CN115703636A - Preparation technology of porous nano silicon carbide and carbon composite material thereof - Google Patents
Preparation technology of porous nano silicon carbide and carbon composite material thereof Download PDFInfo
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- CN115703636A CN115703636A CN202110940786.5A CN202110940786A CN115703636A CN 115703636 A CN115703636 A CN 115703636A CN 202110940786 A CN202110940786 A CN 202110940786A CN 115703636 A CN115703636 A CN 115703636A
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- silicon carbide
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 46
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 32
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000005516 engineering process Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 45
- 239000002002 slurry Substances 0.000 claims abstract description 28
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- 235000015895 biscuits Nutrition 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 239000003999 initiator Substances 0.000 claims abstract description 12
- 239000000178 monomer Substances 0.000 claims abstract description 12
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 238000007599 discharging Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 11
- 229920000058 polyacrylate Polymers 0.000 claims description 11
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 8
- 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 6
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 6
- 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 6
- 229930006000 Sucrose Natural products 0.000 claims description 6
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
- 239000008103 glucose Substances 0.000 claims description 6
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 6
- 239000005720 sucrose Substances 0.000 claims description 6
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 229920002472 Starch Polymers 0.000 claims description 5
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 5
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 5
- 229920001542 oligosaccharide Polymers 0.000 claims description 5
- 150000002482 oligosaccharides Chemical class 0.000 claims description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000008107 starch Substances 0.000 claims description 5
- 235000019698 starch Nutrition 0.000 claims description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 4
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- UXBMPEBBRQPJDL-UHFFFAOYSA-N 3-hydroxy-2-methylprop-2-enamide Chemical compound OC=C(C)C(N)=O UXBMPEBBRQPJDL-UHFFFAOYSA-N 0.000 claims description 3
- PMELSLUAEIGQKI-UHFFFAOYSA-N C=C.C=C.C=C.N.N Chemical compound C=C.C=C.C=C.N.N PMELSLUAEIGQKI-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 238000003828 vacuum filtration Methods 0.000 abstract description 6
- 238000001035 drying Methods 0.000 abstract 1
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 4
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- WPKYZIPODULRBM-UHFFFAOYSA-N azane;prop-2-enoic acid Chemical compound N.OC(=O)C=C WPKYZIPODULRBM-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Ceramic Products (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation technology of porous nano silicon carbide and a carbon composite material thereof, which comprises the following steps: step 1, uniformly mixing ethyl orthosilicate, absolute ethyl alcohol and deionized water, adding an organic carbon source, stirring, and performing vacuum filtration to obtain a filtrate; step 2, placing the filter in a ball milling tank for ball milling, adding an organic monomer, a cross-linking agent, a dispersing agent and a rare earth oxide, and continuing ball milling to obtain slurry A; step 3, adding a catalyst and an initiator into the slurry A, and uniformly stirring to form slurry B; injecting the slurry B into a mold, curing and molding at room temperature, demolding to form a biscuit, and drying; step 4, putting the dried biscuit in a vacuum furnace, and performing heat treatment to obtain a porous nano silicon carbide-carbon composite material; and 5, placing the porous nano silicon carbide-carbon composite material in a muffle furnace, and performing heat treatment to obtain the porous nano silicon carbide material.
Description
Technical Field
The invention relates to a preparation technology of a nano silicon carbide material, in particular to a preparation technology of porous nano silicon carbide and a carbon composite material thereof.
Background
The silicon carbide nano material has the characteristics of high thermal conductivity, strong thermal stability, excellent corrosion resistance and oxidation resistance, low thermal expansion coefficient and the like, and is widely applied to the fields of aerospace, electronic communication, energy chemical industry, intelligent equipment and the like.
The porous nanometer silicon carbide material has nanometer pores, so that the internal pore structure of the material is complex, and the thermal resistance of solid phase heat transfer is further improved. Moreover, the nano-voids can also obstruct the gas flow inside the material, limiting its gas phase heat transfer. Therefore, the porous nanomaterial has more excellent thermal insulation properties than a general porous material. In particular, porous nanomaterials mainly composed of silicon carbide are applied to heat insulating materials in special environments.
