretreated silicon carbide preform into a carbon/carbon sintering furnace, heating at a speed of 10 ℃/min, performing heat treatment at 1100 ℃ for 3 hours, and then adopting natural cooling to room temperature to finish the preparation of the composite material.
The mechanical properties of the composite material prepared in this example were tested, and the flexural strength of the composite material was 205MPa.
Claims (8)
1. The continuous silicon carbide fiber reinforced mullite-based composite material is characterized in that the reinforced phase of the composite material is continuous silicon carbide fiber fabric, the main phase of a matrix is mullite, and the matrix contains one or more of alumina and silica; the silicon carbide fiber fabric is a 2.5-dimensional woven piece, and the mass content of mullite in the matrix is more than 50%; the fiber volume fraction in the composite material is not less than 30%.
2. The method for preparing the continuous silicon carbide fiber reinforced mullite-based composite material as set forth in claim 1, comprising the steps of:
1) Preparation of mullite precursor solution: directly selecting mullite sol as precursor solution or preparing by the following method: mixing silica sol, alumina sol and acid solution according to a specific sequence to obtain a clear solution;
2) Weaving 2.5-dimensional silicon carbide fiber fabric in a specific mode, and cutting into a block-shaped prefabricated member with a specific size;
3) Pouring the mullite precursor solution in the step 1) into a beaker, immersing the silicon carbide fiber fabric in the step 2) into the beaker, putting into a vacuum sealed container, and vacuumizing;
4) Repeating the step 3) until the quality of the mullite precursor solution is not reduced any more to obtain a silicon carbide preform;
5) Spin-drying residual liquid on the surface of the silicon carbide preform by using a spin coater, and putting the residual liquid into a vacuum drying oven for drying pretreatment;
6) And 5) placing the pretreated silicon carbide preform in the step 5) into a carbon-carbon deposition furnace, and performing heat treatment at a specific temperature to obtain the continuous silicon carbide fiber reinforced mullite-based composite material.
3. The method for preparing the continuous silicon carbide fiber reinforced mullite-based composite material according to claim 2, wherein the preparation method of the mullite precursor solution in the step 1) is as follows: mixing alkaline silica sol and acidic aluminum sol, and adjusting the two-phase sol to be neutral by one or more acids selected from citric acid, oxalic acid, hydrochloric acid, nitric acid, acetic acid and phosphoric acid.
4. The method for preparing the continuous silicon carbide fiber reinforced mullite-based composite material according to claim 2, wherein the weaving method of the 2.5D silicon carbide fabric in the step 2) is as follows: the number of warp yarn bundles is 600-1000, the number of weft yarn bundles is 600-1000, warp yarns are bent, and weft yarns are straight.
5. The method for preparing the continuous silicon carbide fiber reinforced mullite-based composite material according to claim 2, wherein the weaving method of the 2.5D silicon carbide fabric in the step 2) is as follows: 600-1000 of warp yarn bundles, 600-1000 of weft yarn bundles, straight warp yarn and bent weft yarn.
6. The method for preparing the continuous silicon carbide fiber reinforced mullite-based composite material according to claim 2, wherein the block-shaped prefabricated member cut by the continuous silicon carbide fiber fabric in the step 2) has a length of 1000-5000mm, a width of 40-60mm, a thickness of 2-4mm and a volume fraction of 30% -50% of the composite material.
7. The method for producing a continuous silicon carbide fiber reinforced mullite-based composite material according to claim 2, wherein the vacuum degree of the vacuum in the step 3) is 3 to 10kPa.
