CN112457034A - Preparation method of C/SiC composite material with vibrissa-nostril-like structure - Google Patents
Preparation method of C/SiC composite material with vibrissa-nostril-like structure Download PDFInfo
- Publication number
- CN112457034A CN112457034A CN202011243124.4A CN202011243124A CN112457034A CN 112457034 A CN112457034 A CN 112457034A CN 202011243124 A CN202011243124 A CN 202011243124A CN 112457034 A CN112457034 A CN 112457034A
- Authority
- CN
- China
- Prior art keywords
- starch
- composite material
- vibrissa
- sol
- nostril
- 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
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229920002472 Starch Polymers 0.000 claims abstract description 32
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 29
- 239000008107 starch Substances 0.000 claims abstract description 28
- 235000019698 starch Nutrition 0.000 claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 26
- 239000006260 foam Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000011148 porous material Substances 0.000 claims abstract description 11
- SICLLPHPVFCNTJ-UHFFFAOYSA-N 1,1,1',1'-tetramethyl-3,3'-spirobi[2h-indene]-5,5'-diol Chemical compound C12=CC(O)=CC=C2C(C)(C)CC11C2=CC(O)=CC=C2C(C)(C)C1 SICLLPHPVFCNTJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 9
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 9
- 239000004088 foaming agent Substances 0.000 claims abstract description 9
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 9
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 8
- 238000005187 foaming Methods 0.000 claims abstract description 6
- 230000005855 radiation Effects 0.000 claims abstract description 5
- 238000006722 reduction reaction Methods 0.000 claims abstract description 5
- 238000003763 carbonization Methods 0.000 claims abstract description 4
- 238000011065 in-situ storage Methods 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 13
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 240000004808 Saccharomyces cerevisiae Species 0.000 claims description 5
- 240000006394 Sorghum bicolor Species 0.000 claims description 4
- 235000011684 Sorghum saccharatum Nutrition 0.000 claims description 4
- 238000010000 carbonizing Methods 0.000 claims description 4
- 229920002401 polyacrylamide Polymers 0.000 claims description 4
- 229940100445 wheat starch Drugs 0.000 claims description 4
- QBKSIHCSDPPLJI-UHFFFAOYSA-N 2-[bis(2-hydroxyethyl)amino]tetradecan-1-ol;sulfuric acid Chemical compound OS(O)(=O)=O.CCCCCCCCCCCCC(CO)N(CCO)CCO QBKSIHCSDPPLJI-UHFFFAOYSA-N 0.000 claims description 3
- 229920002261 Corn starch Polymers 0.000 claims description 3
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 3
- 239000008120 corn starch Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 3
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 claims description 2
- 102000002322 Egg Proteins Human genes 0.000 claims description 2
- 108010000912 Egg Proteins Proteins 0.000 claims description 2
- 244000017020 Ipomoea batatas Species 0.000 claims description 2
- 235000002678 Ipomoea batatas Nutrition 0.000 claims description 2
- 235000014680 Saccharomyces cerevisiae Nutrition 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 235000014103 egg white Nutrition 0.000 claims description 2
- 210000000969 egg white Anatomy 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229920001592 potato starch Polymers 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 claims description 2
- 239000000969 carrier Substances 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000000428 dust Substances 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 230000009970 fire resistant effect Effects 0.000 abstract 1
- 239000006261 foam material Substances 0.000 abstract 1
- 239000011810 insulating material Substances 0.000 abstract 1
- 239000000779 smoke Substances 0.000 abstract 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 238000009413 insulation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- JZKFHQMONDVVNF-UHFFFAOYSA-N dodecyl sulfate;tris(2-hydroxyethyl)azanium Chemical compound OCCN(CCO)CCO.CCCCCCCCCCCCOS(O)(=O)=O JZKFHQMONDVVNF-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 210000003135 vibrissae Anatomy 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- 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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—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
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
- C04B2235/5244—Silicon carbide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/94—Products characterised by their shape
-
- 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
-
- 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)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Silicon Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention provides a C/SiC composite material with a vibrissa-nostril-like structure and a preparation method thereof. The preparation method is to use starch and SiO2The preparation method comprises the following steps of (1) taking water as a solvent, adding a dispersing agent and a foaming agent, and forming silicon dioxide-containing foam carbon by carrying out sol, foaming, gel curing and carbonization on starch; after in-situ high-temperature carbon thermal reduction reaction, a large number of SiC nanowires grow in the pores of the foam carbon, and the generation of the SiC nanowires modifies the pore structure of the foam C, limits convection and radiation heat transfer, and obviously reduces the thermal conductivity of the material. The material has the heat-insulating property of a foam material and the high-temperature resistance of C and SiC materials, and is an excellent high-temperature fire-resistant heat-insulating material. In addition, the material also has application prospects in the fields of catalyst carriers, smoke dust filtration and the like.
