CN114751760A - Method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite material through nano-impregnation transient eutectic - Google Patents
Method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite material through nano-impregnation transient eutectic Download PDFInfo
- Publication number
- CN114751760A CN114751760A CN202210441983.7A CN202210441983A CN114751760A CN 114751760 A CN114751760 A CN 114751760A CN 202210441983 A CN202210441983 A CN 202210441983A CN 114751760 A CN114751760 A CN 114751760A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- nano
- nanofiber
- sic
- single crystal
- 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 153
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 128
- 239000002121 nanofiber Substances 0.000 title claims abstract description 85
- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 31
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 24
- 238000005470 impregnation Methods 0.000 title claims abstract description 17
- 230000005496 eutectics Effects 0.000 title claims abstract description 12
- 230000001052 transient effect Effects 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 title description 12
- 238000005245 sintering Methods 0.000 claims abstract description 49
- 239000002002 slurry Substances 0.000 claims abstract description 26
- 239000000919 ceramic Substances 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 25
- 239000002131 composite material Substances 0.000 claims abstract description 22
- 238000007731 hot pressing Methods 0.000 claims abstract description 20
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 15
- 238000000748 compression moulding Methods 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000007598 dipping method Methods 0.000 claims abstract description 11
- 238000000151 deposition Methods 0.000 claims abstract description 9
- 238000004537 pulping Methods 0.000 claims abstract description 8
- 239000002270 dispersing agent Substances 0.000 claims abstract description 6
- 238000003475 lamination Methods 0.000 claims abstract description 3
- 239000010410 layer Substances 0.000 claims description 26
- 239000000843 powder Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 10
- 239000011247 coating layer Substances 0.000 claims description 8
- 238000010030 laminating Methods 0.000 claims description 8
- 239000011858 nanopowder Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 6
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 6
- 241001330002 Bambuseae Species 0.000 claims description 6
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 6
- 239000011425 bamboo Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 239000012495 reaction gas Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000835 fiber Substances 0.000 abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910002804 graphite Inorganic materials 0.000 abstract description 5
- 239000010439 graphite Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 12
- 235000015895 biscuits Nutrition 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 238000005452 bending Methods 0.000 description 5
- 239000002070 nanowire Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000000197 pyrolysis Methods 0.000 description 4
- 230000002787 reinforcement Effects 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 238000004513 sizing Methods 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000011184 SiC–SiC matrix composite Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 0.000 description 1
- 229920003257 polycarbosilane Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 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
- C04B35/71—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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/575—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by pressure sintering
-
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62844—Coating fibres
- C04B35/62857—Coating fibres with non-oxide ceramics
- C04B35/62873—Carbon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
-
- 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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
-
- 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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
-
- 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
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
-
- 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
- C04B2235/602—Making the green bodies or pre-forms by moulding
-
- 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
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
-
- 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)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Structural Engineering (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a method for preparing a single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite by using nano dipping transient eutectic. Firstly, adopting single crystal silicon carbide nano fibers as a raw material, and depositing an interface layer on the surface of the fibers by using a chemical vapor deposition method; dispersing and pulping the nano-fiber containing the interface layer, and preparing SiC nano-fiber paper with a three-dimensional network structure by a pulping and papermaking process; putting the fiber paper into nano slurry containing a sintering aid, silicon carbide powder and a dispersing agent for vacuum impregnation; after vacuum impregnation is completed, taking out the SiC prepreg tape/sheet for drying, and then carrying out lamination compression molding on the dried prepreg tape/sheet in a mold; and putting the molded preform into a graphite mold, and performing hot-pressing sintering to finish the preparation. Compared with the traditional silicon carbide ceramic, the silicon carbide ceramic has higher fracture toughness and strength, and has important significance for exploring a novel SiCf/SiC composite material.
Description
Technical Field
The invention relates to a preparation method of a silicon carbide ceramic matrix composite, in particular to a preparation technology for preparing a single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite by nanometer dipping transient eutectic.
Background
The silicon carbide ceramic material has the characteristics of light weight, oxidation resistance, thermal shock resistance, radiation resistance, high temperature resistance and the like, and has very wide application prospect in the fields of aviation, aerospace, automobiles, nuclear reactors and the like. However, the characteristics of the SiC ceramics such as intrinsic brittleness and poor reliability have adverse effects on the application and development of the SiC ceramics as a structural material in various fields. Therefore, the development of the preparation technology of the high-strength and high-toughness silicon carbide ceramic matrix composite material has important significance for the application of silicon carbide ceramics and the development of structural ceramics.
