CN112624766B - A kind of preparation method of silicon nitride@silicon carbide@boron nitride composite fiber felt - Google Patents
A kind of preparation method of silicon nitride@silicon carbide@boron nitride composite fiber felt Download PDFInfo
- Publication number
- CN112624766B CN112624766B CN202011602259.5A CN202011602259A CN112624766B CN 112624766 B CN112624766 B CN 112624766B CN 202011602259 A CN202011602259 A CN 202011602259A CN 112624766 B CN112624766 B CN 112624766B
- Authority
- CN
- China
- Prior art keywords
- silicon
- fiber felt
- reaction
- layer
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 85
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 57
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 49
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 17
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
- 238000011068 loading method Methods 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 44
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 44
- 229910052710 silicon Inorganic materials 0.000 claims description 39
- 239000010703 silicon Substances 0.000 claims description 38
- 238000010438 heat treatment Methods 0.000 claims description 30
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- 229910002804 graphite Inorganic materials 0.000 claims description 24
- 239000010439 graphite Substances 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 20
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 19
- 239000004917 carbon fiber Substances 0.000 claims description 19
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 19
- 238000005470 impregnation Methods 0.000 claims description 15
- 229910052796 boron Inorganic materials 0.000 claims description 14
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 9
- 239000007833 carbon precursor Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000011863 silicon-based powder Substances 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000012495 reaction gas Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229930006000 Sucrose Natural products 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 229910021538 borax Inorganic materials 0.000 claims description 2
- 125000005619 boric acid group Chemical group 0.000 claims description 2
- 229910052810 boron oxide Inorganic materials 0.000 claims description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 2
- 239000004328 sodium tetraborate Substances 0.000 claims description 2
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 12
- 239000002657 fibrous material Substances 0.000 abstract description 5
- 239000010410 layer Substances 0.000 description 50
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 7
- 239000012298 atmosphere Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005272 metallurgy Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910018540 Si C Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 229910003465 moissanite Inorganic materials 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001737 promoting 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
- C04B35/515—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
- C04B35/573—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 reaction sintering or recrystallisation
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
- C04B35/591—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained by reaction 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
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62272—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on non-oxide ceramics
- C04B35/62277—Fibres based on carbides
- C04B35/62281—Fibres based on carbides based on 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
- 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
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62272—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on non-oxide ceramics
- C04B35/62286—Fibres based on nitrides
- C04B35/6229—Fibres based on nitrides based on boron nitride
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62272—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on non-oxide ceramics
- C04B35/62286—Fibres based on nitrides
- C04B35/62295—Fibres based on nitrides based on silicon nitride
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/10—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
-
- 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
-
- 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
- C04B2235/6565—Cooling rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Textile Engineering (AREA)
- Ceramic Products (AREA)
Abstract
一种氮化硅@碳化硅@氮化硼复合纤维毡的制备方法，它涉及一种复合纤维毡的制备方法。本发明要解决现有陶瓷纤维材料使用温度低于1200℃的问题。制备方法：一、Si3N4纤维毡的制备；二、包裹碳层；三、Si3N4@SiC纤维毡的制备；四、BN层的负载。本发明用于氮化硅@碳化硅@氮化硼复合纤维毡的制备。
A preparation method of a silicon nitride@silicon carbide@boron nitride composite fiber felt relates to a preparation method of a composite fiber felt. The invention aims to solve the problem that the use temperature of the existing ceramic fiber material is lower than 1200°C. Preparation methods: 1. Preparation of Si 3 N 4 fiber mat; 2. Wrapping carbon layer; 3. Preparation of Si 3 N 4 @SiC fiber mat; 4. Loading of BN layer. The invention is used for the preparation of silicon nitride@silicon carbide@boron nitride composite fiber felt.
Description
Technical Field
The invention relates to a preparation method of a composite fiber felt.
Background
The ceramic fiber felt is used as a light and flexible refractory fiber heat insulation material commonly used at present, has excellent heat insulation performance, and plays an important role in promoting rapid development in the fields of aviation, aerospace, metallurgy, chemical industry, energy and the like. High temperature resistant ceramic fiber materials are considered to be the most promising materials for use in harsh high temperature environments. The service temperature of the ceramic fiber in the international market under the aerobic environment is generally lower than 1200 ℃, and in order to meet the development requirement of future equipment, the development of a novel high-temperature resistant ceramic fiber material is urgently needed. Currently, SiC and Si are commonly used in ultra-high temperature environments3N4Ceramic fiber, wherein the service temperature of the two ceramic materials under the air atmosphere is not higher than 1200 ℃. The service temperature of the ceramic fiber in the international market under the aerobic environment is generally lower than 1200 ℃, and in order to meet the development requirement of future equipment, the development of novel high-temperature resistant ceramic fiber is urgently neededAnd (5) a fiber material.