Description
Technical Field
The invention belongs to the field of porous materials, and particularly relates to a preparation method of a C/SiC composite material with a vibrissa-nostril-like structure.
Background
Foam carbon (foam carbon) refers to a foamed porous carbon material. Carbon foam is a lightweight porous material with a three-dimensional network structure composed of cells and interconnected cell walls. Besides the conventional properties of carbon materials, the carbon foam has the characteristics of small density, high strength, thermal shock resistance, easiness in processing and the like, and good physical and chemical properties of wave absorption and the like, and the excellent properties enable the carbon foam to be applied to various technical fields of chemical industry, aerospace, electronics and the like.
The foam carbon has the high-temperature stability of the C material and the heat insulation performance of the light material. It is a potential high-temperature thermal insulation material for aviation. However, most of the carbon foams are made of organic substances through high-temperature foaming and carbonization, and the materials obtained by the method have large pores (mostly micron-sized or more), and the pores can provide channels for convection and radiation heat transfer at high temperature, so that the thermal conductivity of the materials is obviously increased along with the temperature rise, and the high-temperature heat insulation performance of the materials is not good and does not reach the expected level of people.
Disclosure of Invention
In order to solve the problem of poor high-temperature heat insulation performance of carbon foam, the invention aims to provide a preparation method of a C/SiC composite material with a vibrissa-like nostril structure.
The invention adopts the following technical scheme for achieving the purpose:
a C/SiC composite material with the structure similar to nasal hair and nostril is prepared from starch and SiO2Is prepared from water as solvent, disperser and waterThe foaming agent is prepared by forming silicon dioxide-containing foam carbon by carrying out sol, foaming, gel curing and carbonization on starch; after in-situ high-temperature carbon thermal reduction reaction, a large number of SiC nanowires grow in air holes of foam carbon, the generation of the SiC nanowires modifies the pore structure of the foam C, limits convection and radiation heat transfer, and obviously reduces the thermal conductivity of the material, and the specific steps are as follows:
1) preparing a silicon-containing starch sol:
putting starch, silicon dioxide, water and a dispersing agent into a planetary ball mill according to a certain proportion, and ball-milling and uniformly mixing to obtain stable silicon dioxide-containing starch sol;
2) a foaming step:
adding a foaming agent into the silica-containing starch sol obtained in the step 1), stirring for 20min by using a stirrer, and standing for 2 h at the temperature of 30-45 ℃ to obtain porous sol;
3) and (3) gel curing:
heating the porous sol obtained in the step 2) in a water bath at 80-100 ℃, preserving heat for 40 min, and drying at 110 ℃ to constant weight to obtain porous gel;
4) and (3) carbonizing:
carbonizing the porous gel obtained in the step 3) to constant weight at 600 ℃ under the protection of nitrogen or argon to obtain silicon dioxide-containing foamy carbon;
5) a carbothermic reduction reaction step:
and (3) heating the foam carbon containing the silicon dioxide obtained in the step (4) to 1550-1850 ℃ at a heating rate of 10-15 ℃/min under the protection of argon, preserving heat at 1500-1800 ℃ for 3-10 h, and cooling along with a furnace to obtain the C/SiC composite material with the vibrissa-nostril structure.