At present, the preparation methods of the silicon carbide ceramic matrix composite mainly include a precursor cracking method (PIP), an infiltration Method (MI), a chemical vapor infiltration method (CVI), a nano-impregnation transient eutectic method (NITE) and the like. The CVI process is characterized in that a precursor is introduced into a reaction furnace, and a certain substance is continuously and repeatedly deposited inside a porous fiber fabric prefabricated body to prepare the composite material, wherein the prepared ceramic matrix has high purity and complete crystal form, but the process has long period and high preparation cost, and the SiCf/SiC composite material is difficult to highly densify. The PIP process is characterized in that under a certain temperature and pressure, liquid polymers (such as polycarbosilane, polysilane and the like) with a proper theoretical atomic ratio are impregnated into a porous fiber fabric preform, crosslinking and curing are carried out under the protection of inert gas, then high-temperature pyrolysis treatment is carried out to convert the precursor polymers into a ceramic matrix, and due to pores formed by escape of small molecules in the pyrolysis process and volume shrinkage after pyrolysis of the matrix, impregnation-curing-pyrolysis needs to be carried out repeatedly for many times, but the prepared SiC/SiC composite material still has a large porosity. The MI process is a process in which a SiC-based composite material is prepared by infiltrating molten Si into a silicon carbide fiber-reinforced porous body at a high temperature, and compared with the former two processes, the prepared composite material has a higher compactness and a significantly reduced porosity, but since a certain amount of free silicon exists in the composite material, the composite material may react or volatilize at a high temperature to reduce the strength of the material, which is not favorable for the composite material to be used at a high temperature for a long time. The NITE process is to dip SiC fibers by nano SiC powder and then carry out hot-pressing sintering, thereby preparing the SiC/SiC composite material with high compactness and high performance.
At present, the problems of large brittleness, low density, poor reliability and the like still exist in the silicon carbide ceramic matrix composite material.
Disclosure of Invention
In order to solve the problems in the background technology, the invention provides a method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite by nano dipping transient eutectic by analyzing the structure of the transient eutectic solidification structure of the alumina-based eutectic ceramic and designing the interface structure of the reinforcement. The single crystal silicon carbide nanofiber/silicon carbide ceramic-based composite material is prepared by the processes of gas phase coating of the nano silicon carbide fibers, preparation of the nano SiC fiber paper, preparation of a nano prepreg tape/sheet, further compression molding, hot-pressing sintering and the like. According to the invention, through single-layer and multi-layer reinforcement interface design, compression molding structure design of the nano prepreg tape/sheet and liquid phase mass transfer effect of the sintering aid in the NITE process at high temperature, the prepared composite material has the outstanding advantages of high toughness, high strength and the like.
The technical scheme adopted by the invention comprises the following steps:
1) preparing an interface coating layer of the SiC nano-fibers: placing the cotton-shaped single crystal silicon carbide nano-fibers into a tube furnace for CVD deposition to obtain nano-fibers containing an interface layer;
2) preparing SiC nanofiber paper: dispersing silicon carbide nano-fibers containing an interface layer in a solution, and adopting a pulp making and paper making process to obtain nano-fiber paper with a three-dimensional network structure;
3) preparing nano slurry: mixing and dispersing silicon carbide micro-nano powder, a sintering aid, a solvent and a dispersing agent to obtain nano impregnation slurry;
4) preparation of prepreg tape/sheet: putting the nanofiber paper obtained in the step 2) into the slurry obtained in the step 3) for vacuum impregnation, taking out after complete impregnation, and drying to obtain a prepreg tape/sheet;
5) compression molding of the nanofiber paper prepreg tape/sheet lamination: laminating the prepreg tape/sheet obtained in the step 4) in a mould, and then carrying out compression molding;
6) hot-pressing and sintering: and (3) sintering and molding the preform subjected to compression molding in the step 5) in a hot-pressing sintering manner to obtain the single-crystal silicon carbide nanofiber/silicon carbide ceramic-based composite material.
The step 1) is specifically as follows:
introducing reaction gas and protective gas with the volume ratio of 1 (3-5) into a tubular furnace, and obtaining an interface coating layer with the deposition thickness of 5 nm-50 nm by a Chemical Vapor Deposition (CVD) method for the monocrystalline silicon carbide nano-fiber placed in the tubular furnace;
the reaction conditions of the chemical vapor deposition method are as follows: preserving the heat for 1 to 10 hours at the temperature of 1100 to 1300 ℃, wherein the reaction pressure is 0.015 to 0.03 MPa.
The reaction gas is methane, propane, boron trichloride, ammonia gas and the like, and the protective gas is inert gas such as argon, nitrogen and the like.