Disclosure of Invention
The invention provides a preparation method of a silicon nitride @ silicon carbide @ boron nitride composite fiber felt, aiming at solving the problem that the use temperature of the existing ceramic fiber material is lower than 1200 ℃.
A preparation method of a silicon nitride @ silicon carbide @ boron nitride composite fiber felt is completed according to the following steps:
mono, Si3N4Preparing a fiber felt:
laying reaction silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, then covering a carbon fiber felt on the surface of the reaction silicon source layer, putting the graphite crucible which is not covered with a graphite crucible cover and contains reactants into a tubular furnace, introducing nitrogen as reaction gas at the flow rate of 60-160 mL/min, heating to 1500-1700 ℃ at the heating rate of 1-10 ℃/min, carrying out sintering reaction for 90-240 min at the reaction temperature of 1500-1700 ℃, and naturally cooling to room temperature after the reaction is finished to obtain Si3N4A fiber mat;
the mass ratio of the reaction silicon source powder to the carbon fiber felt is 1 (1-8);
secondly, coating a carbon layer:
mixing Si3N4Soaking the fiber felt in a carbon precursor solution for 12-48 h, drying to obtain a soaked felt, placing the soaked felt in a tubular furnace, heating to 600-1000 ℃ at a heating rate of 5-10 ℃/min under the protection of nitrogen, preserving the heat for 120-480 min at the temperature of 600-1000 ℃, then reducing the temperature to 300-500 ℃ at a cooling rate of 5-10 ℃/min, and naturally cooling along with the furnace to obtain Si coating the C layer3N4A fiber mat;
the concentration of the carbon precursor solution is 0.5-2 mol/L;
III, Si3N4Preparation of @ SiC fiber felt:
laying silicon source powder at the bottom of a graphite crucible to obtain a silicon source layer, and then wrapping Si of the C layer3N4Fiber feltCovering the surface of the silicon source layer, covering a graphite crucible cover, putting the graphite crucible containing reactants into a tube furnace, heating to 1400-1700 ℃ at the heating rate of 1-2.5 ℃/min by taking argon as protective gas, carrying out sintering reaction for 120-360 min at the reaction temperature of 1400-1700 ℃, and naturally cooling to room temperature after the reaction is finished to obtain Si3N4@ SiC fiber felt;
the silicon source powder and Si coating the C layer3N4The mass ratio of the fiber felt is 1 (1-6);
fourthly, loading of the BN layer:
dissolving boron source and nitrogen source in methanol/deionized water solution to obtain impregnation solution, and adding Si3N4Soaking the @ SiC fibrofelt in the impregnation liquid, performing ultrasonic treatment for 0.5 to 5 hours under the condition that the power is 35 to 50W, performing drying treatment after ultrasonic treatment, then placing the fibrofelt in a tubular furnace, heating the fibrofelt to 1500 to 1800 ℃ at the heating rate of 5 to 10 ℃/min under the nitrogen atmosphere, preserving the heat for 2 to 6 hours under the temperature of 1500 to 1800 ℃, and cooling the fibrofelt along with the furnace to obtain the Si3N4@ SiC @ BN composite fiber felt;
the concentration of the boron source in the dipping solution is 0.1-2 mol/L; the concentration of the nitrogen source in the impregnation liquid is 0.1-1 mol/L; the mass percentage of the methanol in the impregnation liquid is 5-20%.
The invention has the beneficial effects that:
the invention develops Si with strong operability and wide industrialization prospect3N4A preparation method of the @ SiC @ BN composite fiber felt is characterized in that a silicon carbide layer is wrapped on the surface of the composite fiber felt by a method of generating silicon nitride fibers on the basis of an original template carbon fiber felt and then carrying out further carbon thermal reduction of a loaded carbon source, and finally, a BN layer is wrapped. BN, SiC, Si3N4The layers are respectively wrapped layer by layer, and the synergistic effect of the unique structure plays a critical role in high-temperature stability. This microstructural characteristic allows the multicomponent composite fiber mat to maintain ultra-high temperature stability. This structural design can maintain the stability of the multi-element ceramic fiber from three aspects: aerobic atmosphereSi unstable under3N4The fiber is positioned at the innermost layer of the gradient fiber and is shielded and blocked by three elements at the outer layer on the atomic scale; the element B is positioned on the outer surface layer, so that high-temperature stability is facilitated; and the Si-C bond formed by the mutual bonding of the intermediate layers on the atomic scale is used as a transition layer due to the unique heat conduction performance of the intermediate layers.