The starch in the step 1) is one or more of wheat starch, corn starch, sweet potato starch, sorghum starch and the like.
The dispersant in the step 1) is one or more of polyacrylamide, CAMTMENT FS20 and tetramethylethylenediamine.
The foaming agent in the step 2) is one or more of lauryl triethanolamine sulfate, yeast, egg white, baking soda and the like.
The mass ratio of the starch to the silicon dioxide to the foaming agent to the water to the dispersing agent is 100: 5-15: 0.5-10: 80-130: 0.02-1.
The preparation method of the C/SiC composite material with the vibrissa-nostril-like structure, which is disclosed by the invention, has the following characteristics by adopting the technical scheme:
1. the material prepared by the method can resist the high temperature of 2000 ℃; the melting point or decomposition temperature of C and SiC in the composite material is more than 2300 ℃, and the obtained composite material can be used at higher temperature
2. The material has excellent high-temperature heat-insulating property. According to the method, the SiC nanowires with high purity and small diameter (< 150 nm) and large length (>100 microns) are obtained through carbon thermal in-situ reaction, the nanowires modify the pore structure performance of the foam carbon, the composite material has a nanometer pore structure, convection and radiation heat transfer of the foam carbon are effectively reduced, and the material has low high-temperature heat conductivity.
3. The method uses starch and SiO2The raw materials are green and cheap, and the preparation process is simple.
Drawings
FIG. 1 is a scanning electron micrograph of the C/SiC composite material prepared in example 1 of the process of the present invention.
FIG. 2 is a scanning electron micrograph of SiC nanowires in the foam gas of the composite material prepared in example 1 of the method of the present invention.
Detailed description of the preferred embodiments
The invention is described with reference to the accompanying drawings and specific examples:
example 1: putting 100 parts of wheat starch, 9 parts of silicon dioxide, 105 parts of water and 0.5 part of polyacrylamide into a planetary ball mill, and ball-milling for 2 hours at the speed of 30 r/min to obtain the product containing SiO2The starch sol of (a); adding 1 part of yeast into the sol, stirring for 20min at the speed of 800 r/min, and preserving heat for 2 h at 35 ℃ to obtain porous sol; putting the porous sol into a water bath, keeping the temperature at 100 ℃ for 40 min, taking out a sample, putting the sample into an oven, and drying the sample at 110 ℃ to constant weight to obtain porous gel; keeping the temperature of 600 ℃ in a nitrogen atmosphere until the weight is constant to obtain porous carbon; under the condition of argon protection, the method comprises the following steps of,raising the temperature to 1530 ℃ at the heating rate of 15 ℃/min, keeping the temperature for 10 h, and cooling along with the furnace, wherein the properties of the prepared C/SiC composite material with the vibrissa-nostril-like structure are shown in the table 1, the microstructure photo of the composite material is shown in the table 1, and the microstructure photo of the SiC nanowires in the foam carbon pores is shown in the table 2.
Example 2: putting 100 parts of sorghum starch, 10 parts of silicon dioxide, 90 parts of water and 0.1 part of tetramethylethylenediamine into a planetary ball mill for ball milling for 2 hours at a speed of 30 r/min to obtain the product containing SiO2The starch sol of (a); adding 1 part of yeast into the sol, stirring for 20min at the speed of 800 r/min, and preserving heat for 2 h at 35 ℃ to obtain porous sol; putting the porous sol into a water bath, keeping the temperature at 95 ℃ for 40 min, taking out a sample, putting the sample into an oven, and drying the sample at 110 ℃ to constant weight to obtain porous gel; keeping the temperature at 600 ℃ in a nitrogen atmosphere until the weight is constant to obtain porous carbon; and under the protection of argon, heating to 1600 ℃ at a heating rate of 14 ℃/min, preserving the heat for 4 h, and cooling along with the furnace to obtain the C/SiC composite material with the vibrissa-nostril structure.