The interface layer is composed of single-layer PyC, BN, SiC or composite interface layer (PyC-SiC) n, (BN/PyC) n.
The step 2) is specifically as follows:
dispersing silicon carbide nano fibers containing the interface layer in an aqueous solution in a magnetic stirring manner, then pulping and molding the silicon carbide nano fibers in the dispersed silicon carbide nano fiber solution by using a bamboo curtain net, and finally drying to obtain the nano fiber paper with the three-dimensional network structure.
The drying conditions are as follows: and drying and forming the nano-fiber paper on a heating platform at the temperature of 100-150 ℃ under the pressure of 100-500N so as to keep the flatness and the integrity of the nano-fiber paper.
The thickness of the obtained nanofiber paper after drying is 0.1 mm-2 mm.
In the step 3):
the mass ratio of the silicon carbide micro-nano powder to the sintering aid to the solvent to the dispersant is (7-9): 1, (50-75): 0.1-0.3); the mixing and dispersing mode is ball milling or stirring;
the preferable mass ratio is 8:1 (50-60): 0.2.
The ball milling mode is that ball milling is carried out for 6-12 h at the rotating speed of (150-. The ball milling mode is high-energy ball milling, vibration ball milling, planetary ball milling and the like;
the stirring mode is mechanical stirring or magnetic stirring.
The solvent is water or absolute ethyl alcohol.
The step 4) is specifically as follows:
immersing the nanofiber paper in the slurry, and then putting the nanofiber paper into a vacuum drying oven with the vacuum degree of-0.06 to-0.1 MPa for vacuum impregnation, wherein the pressure maintaining time is 0.5 to 2 hours; and drying the completely impregnated nano-fiber paper and the residual slurry at the temperature of between 80 and 100 ℃ to obtain a pre-impregnated tape/sheet and slurry powder.
The step 5) is specifically that,
and (2) alternately laying the prepreg tapes/sheets and the slurry powder in a die in a laminated manner, laying the slurry powder between two adjacent prepreg tapes/sheets, and carrying out compression molding on a plurality of nano prepreg tapes/sheets which are arranged in a laminated manner under a certain compression molding condition to prepare a uniform prefabricated body.
The mass of the slurry powder in the uniform preform is 0.1 g-2 g.
The mould pressing condition is that the pressure is maintained for 10min to 30min under the pressure of 10MPa to 30MPa, and the fiber fracture is easily caused by overlarge pressure, so that the overall performance of the composite material is influenced.
In the step 6):
the hot-pressing sintering is to put the prefabricated body into a hot-pressing sintering furnace to be heated to 1700-1900 ℃ at the heating rate of 5-10 ℃/min, and then to be sintered and molded for 1 hour under the pressure of 10-30 MPa.
The preferred reaction temperature is 1850 ℃; the preferred sintering pressure is 30 MPa.
The invention provides a method for preparing a single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite material by adopting a nano dipping transient eutectic method in a hot pressing sintering furnace. The silicon carbide nanofiber paper with the three-dimensional network structure prepared by the invention can fully exert the advantages of high elastic modulus and high strength of the monocrystalline silicon carbide nanowires, and can promote the densification of the composite material by utilizing the liquid-phase mass transfer effect of the oxide sintering aid at high temperature; meanwhile, the laminated compression molding in the invention is beneficial to the performance advantage of laminating the silicon carbide nanofiber paper in the fixed direction, and further realizes the reinforcement and toughening of the composite material. The silicon carbide ceramic matrix composite with higher strength and toughness can be prepared by simpler steps of coating, ball milling, dipping, sintering and the like.
Compared with the traditional ceramic matrix composite preparation method, the preparation process is simpler, and the prepared silicon carbide ceramic matrix composite has higher strength and toughness, and is expected to be industrially applied in high and new technical fields such as aviation and aerospace hot end components, nuclear reactors and the like.
The invention has the beneficial effects that:
1) the invention adopts single crystal silicon carbide nanometer fiber paper with a three-dimensional network structure as a raw material, and carries out single-layer and multi-layer interface structure design on the nanometer SiC fiber so as to achieve the purpose of giving full play to the performance advantages of the silicon carbide nanometer wire. According to the analysis of the transient eutectic solidification structure of the alumina-based eutectic ceramic, the invention provides the method for realizing the densification of the composite material by utilizing the mass transfer effect of the liquid-phase sintering aid in the NITE method at high temperature.
2) The laminated compression molding process is favorable for the performance advantage of laminating the silicon carbide nanofiber paper in a specific direction, and further realizes the reinforcement and toughening of the composite material.