The porous carbon-silicon carbide nano composite material is an electric absorption type absorber, and the wave-absorbing material is mainly applied to the fields of electronic instruments, electromagnetic equipment, high-frequency equipment, shielding boxes and the like. The wave absorbing material is prepared into different shapes such as a sharp cone shape, a sheet shape and the like by adopting a special mode, and is mainly applied to high-power wave absorbing load and wave absorbing dark boxes. And because of the excellent thermal vacuum property, the material is applied to the aerospace field. The porous nano silicon carbide and the carbon composite material thereof have extremely wide and potential application values in many fields due to the unique optical and electrical characteristics and excellent physical and mechanical properties.
However, the current production process of the porous nano silicon carbide and the carbon composite material thereof has the problems of long process, complex process, high cost, unstable performance index and the like, and cannot meet the requirements of related application fields.
Disclosure of Invention
The technical task of the invention is to provide a preparation technology of porous nano silicon carbide and a carbon composite material thereof aiming at the defects in the prior art, and the preparation technology of the porous nano silicon carbide and the carbon composite material thereof has the characteristics of short flow, environmental protection, low cost and high efficiency.
The technical scheme adopted by the invention for solving the technical problem is that the method sequentially comprises the following steps:
step 1, uniformly mixing 520ml of tetraethoxysilane, 1300-2080 ml of absolute ethanol and 1040-2340 ml of deionized water; adding 121.5 to 360g of an organic carbon source under the water bath condition of 65 to 70 ℃, and stirring for 3 to 6 hours; and (5) carrying out vacuum filtration to obtain a filtrate.
And 2, putting the filter material in the step 1 into a ball milling pot, ball milling for 5-10h, then adding 1.5-6g of organic monomer, 0.03-0.12g of cross-linking agent, 0.75-7.5g of dispersing agent and rare earth oxide, and continuing ball milling for 2-4h to obtain slurry A.
Step 3, adding 0.015 to 1.2g of catalyst and 0.15 to 2.25g of initiator into the slurry A in the step 2, and uniformly stirring to form slurry B; injecting the slurry B into a mold, curing and molding at room temperature, and demolding to form a blank; and (3) placing the biscuit in an environment at 100 ℃ and preserving heat for 2-6 h until the weight is not changed.
And 4, putting the dried biscuit in the step 3 into a vacuum furnace, and performing heat treatment to obtain the porous nano silicon carbide-carbon composite material.
And 5, placing the porous nano silicon carbide-carbon composite material in the step 4 in a muffle furnace, and performing heat treatment to obtain the porous nano silicon carbide material.
The invention is also characterized in that:
the organic carbon source in the step 1 comprises one or a combination of sucrose, glucose, oligosaccharide and starch.
The organic monomer in the step 2 comprises one or a combination of more of acrylamide, hydroxyl-methyl-acrylamide and methacrylic acid-2-hydroxyethyl ester.
The cross-linking agent in the step 2 comprises one or a combination of more of trimethylolpropane triacrylate, N' -methylene bisacrylamide and diacetone acrylamide.
The dispersant in the step 2 comprises one or a combination of polyethylene glycol, ammonium polyacrylate, sodium hydroxy cellulose and hexadecyl trimethyl ammonium bromide.
The rare earth oxide in the step 2 comprises one or a combination of more of yttrium oxide, lanthanum oxide and cerium oxide.
The catalyst in the step 3 comprises one or a combination of two of tetramethyl ethylene diamine and triethylene diammonium.
The initiator in the step 3 comprises one or a combination of ammonium carbonate, ammonium polyacrylate, ammonium persulfate and potassium persulfate.
The heat treatment process in the step 4 comprises the following steps: the temperature rise process is divided into three time periods, (1) the temperature rise rate is 2~8 ℃/min, the temperature is raised to 550 to 650 ℃, and the temperature is kept for 1 to 3h; (2) Heating at the temperature rise rate of 5 to 10 ℃/min to 1180 to 1280 ℃, and keeping the temperature for 0.5 to 2h; (3) Heating at the rate of 10-15 ℃/min to 1390-1650 ℃, keeping the temperature for 4-8h, naturally cooling to room temperature, and then discharging.