Example 3: putting 100 parts of corn starch, 11 parts of silicon dioxide, 85 parts of water and 0.05 part of CAMTMENT FS20 into a planetary ball mill, and ball-milling for 2 hours at 30 r/min to obtain the product containing SiO2The starch sol of (a); adding 1 part of yeast and 3 parts of baking soda into the sol, stirring at 800 r/min for 20min, and keeping the temperature at 35 ℃ for 2 h to obtain porous sol; putting the porous sol into a water bath, preserving the heat at 98 ℃ for 40 min, taking out a sample, putting the sample into an oven, and drying the sample at 110 ℃ to constant weight to obtain porous gel; keeping the temperature at 600 ℃ in a nitrogen atmosphere to obtain porous carbon with constant weight; under the protection of argon, the temperature is raised to 1800 ℃ at the heating rate of 12 ℃/min, and the temperature is kept for 2 h and then the C/SiC composite material with the vibrissa-like-nostril structure is obtained after furnace cooling.
Example 4: putting 100 parts of wheat starch, 10 parts of silicon dioxide, 110 parts of water and 0.5 part of polyacrylamide into a planetary ball mill, and ball-milling for 2 hours at the speed of 30 r/min to obtain the product containing SiO2The starch sol of (a); adding 5 parts of dodecyl sulfuric acid triethanolamine into the sol, stirring for 20min at the speed of 800 r/min, and keeping the temperature at 35 ℃ for 2 h to obtain porous sol; putting the porous sol into a water bath, preserving the heat at 100 ℃ for 40 min, taking out a sample, putting the sample into an oven, and drying the sample at 110 ℃ to constant weight to obtain porous gel; nitrogen gasKeeping the temperature at 600 ℃ and balancing the weight to obtain porous carbon; under the protection of argon, the temperature is raised to 1550 ℃ at the heating rate of 10 ℃/min, and the C/SiC composite material with the vibrissa-nostril structure is obtained after the temperature is preserved for 10 h at 1550 ℃. .
Example 5: putting 100 parts of sorghum starch, 8 parts of silicon dioxide, 90 parts of water and 0.05 part of CAMTMENT FS20 into a planetary ball mill for ball milling for 2 hours at a speed of 30 r/min to obtain the product containing SiO2The starch sol of (a); adding 5 parts of lauryl triethanolamine sulfate into the sol, stirring for 10min at a speed of 800 r/min, and keeping the temperature at 25 ℃ for 2 h to obtain porous sol; putting the porous sol into a water bath kettle, preserving the heat at 94 ℃ for 40 min, and drying at 110 ℃ to constant weight to obtain porous gel; keeping the temperature of 600 ℃ in a nitrogen atmosphere until the weight is constant to obtain porous carbon; and under the protection of argon, heating to 1750 ℃ at the heating rate of 10-15 ℃/min, preserving heat for 4 hours, and cooling along with the furnace to obtain the C/SiC composite material with the vibrissa-nostril like structure.
TABLE 1
Claims (5)
1. A preparation method of a C/SiC composite material with a vibrissa-nostril-like structure is characterized by comprising the following steps: the preparation method is to use starch and SiO2The preparation method comprises the following steps of (1) taking water as a solvent, adding a dispersing agent and a foaming agent, and forming silicon dioxide-containing foam carbon by carrying out sol, foaming, gel curing and carbonization on starch; after in-situ high-temperature carbon thermal reduction reaction, a large number of SiC nanowires grow in air holes of foam carbon, the generation of the SiC nanowires modifies the pore structure of the foam C, limits convection and radiation heat transfer, and obviously reduces the thermal conductivity of the material, and the specific steps are as follows:
1) preparing a silicon-containing starch sol:
putting starch, silicon dioxide, water and a dispersing agent into a planetary ball mill according to a certain proportion, and ball-milling and uniformly mixing to obtain stable silicon dioxide-containing starch sol;
2) a foaming step:
adding a foaming agent into the silica-containing starch sol obtained in the step 1), stirring for 20min by using a stirrer, and standing for 2 h at the temperature of 30-45 ℃ to obtain porous sol;
3) and (3) gel curing:
heating the porous sol obtained in the step 2) in a water bath at 80-100 ℃, preserving heat for 40 min, and drying at 110 ℃ to constant weight to obtain porous gel;
4) and (3) carbonizing:
carbonizing the porous gel obtained in the step 3) to constant weight at 600 ℃ under the protection of nitrogen or argon to obtain silicon dioxide-containing foamy carbon;
5) a carbothermic reduction reaction step:
and (3) heating the foam carbon containing the silicon dioxide obtained in the step (4) to 1550-1850 ℃ at a heating rate of 10-15 ℃/min under the protection of argon, preserving heat at 1500-1800 ℃ for 3-10 h, and cooling along with a furnace to obtain the C/SiC composite material with the vibrissa-nostril structure.