3) The silicon carbide ceramic matrix composite with higher strength and toughness can be prepared by simpler steps of coating, ball milling, dipping, sintering and the like.
4) Compared with the traditional ceramic matrix composite preparation method, the preparation process is simple, and the prepared silicon carbide ceramic matrix composite has high strength and toughness and has wide application prospect in high and new technical fields such as aerospace hot-end parts, nuclear reactors and the like.
Drawings
Fig. 1 is a physical image and a high-power scanning electron microscope image of the SiC nanofiber paper used in the present invention.
FIG. 2 is a cross-sectional profile of the ceramic of example 1.
FIG. 3 is a three-point bending resistance test load-displacement curve diagram of the SiC nanofiber reinforced silicon carbide ceramic matrix composite prepared in example 1 of the present invention.
FIG. 4 is a cross-sectional profile of the ceramic of example 3.
FIG. 5 is a three-point bending resistance test load-displacement curve diagram of the SiC nanofiber reinforced silicon carbide ceramic matrix composite prepared in example 3 of the present invention.
Detailed Description
The invention is further illustrated by the following figures and examples. These embodiments are merely illustrative of the present invention and are not intended to limit the scope of the present invention.
The examples of the invention are as follows:
example 1:
a. weighing 2g of SiC nano-fiber in a tube furnace, and introducing CH4And N2And depositing a PyC coating layer on the surface of the SiC nanowire by adopting a Chemical Vapor Deposition (CVD) method. The reaction conditions are as follows: 1100 deg.C, CH4And N2The flow rates of the silicon carbide nano-fibers are respectively 20mL/min and 40mL/min, and the silicon carbide nano-fibers containing the PyC interface layer are obtained after reaction for 60 min.
b. And (b) placing the SiC nano-fiber containing the interface layer in the step a into an ethanol solution, magnetically stirring for 30min for dispersion, then pulping and making paper by using a bamboo curtain net, standing for 1h at room temperature for draining, and finally drying in an oven at 80 ℃ for 6h to obtain the SiC nano-fiber paper containing the interface layer.
c. Weighing 15.6g of silicon carbide micro-nano powder and 2.4g of sintering aid, and putting the powder and the sintering aid into a ball milling tank, wherein Al in the sintering aid2O3And Y2O3The mass ratio of (A) is 3:2, 100mL of absolute ethyl alcohol is added as a solvent, and then wet ball milling is carried out at the speed of 300r/min for 12h to obtain the dipping slurry.
d. The SiC containing PyC interface layer in the step bnfAnd (c) putting the paper into the SiC sizing agent in the step c, carrying out vacuum impregnation for 30min, taking out and drying, and repeating for 3 times. Then drying the SiCnfPre-soaking paper and the residual slurry, and sieving the dried powder with a 100-mesh sieve.
e. Laminating SiC obtained in step dnfThe pre-impregnated paper and the SiC powder are crossly spread in a die and are dry-pressed and molded under the pressure of 15MPa to obtain SiCnfA SiC biscuit.
f. Loading the biscuit into a hot-pressing graphite die, and preparing SiC by vacuum hot-pressing sinteringnfThe sintering temperature of the/SiC ceramic matrix composite material is 1850 ℃, the sintering pressure is 20MPa, and the heat preservation and pressure maintaining are carried out for 1 h.
g. The ceramic sample is cut into standard test strips of 3mm multiplied by 4mm multiplied by 40mm, and then subjected to density and mechanical property tests after grinding, polishing and chamfering treatment.
h. The fracture toughness and the bending strength of the ceramic sample in the present embodiment are 17.68. + -. 1.22 MPa. m1/2 and 423.5. + -. 7.85MPa, respectively.
As shown in FIG. 1, (a) is a real image of SiC nanofiber paper, and (b) is a high-magnification scanning electron microscope image of SiC nanofiber paper
As shown in fig. 2, it can be seen from the SEM image that the ceramic prepared according to the present invention has a phenomenon of fiber extraction bridging.
As shown in fig. 3, as can be seen from the bending test load-displacement graph of the composite material prepared in example 1, the composite material exhibited pseudo-plastic fracture behavior.