The heat treatment process in the step 5 comprises the following steps: heating to 800-980 ℃ at a heating rate of 5~8 ℃/min for 3-7 h, naturally cooling to room temperature, and discharging
Compared with the prior art, the preparation technology of the porous nano silicon carbide material has the following outstanding beneficial effects: energy conservation, environmental protection, short flow, high efficiency and the like.
Detailed Description
The present invention will be described in detail with reference to the following embodiments:
the invention relates to a preparation technology of porous nano silicon carbide and a carbon composite material thereof, which is characterized by sequentially comprising the following steps:
step 1, uniformly mixing 520ml of tetraethoxysilane, 1300-2080 ml of absolute ethanol and 1040-2340 ml of deionized water; adding 121.5 to 360g of an organic carbon source under the water bath condition of 65 to 70 ℃, and stirring for 3 to 6 hours; and (5) carrying out vacuum filtration to obtain a filtrate.
Wherein the organic carbon source comprises one or more of sucrose, glucose, oligosaccharide and starch.
And 2, putting the filter material in the step 1 into a ball milling pot, ball milling for 5-10h, then adding 1.5-6g of organic monomer, 0.03-0.12g of cross-linking agent, 0.75-7.5g of dispersing agent and rare earth oxide, and continuing ball milling for 2-4h to obtain slurry A.
Wherein the organic monomer comprises one or more of acrylamide, hydroxyl-methyl-acrylamide and 2-hydroxyethyl methacrylate; the cross-linking agent comprises one or a combination of more of trimethylolpropane triacrylate, N' -methylene bisacrylamide and diacetone acrylamide; the dispersant comprises one or more of polyethylene glycol, ammonium polyacrylate, sodium hydroxy cellulose and hexadecyl trimethyl ammonium bromide; the rare earth oxide comprises one or more of yttrium oxide, lanthanum oxide and cerium oxide.
Step 3, adding 0.015 to 1.2g of catalyst and 0.15 to 2.25g of initiator into the slurry A in the step 2, and uniformly stirring to form slurry B; injecting the slurry B into a mold, curing and molding at room temperature, and demolding to form a biscuit; and (3) placing the biscuit in an environment at 100 ℃ and preserving heat for 2-6 h until the weight is not changed.
Wherein, the catalyst comprises one or the combination of two of tetramethyl ethylene diamine and triethylene diammonium; the initiator comprises one or a combination of ammonium carbonate, ammonium polyacrylate, ammonium persulfate and potassium persulfate.
And 4, putting the dried biscuit in the step 3 into a vacuum furnace, and performing heat treatment to obtain the porous nano silicon carbide-carbon composite material. The heat treatment process comprises the following steps: the temperature rise process is divided into three time periods, (1) the temperature rise rate is 2~8 ℃/min, the temperature is raised to 550 to 650 ℃, and the temperature is kept for 1 to 3h; (2) Heating at the rate of 5-10 ℃/min to 1180-1280 ℃ and keeping the temperature for 0.5-2h; (3) Heating at the rate of 10 to 15 ℃/min to 1390 to 1650 ℃, keeping the temperature for 4 to 8h, naturally cooling to the room temperature, and discharging.
And 5, placing the porous nano silicon carbide-carbon composite material in the step 4 in a muffle furnace, and performing heat treatment to obtain the porous nano silicon carbide material. The heat treatment process comprises the following steps: heating to 800-980 ℃ at a heating rate of 5~8 ℃/min for 3-7 h, naturally cooling to room temperature, and discharging.
Example 1
Uniformly mixing 520ml of tetraethoxysilane, 1500ml of absolute ethyl alcohol and 1200ml of deionized water; adding 140g of organic carbon source under the condition of 66 ℃ water bath, and stirring for 4h; and (5) carrying out vacuum filtration to obtain a filtrate.
The ratio of sucrose, glucose, oligosaccharide and starch in the organic carbon source is 4.