2. The method of claim 1, wherein the C/SiC composite material has a vibrissa-like-nostril structure, and the method comprises the following steps: the starch in the step 1) is one or more of wheat starch, corn starch, sweet potato starch, sorghum starch and the like.
3. The method of claim 1, wherein the C/SiC composite material has a vibrissa-like-nostril structure, and the method comprises the following steps: the dispersant in the step 1) is one or more of polyacrylamide, CAMTMENT FS20 and tetramethylethylenediamine.
4. The method of claim 1, wherein the C/SiC composite material has a vibrissa-like-nostril structure, and the method comprises the following steps: the foaming agent in the step 2) is one or more of lauryl triethanolamine sulfate, yeast, egg white, baking soda and the like.
5. The method of claim 1, wherein the C/SiC composite material has a vibrissa-like-nostril structure, and the method comprises the following steps: the mass ratio of the starch to the silicon dioxide to the foaming agent to the water to the dispersing agent is 100: 5-15: 0.5-10: 80-130: 0.02-1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011243124.4A CN112457034A (en) | 2020-11-10 | 2020-11-10 | Preparation method of C/SiC composite material with vibrissa-nostril-like structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011243124.4A CN112457034A (en) | 2020-11-10 | 2020-11-10 | Preparation method of C/SiC composite material with vibrissa-nostril-like structure |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112457034A true CN112457034A (en) | 2021-03-09 |
Family
ID=74826372
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011243124.4A Pending CN112457034A (en) | 2020-11-10 | 2020-11-10 | Preparation method of C/SiC composite material with vibrissa-nostril-like structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112457034A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118302384A (en) * | 2021-12-02 | 2024-07-05 | 尼邦科恩迈尔特种石墨集团有限责任公司 | Method for producing high purity silicon carbide powder |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0303479A2 (en) * | 1987-08-12 | 1989-02-15 | Alcan International Limited | Method of preparing whiskers of silicon carbide and other materials |
| EP0677496A2 (en) * | 1994-04-12 | 1995-10-18 | New Oji Paper Co., Ltd. | Process for producing silicon carbide material |
| CN106747628A (en) * | 2017-02-22 | 2017-05-31 | 南京航空航天大学 | A kind of high temperature resistant foam strengthens SiO2Aerogel insulating material and preparation method thereof |
| CN108751159A (en) * | 2018-05-27 | 2018-11-06 | 南京航空航天大学 | A kind of compound carbon foam of CVI-SiC nano wires enhancing |
| CN109320277A (en) * | 2018-11-16 | 2019-02-12 | 江苏科技大学 | A kind of preparation method of SiCnw/C nanocomposite |
| CN110590394A (en) * | 2019-10-29 | 2019-12-20 | 中钢集团洛阳耐火材料研究院有限公司 | Low-cost preparation method of large-size SiC nanowire aerogel |
-
2020
- 2020-11-10 CN CN202011243124.4A patent/CN112457034A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0303479A2 (en) * | 1987-08-12 | 1989-02-15 | Alcan International Limited | Method of preparing whiskers of silicon carbide and other materials |
| EP0677496A2 (en) * | 1994-04-12 | 1995-10-18 | New Oji Paper Co., Ltd. | Process for producing silicon carbide material |
| CN106747628A (en) * | 2017-02-22 | 2017-05-31 | 南京航空航天大学 | A kind of high temperature resistant foam strengthens SiO2Aerogel insulating material and preparation method thereof |
| CN108751159A (en) * | 2018-05-27 | 2018-11-06 | 南京航空航天大学 | A kind of compound carbon foam of CVI-SiC nano wires enhancing |
| CN109320277A (en) * | 2018-11-16 | 2019-02-12 | 江苏科技大学 | A kind of preparation method of SiCnw/C nanocomposite |