The method is simple, and each component of the obtained fiber felt is tightly combined. Si prepared by the invention3N4The heat conductivity of the @ SiC @ BN composite fiber felt is only 0.09W/m.K at normal temperature, the temperature is increased to 1600 ℃ in high-purity air, the quality is not reduced, and the high-temperature stability is good. The Si is3N4The @ SiC @ BN composite fiber felt has good high-temperature-resistant heat-insulating property and good application prospect in the high-temperature application fields of aviation, aerospace, metallurgy, chemical industry and the like.
The invention relates to a preparation method of a silicon nitride @ silicon carbide @ boron nitride composite fiber felt.
Drawings
FIG. 1 shows Si prepared in one step three of the example3N4A microstructure diagram of the @ SiC fibrofelt;
FIG. 2 shows Si prepared in example one3N4A micro-topography of the @ SiC @ BN composite fiber felt;
FIG. 3 is a chart of EDS elements for region A of FIG. 2;
FIG. 4 shows Si prepared in example one3N4High temperature thermal weight loss curve of @ SiC @ BN fibrofelt.
Detailed Description
The first embodiment is as follows: the embodiment of the invention relates to a preparation method of a silicon nitride @ silicon carbide @ boron nitride composite fiber felt, which is completed according to the following steps:
mono, Si3N4Preparing a fiber felt:
laying reaction silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, then covering a carbon fiber felt on the surface of the reaction silicon source layer, putting the graphite crucible which is not covered with a graphite crucible cover and contains reactants into a tubular furnace, introducing nitrogen as reaction gas at the flow rate of 60-160 mL/min, and raising the pressure of the reaction gasHeating to 1500-1700 ℃ at a temperature rate of 1-10 ℃/min, carrying out sintering reaction for 90-240 min at a reaction temperature of 1500-1700 ℃, and naturally cooling to room temperature after the reaction is finished to obtain Si3N4A fiber mat;
the mass ratio of the reaction silicon source powder to the carbon fiber felt is 1 (1-8);
secondly, coating a carbon layer:
mixing Si3N4Soaking the fiber felt in a carbon precursor solution for 12-48 h, drying to obtain a soaked felt, placing the soaked felt in a tubular furnace, heating to 600-1000 ℃ at a heating rate of 5-10 ℃/min under the protection of nitrogen, preserving the heat for 120-480 min at the temperature of 600-1000 ℃, then reducing the temperature to 300-500 ℃ at a cooling rate of 5-10 ℃/min, and naturally cooling along with the furnace to obtain Si coating the C layer3N4A fiber mat;
the concentration of the carbon precursor solution is 0.5-2 mol/L;
III, Si3N4Preparation of @ SiC fiber felt:
laying silicon source powder at the bottom of a graphite crucible to obtain a silicon source layer, and then wrapping Si of the C layer3N4Covering a fibrofelt on the surface of the silicon source layer, covering a graphite crucible cover, putting the graphite crucible containing reactants into a tubular furnace, heating to 1400-1700 ℃ at the heating rate of 1-2.5 ℃/min by taking argon as protective gas, carrying out sintering reaction for 120-360 min at the reaction temperature of 1400-1700 ℃, and naturally cooling to room temperature after the reaction is finished to obtain Si3N4@ SiC fiber felt;
the silicon source powder and Si coating the C layer3N4The mass ratio of the fiber felt is 1 (1-6);
fourthly, loading of the BN layer:
dissolving boron source and nitrogen source in methanol/deionized water solution to obtain impregnation solution, and adding Si3N4The @ SiC fiber felt is immersed in the immersion liquid, under the condition that the power is 35W-50W,ultrasonic treatment for 0.5-5 h, drying after ultrasonic treatment, then placing in a tube furnace, heating to 1500-1800 ℃ at a heating rate of 5-10 ℃/min in a nitrogen atmosphere, keeping the temperature at 1500-1800 ℃ for 2-6 h, and furnace cooling to obtain Si3N4@ SiC @ BN composite fiber felt;
the concentration of the boron source in the dipping solution is 0.1-2 mol/L; the concentration of the nitrogen source in the impregnation liquid is 0.1-1 mol/L; the mass percentage of the methanol in the impregnation liquid is 5-20%.