Example 2:
a. weighing 2g of SiC nano-fiber paper, placing the SiC nano-fiber paper in a tube furnace, and introducing CH4And N2And depositing a PyC coating layer on the surface of the SiC nanowire by adopting a Chemical Vapor Deposition (CVD) method. The reaction conditions are as follows: 1100 ℃ C, CH4And N2The flow rates of the above steps are respectively 20mL/min and 40mL/min, and the silicon carbide nanofiber paper containing the PyC interface layer is obtained after reaction for 90 min.
b. And (b) placing the SiC nano-fiber containing the interface layer in the step a into an ethanol solution, magnetically stirring for 30min for dispersion, then pulping and making paper by using a bamboo curtain net, standing for 1h at room temperature for draining, and finally drying in an oven at 80 ℃ for 6h to obtain the SiC nano-fiber paper containing the interface layer.
c. Weighing 15.6g of silicon carbide micro-nano powder and 2.4g of sintering aid, and putting the powder and the sintering aid into a ball milling tank, wherein Al in the sintering aid2O3And Y2O3The mass ratio of (2) is 3:2, 100mL of absolute ethyl alcohol is added as a solvent, and then wet ball milling is carried out for 12 hours at the speed of 300r/min to obtain the dipping slurry.
d. Mixing SiC containing PyC interface layer in the step bnfAnd (c) putting the paper into the SiC sizing agent in the step c, carrying out vacuum impregnation for 30min, taking out and drying, and repeating for 3 times. Then drying the SiCnfPre-soaking paper and the residual slurry, and sieving the dried powder with a 100-mesh sieve.
e. Laminating SiC obtained in step dnfThe pre-impregnated paper and the SiC powder are crossly spread in a die and are dry-pressed and molded under the pressure of 15MPa to obtain SiCnfA SiC biscuit.
f. Loading the biscuit into a hot-pressing graphite die, and preparing SiC by vacuum hot-pressing sinteringnfThe sintering temperature of the/SiC ceramic matrix composite material is 1850 ℃, the sintering pressure is 20MPa, and the heat preservation and pressure maintaining are carried out for 1 h.
g. The ceramic sample is cut into standard test strips of 3mm multiplied by 4mm multiplied by 40mm, and then subjected to density and mechanical property tests after grinding, polishing and chamfering treatment.
h. The fracture toughness and the bending strength of the ceramic sample in the present embodiment were 17.69. + -. 1.72MPa · m, respectively1/2、416±13.88MPa。
Example 3:
a. weighing 2g of SiC nano-fiber paper, placing the SiC nano-fiber paper in a tube furnace, and introducing CH4And N2And depositing a PyC coating layer on the surface of the SiC nanowire by adopting a Chemical Vapor Deposition (CVD) method. The reaction conditions are as follows: 1100 ℃ C, CH4And N2The flow rates of the above steps are respectively 20mL/min and 40mL/min, and the silicon carbide nanofiber paper containing the PyC interface layer is obtained after reaction for 120 min.
b. And (b) placing the SiC nano-fiber containing the interface layer in the step (a) into an ethanol solution, magnetically stirring for 30min for dispersion, then pulping and making paper by using a bamboo curtain net, standing for 1h at room temperature for draining, and finally drying in an oven at 80 ℃ for 6h to obtain the SiC nano-fiber paper containing the interface layer.
c. Weighing 15.6g of silicon carbide micro-nano powder and 2.4g of sintering aid, and putting the powder and the sintering aid into a ball milling tank, wherein Al in the sintering aid2O3And Y2O3The mass ratio of (2) is 3:2, 100mL of absolute ethyl alcohol is added as a solvent, and then wet ball milling is carried out for 12 hours at the speed of 300r/min to obtain the dipping slurry.
d. The SiC containing PyC interface layer in the step bnfAnd (c) putting the paper into the SiC sizing agent in the step c, carrying out vacuum impregnation for 30min, taking out and drying, and repeating for 3 times. Then drying the SiCnfPre-soaking paper and the residual slurry, and sieving the dried powder with a 100-mesh sieve.
e. Laminating SiC in the step dnfThe pre-impregnated paper and the SiC powder are crossly spread in a die and are dry-pressed and molded under the pressure of 15MPa to obtain SiCnfA SiC biscuit.
f. Loading the biscuit into a hot-pressing graphite die, and preparing SiC by vacuum hot-pressing sinteringnfThe sintering temperature of the/SiC ceramic matrix composite material is 1850 ℃, the sintering pressure is 20MPa, and the heat preservation and pressure maintaining are carried out for 1 h.
g. The ceramic sample is cut into standard test strips of 3mm multiplied by 4mm multiplied by 40mm, and then subjected to density and mechanical property tests after grinding, polishing and chamfering treatment.
h. The fracture toughness and the flexural strength of the ceramic sample in this example were 21.73. + -. 1.74 MPa-m, respectively1/2、150.75±12.55MPa。
As shown in fig. 4, it can be seen from the SEM image that the ceramic prepared according to the present invention shows a large amount of fiber pullout and fiber bridging.