8. The method for preparing a continuous silicon carbide fiber reinforced mullite-based composite material according to claim 2, wherein in the step 6), the heating rate of the heat treatment is 3-20 ℃/min, the heat treatment is performed at 500-1500 ℃, and the heat treatment atmosphere is N 2 、Ar、O 2 One or more of the air and the temperature control is adopted to cool down or naturally cool down to the room temperature.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202310426528.4A CN116375461A (en) | 2023-04-20 | 2023-04-20 | Continuous silicon carbide fiber reinforced mullite-based composite material and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202310426528.4A CN116375461A (en) | 2023-04-20 | 2023-04-20 | Continuous silicon carbide fiber reinforced mullite-based composite material and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN116375461A true CN116375461A (en) | 2023-07-04 |
Family
ID=86980608
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202310426528.4A Pending CN116375461A (en) | 2023-04-20 | 2023-04-20 | Continuous silicon carbide fiber reinforced mullite-based composite material and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN116375461A (en) |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100901458B1 (en) * | 2008-05-01 | 2009-06-08 | 한국전기연구원 | Heating element impregnated with sol |
CN104860695A (en) * | 2015-04-30 | 2015-08-26 | 中国人民解放军国防科学技术大学 | Three-dimensional fiber prefabricated-part enhancement mullite composite and preparation method thereof |
-
2023
- 2023-04-20 CN CN202310426528.4A patent/CN116375461A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100901458B1 (en) * | 2008-05-01 | 2009-06-08 | 한국전기연구원 | Heating element impregnated with sol |
CN104860695A (en) * | 2015-04-30 | 2015-08-26 | 中国人民解放军国防科学技术大学 | Three-dimensional fiber prefabricated-part enhancement mullite composite and preparation method thereof |
Non-Patent Citations (3)
Title |
---|
HUI GAO等: ""Influence of different matrices on the mechanical and microwave absorption properties of SiC fiber-reinforced oxide matrix composites", CERAMICS INTERNATIONAL, vol. 44, no. 6, pages 6010 - 6015 * |
梁松林;马青松;刘海韬;戴科伟;: "Sol-Gel工艺制备三维碳纤维增强Al_2O_3-SiO_2基复合材料研究", 稀有金属材料与工程, no. 1, pages 585 - 589 * |
高慧等: "SiCf/mullite复合材料制备工艺及吸波性能研究", 万方期刊网, pages 1 - 115 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN109293383B (en) | Fiber-reinforced carbon-silicon carbide ceramic matrix composite and preparation method thereof | |
CN109053207B (en) | Yttrium silicate modified silicon carbide fiber reinforced silicon carbide composite material and preparation method thereof | |
CN107353025B (en) | Preparation method of 1200-DEG C-resistant and oxidation-resistant ceramic matrix composite | |
US5371050A (en) | Aluminum phosphate bonded fiber reinforced composite material containing metal coated fibers | |
CN107540400A (en) | A kind of SiC with compound interfacef/ SiC ceramic based composites | |
CN109553430A (en) | A kind of SiC with compound interfacef/ SiC ceramic based composites and preparation method thereof | |
CN100363303C (en) | Silicon carbide base multiphase composite ceramic and its preparation method | |
CN104261850A (en) | High-temperature-resistant wave-transparent silicon nitride fiber-reinforced composite material and preparation method thereof | |
CN110002892A (en) | A kind of hafnium tantalum silicon ternary complex phase ceramic presoma, carbon/hafnium tantalum carbon solid solution-carbon/silicon carbide ceramic matrix composite and preparation method thereof | |
CN112374917B (en) | High-temperature ceramic coating and preparation method thereof | |
CN105016759A (en) | Rapid preparation method for C/SiC composite material | |
CN112341235A (en) | Multiphase coupling rapid densification method for ultrahigh-temperature self-healing ceramic matrix composite | |
CN109293367B (en) | Cerium phosphate modified silicon carbide fiber reinforced silicon carbide composite material and preparation method thereof | |
CN114656275B (en) | SiC preparation by vacuum impregnation combined with reaction melt infiltration f Method for preparing/Si-Y-B-C composite material | |
CN113880597B (en) | Preparation method of modified carbon fiber toughened alumina self-healing ceramic | |
CN104926346B (en) | A kind of alumina fibre fabric containing interface phase strengthens silicon carbide ceramics and preparation method thereof | |
CN102659442A (en) | Preparation method for oxide fiber toughened silicon dioxide ceramic-based composite material gap interface | |
CN112898023A (en) | Cf/Ta4HfC5-SiC superhigh temperature ceramic matrix composite material and preparation method thereof | |
CN115385712A (en) | High-entropy ultra-high temperature ceramic matrix composite and preparation method thereof | |
CN104926343B (en) | Aluminum silicate fiber reinforced oxide ceramic containing interface phase and preparation method thereof | |
CN110304932B (en) | Preparation method of Cf/SiC composite material with HfB2 interface | |
CN112521156B (en) | Hybrid matrix SiCf/SiC composite material and preparation method thereof | |
CN114045671B (en) | Continuous oxide fiber fabric with lanthanum phosphate layer and preparation method thereof | |
CN110407597A (en) | A kind of rare-earth oxide modified carbon/silicon carbide ceramic matrix composite and preparation method thereof | |
CN116375461A (en) | Continuous silicon carbide fiber reinforced mullite-based composite material 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 |