The beneficial effects of the embodiment are as follows:
the embodiment develops the Si with strong operability and wide industrialization prospect3N4A preparation method of the @ SiC @ BN composite fiber felt is characterized in that a silicon carbide layer is wrapped on the surface of the composite fiber felt by a method of generating silicon nitride fibers on the basis of an original template carbon fiber felt and then carrying out further carbon thermal reduction of a loaded carbon source, and finally, a BN layer is wrapped. BN, SiC, Si3N4The layers are respectively wrapped layer by layer, and the synergistic effect of the unique structure plays a critical role in high-temperature stability. This microstructural characteristic allows the multicomponent composite fiber mat to maintain ultra-high temperature stability. This structural design can maintain the stability of the multi-element ceramic fiber from three aspects: [ unstable Si in oxygen atmosphere3N4The fiber is positioned at the innermost layer of the gradient fiber and is shielded and blocked by three elements at the outer layer on the atomic scale; the element B is positioned on the outer surface layer, so that high-temperature stability is facilitated; and the Si-C bond formed by the mutual bonding of the intermediate layers on the atomic scale is used as a transition layer due to the unique heat conduction performance of the intermediate layers.
The method of the embodiment is simple, and each component of the obtained fiber felt is tightly combined. Si prepared in the present embodiment3N4The heat conductivity of the @ SiC @ BN composite fiber felt is only 0.09W/m.K at normal temperature, the temperature is increased to 1600 ℃ in high-purity air, the quality is not reduced, and the high-temperature stability is good. The Si is3N4The @ SiC @ BN composite fiber felt has good high-temperature-resistant heat-insulating property and good high-temperature application fields of aviation, aerospace, metallurgy, chemical industry and the likeThe application prospect of (1).
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the carbon fiber felt in the step one is 400g/m of unit mass2～1000g/m2The carbon fiber felt of (1); the thickness of the carbon fiber felt in the step one is 3 mm-10 mm. The rest is the same as the first embodiment.
The third concrete implementation mode: this embodiment is different from the first or second embodiment in that: the reaction silicon source powder in the first step is a mixture of silicon dioxide powder and silicon powder in a molar ratio of 1 (1-6). The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the drying in the second step is drying for 6 to 12 hours under the condition that the treatment temperature is 60 to 160 ℃. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: and the precursor solution in the second step is sucrose solution, glucose solution, starch solution, polyacrylonitrile solution or phenolic resin solution. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: and the silicon source powder in the third step is a mixture of silicon dioxide powder and silicon powder in a molar ratio of 1 (1-6). The rest is the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the drying treatment in the fourth step is drying for 6 to 12 hours at the treatment temperature of 60 to 160 ℃. The others are the same as the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: the concentration of the boron source in the impregnating solution in the fourth step is 1 mol/L-2 mol/L; the concentration of the nitrogen source in the steeping liquor in the fourth step is 0.5-1 mol/L; the mass percent of the methanol in the steeping liquor in the fourth step is 10-20%. The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: the boron source in the fourth step is boric acid, boron oxide or borax. The other points are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: the nitrogen source in the fourth step is urea, ammonium nitrate or melamine. The other points are the same as those in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
a preparation method of a silicon nitride @ silicon carbide @ boron nitride composite fiber felt is completed according to the following steps:
mono, Si3N4Preparing a fiber felt:
laying reaction silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, then covering a carbon fiber felt on the surface of the reaction silicon source layer, putting the graphite crucible which is not covered with a graphite crucible cover and contains reactants into a tubular furnace, introducing nitrogen as reaction gas at the flow rate of 60mL/min, heating to 1500 ℃ at the heating rate of 2.5 ℃/min, carrying out sintering reaction for 2h under the condition that the reaction temperature is 1500 ℃, naturally cooling to room temperature after the reaction is finished to obtain Si3N4A fiber mat;