As shown in fig. 5, as can be seen from the bending test load-displacement graph of the composite material prepared in example 3, the composite material exhibited pseudo-plastic fracture behavior.
Example 4:
a. weighing 2g of SiC nanofiber paper, placing the SiC nanofiber paper in a tube furnace, and introducing CH4And N2And depositing a PyC coating layer on the surface of the SiC nanowire by adopting a Chemical Vapor Deposition (CVD) method. The reaction conditions are as follows: 1100 ℃ C, CH4And N2The flow rates of the above steps are respectively 20mL/min and 40mL/min, and after reaction for 150min, the silicon carbide nanofiber paper containing the PyC interface layer is obtained.
b. And (3) placing the SiC nano-fiber containing the interface layer into an ethanol solution, magnetically stirring for 30min for dispersing, then pulping and making paper by using a bamboo screen mesh, standing for 1h at room temperature for draining, and finally drying in an oven at 80 ℃ for 6h to obtain the SiC nano-fiber paper containing the interface layer.
c. Weighing 15.6g of silicon carbide micro-nano powder and 2.4g of sintering aid, and putting the powder and the sintering aid into a ball milling tank, wherein Al in the sintering aid2O3And Y2O3The mass ratio of (A) is 3:2, 100mL of absolute ethyl alcohol is added as a solvent, 3mL of polyvinyl alcohol is added as a dispersing agent, and then wet ball milling is carried out for 12 hours at the speed of 300r/min to obtain the dipping slurry.
d. Mixing SiC containing PyC interface layer in the step bnfAnd (c) putting the paper into the SiC sizing agent in the step c, carrying out vacuum impregnation for 30min, taking out and drying, and repeating for 3 times. Then drying the SiCnfPre-soaking paper and the residual slurry, and sieving the dried powder with a 100-mesh sieve.
e. Laminating SiC obtained in step dnfThe pre-impregnated paper and the SiC powder are crossly spread in a die and are dry-pressed and molded under the pressure of 15MPa to obtain SiCnfA SiC biscuit.
f. Loading the biscuit into a hot-pressing graphite die, and preparing SiC by vacuum hot-pressing sinteringnfThe sintering temperature of the/SiC ceramic matrix composite material is 1850 ℃, the sintering pressure is 20MPa, and the heat preservation and pressure maintaining are carried out for 1 h.
g. The ceramic sample is cut into standard test strips of 3mm multiplied by 4mm multiplied by 40mm, and then subjected to density and mechanical property tests after grinding, polishing and chamfering treatment.
h. The fracture toughness and the bending strength of the ceramic sample in the present embodiment were 15.78. + -. 2.46MPa · m, respectively1/2、184±6.24MPa。
Claims (9)
1. A method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite by nano dipping transient eutectic is characterized by comprising the following steps:
1) preparing an interface coating layer of the SiC nano-fibers: putting the cotton-shaped single crystal silicon carbide nano-fiber into a tube furnace for CVD deposition to obtain nano-fiber containing an interface layer;
2) preparing SiC nanofiber paper: dispersing the silicon carbide nanofibers containing the interface layer in a solution, and obtaining nanofiber paper with a three-dimensional network structure by adopting a papermaking process;
3) preparing nano slurry: mixing and dispersing silicon carbide micro-nano powder, a sintering aid, a solvent and a dispersing agent to obtain nano impregnation slurry;
4) preparation of prepreg tape/sheet: putting the nanofiber paper obtained in the step 2) into the slurry obtained in the step 3) for vacuum impregnation, taking out after complete impregnation, and drying to obtain a prepreg tape/sheet;
5) compression molding of the nanofiber paper prepreg tape/sheet lamination: laminating the prepreg tape/sheet obtained in the step 4) in a mould, and then carrying out compression molding;
6) hot-pressing and sintering: and (3) sintering and molding the preform subjected to compression molding in the step 5) in a hot-pressing sintering manner to obtain the single-crystal silicon carbide nanofiber/silicon carbide ceramic-based composite material.
2. The method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite according to claim 1, wherein the step 1) is specifically:
introducing reaction gas and protective gas with the volume ratio of 1 (3-5) into a tubular furnace, and obtaining an interface coating layer with the deposition thickness of 5 nm-50 nm by a chemical vapor deposition method for the monocrystalline silicon carbide nano-fiber placed in the tubular furnace;
the reaction conditions of the chemical vapor deposition method are as follows: the temperature is kept at 1100-1300 ℃ for 1-10 h, and the reaction pressure is 0.015-0.03 MPa.