And (3) placing the filter in a ball milling tank for ball milling for 6h, adding 2g of organic monomer, 0.06g of cross-linking agent, 3g of dispersing agent and 1g of rare earth oxide, and continuing ball milling for 3h to obtain slurry A.
The proportion of organic monomers acrylamide, hydroxy-methyl-acrylamide and 2-hydroxyethyl methacrylate is 7; the proportion of the cross-linking agent trimethylolpropane triacrylate, N' -methylene bisacrylamide and diacetone acrylamide is 7; the proportion of the dispersant polyethylene glycol, ammonium polyacrylate, sodium hydroxy cellulose and hexadecyl trimethyl ammonium bromide is 7; the proportion of rare earth oxide yttrium oxide, lanthanum oxide and cerium oxide is 8.
Adding 0.6g of catalyst and 1.2g of initiator into the slurry A, and uniformly stirring to form slurry B; injecting the slurry B into a mold, curing and molding at room temperature, and demolding to form a biscuit; and (3) placing the embryo in an environment of 100 ℃ and preserving heat for 4h until the weight is not changed.
The ratio of the catalyst tetramethylethylenediamine to the catalyst triethylenediamine is 7:3; the ratio of the initiator ammonium carbonate, ammonium polyacrylate, ammonium persulfate and potassium persulfate is 7.
Putting the dried biscuit in a vacuum furnace, wherein the heating process is divided into three periods, (1) the heating rate is 6 ℃/min, and the biscuit is heated to 600 ℃ and is kept for 2 hours; (2) heating to 1200 ℃ at a heating rate of 7 ℃/min, and keeping the temperature for 1h; (3) Heating to 1550 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 5h, naturally cooling to room temperature, and discharging. The porous nano silicon carbide-carbon composite material is obtained, the aperture is 200nm, and the porosity is 87%.
Placing the porous nano silicon carbide-carbon composite material in a muffle furnace, heating to 920 ℃ at the heating rate of 6 ℃/min, keeping the temperature for 5 hours, naturally cooling to room temperature, and discharging. Finally obtaining the porous nano silicon carbide material with the aperture of 350nm and the porosity of 96%.
Example 2
Mixing 520ml of tetraethoxysilane, 1800ml of absolute ethyl alcohol and 1100ml of deionized water uniformly; adding 300g of organic carbon source under the condition of 70 ℃ water bath, and stirring for 5h; and (5) carrying out vacuum filtration to obtain a filtrate.
The ratio of sucrose, glucose, oligosaccharide and starch in the organic carbon source is 1.
And (3) placing the filter in a ball milling tank for ball milling for 8h, adding 4g of organic monomer amine acrylate, 0.09g of cross-linking agent trimethylolpropane triacrylate, 6g of dispersing agent ammonium polyacrylate and 1.5g of rare earth oxide yttrium oxide, and continuing ball milling for 2h to obtain slurry A.
Adding 0.08g of catalyst tetramethylethylenediamine and 1.8g of initiator ammonium persulfate into the slurry A, and uniformly stirring to form slurry B; injecting the slurry B into a mold, curing and molding at room temperature, and demolding to form a biscuit; and (3) placing the blank in an environment of 100 ℃ and preserving heat for 5 hours until the weight is not changed.
Putting the dried biscuit in a vacuum furnace, wherein the heating process is divided into three periods, (1) the heating rate is 5 ℃/min, and the biscuit is heated to 650 ℃ and is kept for 2.5h; (2) raising the temperature to 1250 ℃ at the heating rate of 10 ℃/min and preserving the heat for 2h; (3) Raising the temperature to 1450 ℃ at a heating rate of 15 ℃/min, preserving the heat for 8h, naturally cooling to room temperature, and discharging. The porous nano silicon carbide-carbon composite material is obtained, the aperture is 150nm, and the porosity is 88%.
Placing the porous nano silicon carbide-carbon composite material in a muffle furnace, heating to 950 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 6 hours, naturally cooling to room temperature, and discharging. Finally obtaining the porous nano silicon carbide material with the aperture of 300nm and the porosity of 95 percent.