the mass ratio of the reaction silicon source powder to the carbon fiber felt is 1: 4;
secondly, coating a carbon layer:
mixing Si3N4Soaking the fiber felt in a carbon precursor solution for 24h, drying to obtain a soaked felt, placing the soaked felt in a tubular furnace, heating to 800 ℃ at a heating rate of 5 ℃/min under the protection of nitrogen, keeping the temperature for 120min at the temperature of 800 ℃, then cooling to 300 ℃ at a cooling rate of 10 ℃/min, and naturally cooling with the furnace to obtain Si coated with the C layer3N4A fiber mat;
the concentration of the carbon precursor solution is 1 mol/L;
III, Si3N4Preparation of @ SiC fiber felt:
laying silicon source powder at the bottom of a graphite crucible to obtain a silicon source layer, and then wrapping Si of the C layer3N4Covering a fibrofelt on the surface of the silicon source layer, covering a graphite crucible cover, putting the graphite crucible containing reactants into a tubular furnace, heating to 1500 ℃ at the heating rate of 2.5 ℃/min by taking argon as protective gas, sintering and reacting for 120min at the reaction temperature of 1500 ℃, and naturally cooling to room temperature after the reaction is finished to obtain Si3N4@ SiC fiber felt;
the silicon source powder and Si coating the C layer3N4The mass ratio of the fiber felt is 1: 1;
fourthly, loading of the BN layer:
dissolving boron source and nitrogen source in methanol/deionized water solution to obtain impregnation solution, and adding Si3N4Soaking the @ SiC fibrofelt in the impregnation liquid, carrying out ultrasonic treatment for 0.5h under the condition that the power is 35W, carrying out drying treatment after ultrasonic treatment, then placing the fibrofelt in a tube furnace, heating the fibrofelt to 1600 ℃ under the nitrogen atmosphere at the heating rate of 5 ℃/min, keeping the temperature for 3h under the condition that the temperature is 1600 ℃, and carrying out furnace cooling to obtain the Si-based composite material3N4@ SiC @ BN composite fiber felt;
the concentration of the boron source in the impregnating solution is 1 mol/L; the concentration of the nitrogen source in the impregnation liquid is 1 mol/L; the mass percentage of the methanol in the impregnation liquid is 10%.
The unit mass of the carbon fiber felt in the step one is 750g/m2The carbon fiber felt of (1). The thickness of the carbon fiber felt in the step one is 5 mm.
The reaction silicon source powder in the first step is a mixture of silicon dioxide powder and silicon powder in a molar ratio of 1: 1.
The purity of the nitrogen in the first step is 99.99%.
The drying in the second step is drying for 10 hours under the condition that the treatment temperature is 80 ℃.
And the precursor solution in the second step is a sucrose solution.
The silicon source powder in the third step is a mixture of silicon dioxide powder and silicon powder with a molar ratio of 1: 1.
The purity of the argon in the third step is 99.99 percent.
The drying treatment in the fourth step is drying for 8 hours at the treatment temperature of 85 ℃.
The boron source in step four is boric acid.
The nitrogen source in the fourth step is urea.
FIG. 1 shows Si prepared in one step three of the example3N4A microstructure diagram of the @ SiC fibrofelt; as can be seen, the surface of the prepared silicon nitride fiber is successfully wrapped with a silicon carbide layer, and the thickness of the silicon carbide layer is about 2 microns.
FIG. 2 shows Si prepared in example one3N4A micro-topography of the @ SiC @ BN composite fiber felt; as can be seen from the figure, a layer of BN layered structure is loaded after the boron source is dipped and the high-temperature sintering reaction is carried out under the nitrogen, and the thickness is 1 micron.
FIG. 3 is a chart of EDS elements for region A of FIG. 2; as can be seen from the figure, the side surface of the prepared fiber felt with four elements of Si, B, C and N shows that the Si is present3N4And (3) preparing the @ SiC @ BN composite fiber felt.
Si prepared for example one3N4The thermal conductivity of the @ SiC @ BN composite fiber felt is tested, and the thermal conductivity of the composite fiber felt is only 0.09W/m.K at normal temperature. The thermal conductivity is significantly lower than that of a large number of porous ceramic structures, and is a candidate for an excellent heat-proof and heat-insulating material.
FIG. 4 shows Si prepared in example one3N4According to the high-temperature thermal weight loss curve of the @ SiC @ BN fibrofelt, the test atmosphere is high-purity air, the quality is not reduced when the temperature is increased to 1600 ℃, and the high-temperature stability is better.