3. The method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite according to claim 1, wherein the step 2) is specifically,
dispersing silicon carbide nanofibers containing the interface layer in an aqueous solution in a magnetic stirring mode, then pulping and forming the silicon carbide nanofibers in the dispersed silicon carbide nanofiber solution by using a bamboo curtain net, and finally drying to obtain the nanofiber paper with a three-dimensional network structure.
4. The method for preparing single crystal SiC nanofiber/SiC ceramic matrix composite according to claim 3,
the drying conditions are as follows: drying and molding on a heating platform at 100-150 ℃ under the pressure of 100-500N;
the thickness of the obtained nanofiber paper after drying is 0.1 mm-2 mm.
5. The method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite according to claim 1, wherein the method comprises the following steps: in the step 3):
the mass ratio of the silicon carbide micro-nano powder to the sintering aid to the solvent to the dispersant is (7-9) to (1), (50-75) to (0.1-0.3); the mixing and dispersing mode is ball milling or stirring;
the solvent is water or absolute ethyl alcohol.
6. The method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite according to claim 1, wherein the method comprises the following steps: the step 4) is specifically as follows:
immersing the nanofiber paper in the slurry, and then putting the nanofiber paper into a vacuum drying oven with the vacuum degree of-0.06 to-0.1 MPa for vacuum impregnation, wherein the pressure maintaining time is 0.5 to 2 hours; and drying the completely impregnated nano-fiber paper and the residual slurry at the temperature of between 80 and 100 ℃ to obtain a pre-impregnated tape/sheet and slurry powder.
7. The method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite according to claim 1, wherein the method comprises the following steps: the step 5) is specifically that,
and (2) alternately laying the prepreg tapes/sheets and the slurry powder in a die in a laminated manner, laying the slurry powder between two adjacent prepreg tapes/sheets, and carrying out compression molding on a plurality of nano prepreg tapes/sheets which are arranged in a laminated manner under a certain compression molding condition to prepare a uniform prefabricated body.
8. The method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite according to claim 7, wherein the method comprises the following steps: the mould pressing condition is that the pressure is maintained for 10min to 30min under the pressure of 10MPa to 30 MPa.
9. The method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite according to claim 1, wherein the method comprises the following steps: in the step 6):
the hot-pressing sintering is to put the prefabricated body into a hot-pressing sintering furnace to be heated to 1700-1900 ℃ at the heating rate of 5-10 ℃/min, and then to be sintered and molded for 1 hour under the pressure of 10-30 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210441983.7A CN114751760A (en) | 2022-04-25 | 2022-04-25 | Method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite material through nano-impregnation transient eutectic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210441983.7A CN114751760A (en) | 2022-04-25 | 2022-04-25 | Method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite material through nano-impregnation transient eutectic |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114751760A true CN114751760A (en) | 2022-07-15 |
Family
ID=82332522
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210441983.7A Pending CN114751760A (en) | 2022-04-25 | 2022-04-25 | Method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite material through nano-impregnation transient eutectic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114751760A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103103869A (en) * | 2012-12-28 | 2013-05-15 | 东华大学 | Method for preparing carbon fiber composite functional paper |
| CN103835181A (en) * | 2014-03-03 | 2014-06-04 | 浙江理工大学 | Preparation method of SiC nanofiber paper |
| CN109437957A (en) * | 2018-11-15 | 2019-03-08 | 广东工业大学 | A kind of ceramic connecting piece of connection method and the preparation of nm immersion transient state eutectic phase combination chemical vapor infiltration realization SiC ceramic |
| CN109437910A (en) * | 2018-11-15 | 2019-03-08 | 广东工业大学 | A kind of nm immersion transient state eutectic is connected the method for SiC ceramic and its ceramics of preparation and application |
| CN110256082A (en) * | 2019-05-17 | 2019-09-20 | 浙江理工大学 | Reaction-sintered prepares monocrystalline silicon carbide nanofiber/carbon/silicon carbide ceramic matrix composite method |
| CN111910467A (en) * | 2020-07-21 | 2020-11-10 | 中国科学院上海硅酸盐研究所 | Barium sulfate fiber inorganic refractory paper and preparation method and application thereof |