Example 3
Mixing 520ml of tetraethoxysilane, 2000ml of absolute ethyl alcohol and 1500ml of deionized water uniformly; adding 360g of organic carbon source under the condition of 70 ℃ water bath, and stirring for 3.5h; and (5) carrying out vacuum filtration to obtain a filtrate.
The ratio of sucrose to glucose in the organic carbon source is 3:7.
And (3) placing the filter in a ball milling tank for ball milling for 5 hours, then adding 1.6g of organic monomer, 0.04g of cross-linking agent, 4.5g of dispersing agent and 2.5g of rare earth oxide, and continuing ball milling for 4 hours to obtain slurry A.
The ratio of the organic monomer acrylamide to the hydroxy-methyl-acrylamide is 9:1; the proportion of the cross-linking agent trimethylolpropane triacrylate and N, N' -methylenebisacrylamide is 8:2; the proportion of the dispersant polyethylene glycol and the ammonium polyacrylate is 6:4; the ratio of rare earth oxide yttrium oxide to cerium oxide is 9:1.
Adding 1g of catalyst and 0.8g of initiator into the slurry A, and uniformly stirring to form slurry B; injecting the slurry B into a mold, curing and molding at room temperature, and demolding to form a biscuit; and (3) placing the blank in an environment of 100 ℃ for heat preservation for 4 hours until the weight is not changed.
The ratio of the catalyst tetramethylethylenediamine to the catalyst triethylenediamine is 9:1; the ratio of the initiator ammonium polyacrylate to the ammonium persulfate is 2:8.
Putting the dried biscuit in a vacuum furnace, wherein the heating process is divided into three periods, (1) the heating rate is 3 ℃/min, and the biscuit is heated to 580 ℃ and is kept for 1h; (2) raising the temperature to 1180 ℃ at the rate of 5 ℃/min and keeping the temperature for 0.5h; (3) Raising the temperature to 1550 ℃ at the heating rate of 5 ℃/min, preserving the heat for 5h, naturally cooling to room temperature, and discharging. The porous nano silicon carbide-carbon composite material is obtained, the aperture is 320nm, and the porosity is 90%.
Placing the porous nano silicon carbide-carbon composite material in a muffle furnace, heating to 970 ℃ at the heating rate of 8 ℃/min, keeping the temperature for 3h, naturally cooling to room temperature, and discharging. Finally obtaining the porous nano silicon carbide material with the pore diameter of 430nm and the porosity of 93 percent.
Claims (10)
1. A preparation technology of porous nanometer silicon carbide and a carbon composite material thereof is characterized by sequentially comprising the following steps:
step 1, uniformly mixing 520ml of tetraethoxysilane, 1300-2080 ml of absolute ethanol and 1040-2340 ml of deionized water; adding 121.5 to 360g of an organic carbon source under the water bath condition of 65 to 70 ℃, and stirring for 3 to 6 hours; vacuum filtering to obtain filtrate;
step 2, putting the filter material in the step 1 into a ball milling pot, ball milling for 5-10h, then adding 1.5-6g of organic monomer, 0.03-0.12g of cross-linking agent, 0.75-7.5g of dispersing agent and rare earth oxide, and continuing ball milling for 2-4h to obtain slurry A;
step 3, adding 0.015 to 1.2g of catalyst and 0.15 to 2.25g of initiator into the slurry A in the step 2, and uniformly stirring to form slurry B; injecting the slurry B into a mold, curing and molding at room temperature, and demolding to form a biscuit; placing the biscuit in an environment of 100 ℃ and preserving heat for 2-6 h until the weight is not changed;
step 4, putting the dried biscuit blank obtained in the step 3 into a vacuum furnace, and performing heat treatment to obtain a porous nano silicon carbide-carbon composite material;
and 5, placing the porous nano silicon carbide-carbon composite material in the step 4 in a muffle furnace, and performing heat treatment to obtain the porous nano silicon carbide material.
2. The technology for preparing the porous nano silicon carbide and the carbon composite material thereof according to the claim 1, wherein the organic carbon source in the step 1 comprises one or more of sucrose, glucose, oligosaccharide and starch.