Claims (9)
1. A preparation method of a silicon nitride @ silicon carbide @ boron nitride composite fiber felt is characterized by comprising the following steps:
mono, Si3N4Preparing a fiber felt:
laying reaction silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, then covering a carbon fiber felt on the surface of the reaction silicon source layer, putting the graphite crucible which is not covered with a graphite crucible cover and contains reactants into a tubular furnace, introducing nitrogen as reaction gas at the flow rate of 60-160 mL/min, heating to 1500-1700 ℃ at the heating rate of 1-10 ℃/min, carrying out sintering reaction for 90-240 min at the reaction temperature of 1500-1700 ℃, and naturally cooling to room temperature after the reaction is finished to obtain Si3N4A fiber mat;
the mass ratio of the reaction silicon source powder to the carbon fiber felt is 1 (1-8);
secondly, coating a carbon layer:
mixing Si3N4Soaking the fiber felt in a carbon precursor solution for 12-48 h, drying to obtain a soaked felt, placing the soaked felt in a tubular furnace, heating to 600-1000 ℃ at a heating rate of 5-10 ℃/min under the protection of nitrogen, preserving the heat for 120-480 min at the temperature of 600-1000 ℃, then reducing the temperature to 300-500 ℃ at a cooling rate of 5-10 ℃/min, and naturally cooling along with the furnace to obtain Si coating the C layer3N4A fiber mat;
the concentration of the carbon precursor solution is 0.5-2 mol/L;
III, Si3N4Preparation of @ SiC fiber felt:
laying silicon source powder at the bottom of a graphite crucible to obtain a silicon source layer, and then wrapping Si of the C layer3N4Covering a fibrofelt on the surface of the silicon source layer, covering a graphite crucible cover, putting the graphite crucible containing reactants into a tubular furnace, heating to 1400-1700 ℃ at the heating rate of 1-2.5 ℃/min by taking argon as protective gas, carrying out sintering reaction for 120-360 min at the reaction temperature of 1400-1700 ℃, and naturally cooling to room temperature after the reaction is finished to obtain Si3N4@ SiC fiber felt;
the silicon source powder and Si coating the C layer3N4The mass ratio of the fiber felt is 1:(1～6)；
Fourthly, loading of the BN layer:
dissolving boron source and nitrogen source in methanol/deionized water solution to obtain impregnation solution, and adding Si3N4Soaking the @ SiC fibrofelt in the impregnation liquid, performing ultrasonic treatment for 0.5 to 5 hours under the condition that the power is 35 to 50W, performing drying treatment after ultrasonic treatment, then placing the fibrofelt in a tubular furnace, heating the fibrofelt to 1500 to 1800 ℃ at the heating rate of 5 to 10 ℃/min under the nitrogen atmosphere, preserving the heat for 2 to 6 hours under the temperature of 1500 to 1800 ℃, and cooling the fibrofelt along with the furnace to obtain the Si3N4@ SiC @ BN composite fiber felt;
the concentration of the boron source in the impregnating solution is 1 mol/L; the concentration of the nitrogen source in the impregnation liquid is 1 mol/L; the mass percentage of the methanol in the impregnation liquid is 5-20%.
2. The method for preparing the silicon nitride @ silicon carbide @ boron nitride composite fiber felt according to claim 1, wherein the carbon fiber felt in the first step is 400g/m in unit mass2～1000g/m2The carbon fiber felt of (1); the thickness of the carbon fiber felt in the step one is 3 mm-10 mm.
3. The preparation method of the silicon nitride @ silicon carbide @ boron nitride composite fibrofelt according to claim 1, wherein the reaction silicon source powder in the first step is a mixture of silicon dioxide powder and silicon powder in a molar ratio of 1 (1-6).
4. The preparation method of the silicon nitride @ silicon carbide @ boron nitride composite fiber felt according to claim 1, wherein the drying in the second step is drying for 6 to 12 hours at a treatment temperature of 60 to 160 ℃.
5. The method for preparing the silicon nitride @ silicon carbide @ boron nitride composite fiber felt according to claim 1, wherein the precursor solution in the second step is a sucrose solution, a glucose solution, a starch solution, a polyacrylonitrile solution or a phenolic resin solution.
6. The preparation method of the silicon nitride @ silicon carbide @ boron nitride composite fibrofelt according to claim 1, wherein the silicon source powder in the third step is a mixture of silicon dioxide powder and silicon powder in a molar ratio of 1 (1-6).
7. The preparation method of the silicon nitride @ silicon carbide @ boron nitride composite fibrofelt according to claim 1, wherein the drying treatment in the fourth step is drying for 6 to 12 hours at a treatment temperature of 60 to 160 ℃.