| CN113308935A (en) * | 2021-04-27 | 2021-08-27 | 浙江理工大学 | Preparation method of silicon carbide nanofiber refractory paper |
-
2022
- 2022-04-25 CN CN202210441983.7A patent/CN114751760A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103103869A (en) * | 2012-12-28 | 2013-05-15 | 东华大学 | Method for preparing carbon fiber composite functional paper |
| CN103835181A (en) * | 2014-03-03 | 2014-06-04 | 浙江理工大学 | Preparation method of SiC nanofiber paper |
| CN109437957A (en) * | 2018-11-15 | 2019-03-08 | 广东工业大学 | A kind of ceramic connecting piece of connection method and the preparation of nm immersion transient state eutectic phase combination chemical vapor infiltration realization SiC ceramic |
| CN109437910A (en) * | 2018-11-15 | 2019-03-08 | 广东工业大学 | A kind of nm immersion transient state eutectic is connected the method for SiC ceramic and its ceramics of preparation and application |
| CN110256082A (en) * | 2019-05-17 | 2019-09-20 | 浙江理工大学 | Reaction-sintered prepares monocrystalline silicon carbide nanofiber/carbon/silicon carbide ceramic matrix composite method |
| CN111910467A (en) * | 2020-07-21 | 2020-11-10 | 中国科学院上海硅酸盐研究所 | Barium sulfate fiber inorganic refractory paper and preparation method and application thereof |
| CN113308935A (en) * | 2021-04-27 | 2021-08-27 | 浙江理工大学 | Preparation method of silicon carbide nanofiber refractory paper |
Non-Patent Citations (3)
| Title |
|---|
| NAOFUMI NAKAZATO ET AL.: "《Appropriate thickness of pyrolytic carbon coating on SiC fiber reinforcement to secure reasonable quasi-ductility on NITE SiC/SiC composites》", 《CERAMICS INTERNATIONAL》, 30 November 2018 (2018-11-30), pages 19308 - 19309 * |
| 孙传尧等, 武汉大学出版社 * |
| 成来飞等: "《复合材料原理及工艺》", 西北工业大学出版社, pages: 122 - 123 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8039053B2 (en) | Method for making a part of composite material with ceramic matrix and resulting part | |
| KR100624094B1 (en) | The method of producing carbon fiber reinforced ceramic matrix composites | |
| JP3096716B1 (en) | Method for producing fiber-reinforced silicon carbide composite | |
| CN110256082B (en) | Method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite material by reaction sintering | |
| CN112341235B (en) | Multiphase coupling rapid densification method for ultrahigh-temperature self-healing ceramic matrix composite | |
| US8529995B2 (en) | Method for producing parts made of a thermostructural composite material | |
| CN113307643B (en) | SiC based on one-way belt f Preparation method of/SiC composite material | |
| CN108484173B (en) | SiCf/SiC composite material and preparation method thereof | |
| CN111217616B (en) | Preparation method of C/SiC structural material with near-zero expansion characteristic | |
| CN105016759A (en) | Rapid preparation method for C/SiC composite material | |
| CN104311090A (en) | Method for preparing Cf/ZrC-SiC superhigh-temperature ceramic composite material through hot-pressing sintering/precursor cracking process | |
| CN111170754B (en) | Composite material with Si-Y-C ternary ceramic matrix and preparation method thereof | |
| CN107311682A (en) | A kind of SiC nanowire enhancing Cf/SiC ceramic matric composites and preparation method thereof | |
| CN109608218B (en) | Self-healing ceramic matrix composite and low-temperature rapid preparation method thereof | |
| CN108101566A (en) | The method that RTM technique auxiliary prepares carbon/silicon carbide ceramic matrix composite component | |
| CN106495725A (en) | A kind of preparation method and application of carbon fibre carbonizing silicon nanowires Strengthening and Toughening ZrC SiC ceramic composite | |
| CN114988901A (en) | Rapid preparation method of high-density SiC/SiC composite material | |
| KR101101244B1 (en) | Method for manufacturing high density SiCf/SiC composites | |
| CN114716258A (en) | Preparation method of carbon fiber reinforced boron carbide composite material | |
| JP5168451B2 (en) | Method for producing porous molded body and method for producing porous filled molded body | |
| Zhang et al. | Preparation and characterization of lightweight SiC frameworks by connecting SiC fibers with SiC joints | |
| Zhang et al. | Fabrication and properties of three-dimensional braided carbon fiber reinforced SiOa-rich mullite composites | |
| CN114751760A (en) | Method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite material through nano-impregnation transient eutectic | |
| KR100829711B1 (en) | Fabrication method of high density silicon carbide fiber reinforced silicon carbide composite materials | |
| KR100838825B1 (en) | Sic fiber reinforced reaction bonded sic porous body and its fabrication process |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220715 |
|
| RJ01 | Rejection of invention patent application after publication |