| CN110590394A (en) * | 2019-10-29 | 2019-12-20 | 中钢集团洛阳耐火材料研究院有限公司 | Low-cost preparation method of large-size SiC nanowire aerogel |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118302384A (en) * | 2021-12-02 | 2024-07-05 | 尼邦科恩迈尔特种石墨集团有限责任公司 | Method for producing high purity silicon carbide powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110590394B (en) | Low-cost preparation method of large-size SiC nanowire aerogel | |
| CN109868118B (en) | Preparation method of aluminum nitride-aluminum oxide core-shell structure with high thermal conductivity | |
| CN109652022B (en) | Preparation method of novel composite diatomite phase change energy storage material carrier | |
| CN110066175B (en) | Preparation method of ultralight carbide ceramic foam | |
| CN112457034A (en) | Preparation method of C/SiC composite material with vibrissa-nostril-like structure | |
| CN113716966B (en) | SiCN ceramic aerogel and preparation method and application thereof | |
| CN113663611A (en) | High-temperature-resistant composite nanofiber aerogel material and preparation method thereof | |
| CN114572985A (en) | Preparation method and application of starch-based carbon aerogel | |
| CN114213696A (en) | Light flexible high-temperature-resistant heat-insulating polyimide foam and preparation method and application thereof | |
| CN114715896A (en) | Preparation method of silicon carbide nanotube aerogel | |
| CN108102348A (en) | A kind of phosphor-containing flame-proof hard polyurethane foams based on expansible graphite and preparation method thereof | |
| CN112521178A (en) | Preparation method of alumina foamed ceramic | |
| CN113698762A (en) | Low-density high-toughness bismaleimide foam material and preparation method thereof | |
| CN112047742B (en) | Low-cost preparation method of large-size silicon nitride nanobelt aerogel | |
| CN107043224A (en) | Foam glass-SiO2Method for producing aerogels | |
| CN108752038A (en) | It is a kind of with can be thermally cured Polycarbosilane preparation foam silicon carbide ceramics | |
| CN112175231A (en) | Phenolic toughening modified porous hybrid silicon resin, preparation method and application | |
| CN114604857A (en) | Graphitization treatment method for graphene heat-conducting film | |
| CN111253144A (en) | Preparation method of titanium-doped silicon dioxide aerogel/fiber composite material | |
| CN113648940A (en) | Ultra-light high-elasticity radiation-resistant nanofiber aerogel material and preparation method thereof | |
| CN111548183B (en) | Method for preparing graded porous silicon carbide ceramic by gel casting and carbothermic reduction | |
| CN106395873A (en) | Preparation method of ultra-light blocky aluminum oxide aerogel | |
| CN110317977A (en) | A kind of preparation method of graphene aerogel aluminium composite material | |
| CN115611632B (en) | Preparation method of flexible high-temperature-resistant silicon carbide aerogel composite heat insulation material | |
| CN111825073A (en) | Preparation method of fluorinated graphene |
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 | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20220602 Address after: 471039 No. 43, Xiyuan Road, Jianxi District, Henan, Luoyang Applicant after: SINOSTEEL LUOYANG INSTITUTE OF REFRACTORIES RESEARCH Co.,Ltd. Address before: No.70 Phoenix Road, Jiangning District, Nanjing City, Jiangsu Province (Jiangning Development Zone) Applicant before: Sinosteel Nanjing Environmental Engineering Technology Research Institute Co.,Ltd. Applicant before: SINOSTEEL LUOYANG INSTITUTE OF REFRACTORIES RESEARCH Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210309 |
|
| RJ01 | Rejection of invention patent application after publication |