8. The method of claim 1, wherein in step four said boron source is boric acid, boron oxide, or borax.
9. The preparation method of the silicon nitride @ silicon carbide @ boron nitride composite fiber felt according to claim 1, wherein the nitrogen source in the fourth step is urea, ammonium nitrate or melamine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011602259.5A CN112624766B (en) | 2020-12-29 | 2020-12-29 | A kind of preparation method of silicon nitride@silicon carbide@boron nitride composite fiber felt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011602259.5A CN112624766B (en) | 2020-12-29 | 2020-12-29 | A kind of preparation method of silicon nitride@silicon carbide@boron nitride composite fiber felt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112624766A CN112624766A (en) | 2021-04-09 |
| CN112624766B true CN112624766B (en) | 2021-11-16 |
Family
ID=75286971
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011602259.5A Active CN112624766B (en) | 2020-12-29 | 2020-12-29 | A kind of preparation method of silicon nitride@silicon carbide@boron nitride composite fiber felt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112624766B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112608156B (en) * | 2020-12-29 | 2021-12-03 | 内蒙古海特华材科技有限公司 | Preparation method of micro-nano mixed SiC chopped fibers |
| CN114890770B (en) * | 2022-05-31 | 2023-04-28 | 哈尔滨工业大学 | Preparation method of porous silicon carbide/carbon composite aerogel |
| CN117602951A (en) * | 2023-12-08 | 2024-02-27 | 湖南泽睿新材料有限公司 | A continuous preparation method of BN coating on SiC fiber surface |
| CN118026700A (en) * | 2023-12-29 | 2024-05-14 | 山东工业陶瓷研究设计院有限公司 | High-temperature-resistant creep-resistant ceramic material and preparation method thereof |
| CN118026715A (en) * | 2024-03-05 | 2024-05-14 | 中国科学院合肥物质科学研究院 | Carbon@silicon carbide nanofiber aerogel and its preparation method and application |
| CN118792772B (en) * | 2024-09-13 | 2025-01-07 | 天津工业大学 | Preparation method of continuous silicon nitride flexible belt with sheath-core structure |
| CN119551998A (en) * | 2025-01-24 | 2025-03-04 | 北京玻钢院复合材料有限公司 | A SiC-BN multiphase ceramic matrix composite material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005061401A2 (en) * | 2003-09-18 | 2005-07-07 | 3M Innovative Properties Company | CERAMICS AND GLASS COMPRISING Al2O3, REO, ZrO2 AND/OR HFO2, AND Nb2O5 AND/OR Ta2O5 AND/OR METHODS OF MAKING THE SAME |
| US20060236724A1 (en) * | 2000-07-31 | 2006-10-26 | Shin-Etsu Quartz Products Co., Ltd. | Mandrel for producing quartz glass and production method for optical fiber mother material, optical fiber and quartz glass body using the same |
| US20110315911A1 (en) * | 2007-03-16 | 2011-12-29 | Chemex Gmbh | Core-sheath particle for use as a filler for feeder masses |
| US20180370859A1 (en) * | 2015-12-21 | 2018-12-27 | Safran Ceramics | A method of fabricating a ceramic from a chemical reaction |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4908340A (en) * | 1987-07-16 | 1990-03-13 | The Standard Oil Company | Non-oxide sintered ceramic fibers |
| US5252361A (en) * | 1990-01-19 | 1993-10-12 | The Carborundum Company | Protective coating for non-oxide sintered fibers generated by in situ chemical reaction |
| DE19746598C2 (en) * | 1997-10-22 | 2000-12-07 | Dornier Gmbh | Ceramic composite and its use |
| CN104326750B (en) * | 2014-10-21 | 2016-01-20 | 山东理工大学 | A kind of preparation method of continuous nitride silica fibre |
| CN104557050B (en) * | 2014-12-20 | 2017-02-22 | 北京矿冶研究总院 | ZrB2-SiC/Si composite powder with core-shell structure and preparation method thereof |
| CN105502315B (en) * | 2016-01-28 | 2017-11-03 | 哈尔滨工业大学 | A kind of method that ex situ in situ grows overlength silicon nitride nano-material simultaneously |
| CN106495702B (en) * | 2016-10-14 | 2019-06-25 | 湖南工业大学 | It is a kind of to prepare carbon fiber/silicon nitride structure absorbing material process |
| CN106986666A (en) * | 2017-03-17 | 2017-07-28 | 昆明理工大学 | A kind of preparation method without sintering ceramics preparative composite material |
| CN109704778A (en) * | 2019-01-21 | 2019-05-03 | 武汉科技大学 | A kind of SiBCN ceramic and preparation method thereof |
| CN111441104B (en) * | 2020-03-10 | 2022-10-28 | 哈尔滨工业大学 | Method for preparing CSiNB quaternary fibers from carbon fibers |
-
2020