3. The preparation technology of the porous nano silicon carbide and the carbon composite material thereof according to claim 1, wherein the organic monomer in the step 2 comprises one or more of acrylamide, hydroxyl-methyl-acrylamide and 2-hydroxyethyl methacrylate.
4. The preparation technology of the porous nano silicon carbide and the carbon composite material thereof according to the claim 1, wherein the cross-linking agent in the step 2 comprises one or more of trimethylolpropane triacrylate, N' -methylenebisacrylamide and bisacetoacrylic acid amine.
5. The preparation technology of the porous nano silicon carbide and the carbon composite material thereof according to claim 1, wherein the dispersant in the step 2 comprises one or more of polyethylene glycol, ammonium polyacrylate, sodium hydroxy cellulose and hexadecyl trimethyl ammonium bromide.
6. The preparation technology of the porous nano silicon carbide and the carbon composite material thereof as claimed in claim 1, wherein the rare earth oxide in step 2 comprises one or more of yttrium oxide, lanthanum oxide and cerium oxide.
7. The technology for preparing the porous nano silicon carbide and the carbon composite material thereof according to the claim 1, wherein the catalyst in the step 3 comprises one or a combination of tetramethyl ethylene diamine and triethylene diammonium.
8. The technology for preparing the porous nano silicon carbide and the carbon composite material thereof according to the claim 1, wherein the initiator in the step 3 comprises one or more of ammonium carbonate, ammonium polyacrylate, ammonium persulfate and potassium persulfate.
9. The preparation technology of the porous nano silicon carbide and the carbon composite material thereof according to the claim 1, characterized in that the heat treatment process in the step 4 is as follows: the temperature rise process is divided into three time periods, (1) the temperature rise rate is 2~8 ℃/min, the temperature is raised to 550 to 650 ℃, and the temperature is kept for 1 to 3h; (2) Heating at the temperature rise rate of 5 to 10 ℃/min to 1180 to 1280 ℃, and keeping the temperature for 0.5 to 2h; (3) Heating at the rate of 10-15 ℃/min to 1390-1650 ℃, keeping the temperature for 4-8h, naturally cooling to room temperature, and then discharging.
10. The preparation technology of the porous nano silicon carbide and the carbon composite material thereof according to the claim 1, characterized in that the heat treatment process in the step 5 is as follows: heating to 800-980 ℃ at a heating rate of 5~8 ℃/min for 3-7 h, naturally cooling to room temperature, and discharging.
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|---|---|---|---|---|
| CN102030534A (en) * | 2010-11-09 | 2011-04-27 | 浙江大学 | Method for preparing silicon carbide ceramic |
| JP2014181144A (en) * | 2013-03-18 | 2014-09-29 | Gaia Institute Of Environmental Technology Inc | Rice husk coal or rice straw coal including abundance of amorphous silica, method for manufacturing rice husk coal or rice straw coal including abundance of amorphous silica, and food, agricultural fertilizer, and fodder each including abundance of amorphous silica |
| CN105036751A (en) * | 2015-09-06 | 2015-11-11 | 哈尔滨工业大学 | Method for preparing ceramic through micro-nano grain-size grading |
| CN111825093A (en) * | 2020-07-31 | 2020-10-27 | 黑龙江冠瓷科技有限公司 | Preparation method of SiC nano powder particles |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030534A (en) * | 2010-11-09 | 2011-04-27 | 浙江大学 | Method for preparing silicon carbide ceramic |
| JP2014181144A (en) * | 2013-03-18 | 2014-09-29 | Gaia Institute Of Environmental Technology Inc | Rice husk coal or rice straw coal including abundance of amorphous silica, method for manufacturing rice husk coal or rice straw coal including abundance of amorphous silica, and food, agricultural fertilizer, and fodder each including abundance of amorphous silica |
| CN105036751A (en) * | 2015-09-06 | 2015-11-11 | 哈尔滨工业大学 | Method for preparing ceramic through micro-nano grain-size grading |
| CN111825093A (en) * | 2020-07-31 | 2020-10-27 | 黑龙江冠瓷科技有限公司 | Preparation method of SiC nano powder particles |
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