- 2020-12-29 CN CN202011602259.5A patent/CN112624766B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060236724A1 (en) * | 2000-07-31 | 2006-10-26 | Shin-Etsu Quartz Products Co., Ltd. | Mandrel for producing quartz glass and production method for optical fiber mother material, optical fiber and quartz glass body using the same |
| WO2005061401A2 (en) * | 2003-09-18 | 2005-07-07 | 3M Innovative Properties Company | CERAMICS AND GLASS COMPRISING Al2O3, REO, ZrO2 AND/OR HFO2, AND Nb2O5 AND/OR Ta2O5 AND/OR METHODS OF MAKING THE SAME |
| US20110315911A1 (en) * | 2007-03-16 | 2011-12-29 | Chemex Gmbh | Core-sheath particle for use as a filler for feeder masses |
| US20180370859A1 (en) * | 2015-12-21 | 2018-12-27 | Safran Ceramics | A method of fabricating a ceramic from a chemical reaction |
Non-Patent Citations (3)
| Title |
|---|
| "Subsurface oxidation of boron nitride coatings on silicon carbide fibers in SiC/SiC ceramic matrix composites";Bradley L. Wing et al;《Ceramics International》;20180627;第17499-17505页 * |
| "Tensile properties and microstructural characterization of Hi-Nicalon SiC/RBSN composites";Ramakrishna T. Bhatt;《Ceramics International》;20000713;第535-539页 * |
| "碳化硅陶瓷基复合材料界面层技术研究进展";杨金华等;《航空制造技术》;20180815;第61卷(第11期);第79-87页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112624766A (en) | 2021-04-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112624766B (en) | A kind of preparation method of silicon nitride@silicon carbide@boron nitride composite fiber felt | |
| CN102276279B (en) | Preparation method of silicon carbide fiber reinforced silicon carbide composite material | |
| Ma et al. | Fabrication and oxidation resistance of mullite/yttrium silicate multilayer coatings on C/SiC composites | |
| CN114988906B (en) | Continuous fiber reinforced alumina ceramic matrix composite and preparation method thereof | |
| CN100564320C (en) | With charcoal nanofiber method of strengthening coal | |
| JP4014254B2 (en) | Si concentration step-variable Si-SiC material, Si concentration step change-type SiC fiber reinforced Si-SiC composite material, and production method thereof | |
| CN111454071B (en) | Rock wool fiber reinforced silica-based high-strength heat insulation composite material and preparation method thereof | |
| CN109053207A (en) | A kind of modified silicon carbide fiber reinforced silicon carbide composite material and preparation method of yttrium silicate | |
| CN104860695B (en) | Three-dimensional fiber prefabricated component strengthens mullite composite material and preparation method thereof | |
| CN110357635A (en) | A method of improving carbon-based or ceramic matric composite surface oxidation-resistant coating bond strength | |
| CN107141005B (en) | Silicon nitride fiber reinforced silica and boron nitride ceramic matrix composite material and its preparation method and application | |
| CN101863665A (en) | Preparation method of self-healing and anti-oxidation functional fiber reinforced ceramic matrix composites | |
| CN113666765B (en) | Continuous fiber reinforced high-entropy ceramic matrix composite and preparation method thereof | |
| JP2000327441A (en) | Composite carbonaceous thermal insulant and its production | |
| CN115124361B (en) | A kind of ceramic matrix composite material with hybrid structure and its preparation method | |
| CN111285699A (en) | A kind of lightweight and reusable anti-thermal insulation material and preparation method thereof | |
| CN109369187A (en) | A kind of preparation method of SiC nanowire reinforced C/C-SiC-ZrC ceramic matrix composites | |
| CN119059832B (en) | Aerogel heat insulation material with high mechanical strength and preparation method thereof | |
| CN107973612B (en) | A kind of PCS/LPVCS combination uses the method for preparing Cf/SiC composite material | |
| CN108530104A (en) | PIP combinations growth in situ graphene/boron nitride nano-tube ceramic matric composite densifying method | |
| Zhang et al. | Investigation of in-situ microstructural mechanical properties and thermal damage mechanisms of SiCf/SiC under CVI and PIP processes | |
| CN114751760A (en) | A method for preparing single crystal silicon carbide nanofiber/silicon carbide ceramic matrix composite material by nano-impregnation transient eutectic | |
| CN106507785B (en) | The preparation method of carbon/carbon-silicon carbide brake material | |
| Zeng et al. | Improved oxidation and thermal shock resistance of SiC-Si coating with a SiCw/PyC network structure toughened buffer layer | |
| CN112707741B (en) | A kind of preparation method of CSiNB-based multi-component integrated fiber felt material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |