CN102674354A - Preparation method for mesoporous silicon carbide material - Google Patents
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- CN102674354A CN102674354A CN2012101460696A CN201210146069A CN102674354A CN 102674354 A CN102674354 A CN 102674354A CN 2012101460696 A CN2012101460696 A CN 2012101460696A CN 201210146069 A CN201210146069 A CN 201210146069A CN 102674354 A CN102674354 A CN 102674354A
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- 239000013370 mesoporous silicon carbide Substances 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 34
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002243 precursor Substances 0.000 claims abstract description 20
- 239000011240 wet gel Substances 0.000 claims abstract description 19
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000000499 gel Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 230000032683 aging Effects 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 20
- 229910052786 argon Inorganic materials 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 239000003610 charcoal Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 13
- 239000002245 particle Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract 2
- 239000002253 acid Substances 0.000 abstract 1
- 239000003513 alkali Substances 0.000 abstract 1
- 238000001354 calcination Methods 0.000 abstract 1
- 235000019256 formaldehyde Nutrition 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 238000009991 scouring Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- 239000000377 silicon dioxide Substances 0.000 description 8
- 229960001866 silicon dioxide Drugs 0.000 description 7
- 235000012239 silicon dioxide Nutrition 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 230000036760 body temperature Effects 0.000 description 6
- 239000013335 mesoporous material Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 238000003980 solgel method Methods 0.000 description 4
- 238000002336 sorption--desorption measurement Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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Abstract
The invention belongs to the field of inorganic materials and material synthesis process, relating to a preparation method for a mesoporous silicon carbide material. The preparation method comprises the following steps of: preparing wet gel by taking resorcinol, methanal and tetraethyl orthosilicate are reactants, taking acid and alkali as catalysts and performing a sol-gel reaction; aging the wet gel, and drying the wet gel under the normal pressure to obtain silicon carbide precursors; performing carbon thermal reduction on the silicon carbide precursors by means of inert gas shielding to produce silicon carbide; and calcining, scouring, washing, filtering and drying the silicon carbide to obtain the mesoporous silicon carbide material. The preparation method has the advantages of readily available raw materials, simple equipment, and small particle sizes and larger specific surface areas of the silicon carbide.
Description
Technical field
The invention belongs to inorganic materials and material synthesis technique field, relate to a kind of preparation method of mesoporous silicon carbide material.
Background technology
Silit (SiC) material has many excellent properties such as good thermal conductivity and electroconductibility, resistance to elevated temperatures and chemicalstability, shaking property of heat resistanceheat resistant, low thermal coefficient of expansion, high firmness, in ceramic composite, high-abrasive material, catalyzer and photoelectron material field very big application potential is arranged.
SiC can prepare through methods such as traditional Acheson technology, precursor infiltration and pyrolysis method and shape memory synthesis methods, but these compound method carbothermic reduction temperature are higher, as the temperature of reaction of Acheson technology at 2000 ° more than the C.In addition, the porous SiC material granule that synthesizes of aforesaid method and aperture big (generally in micron level), specific surface area is little (generally is no more than 70m
2/ g).It is a kind of effective way for preparing high-specific surface area SiC mesoporous material or nano particle that sol-gel method combines carbo-thermal process, and this method utilizes sol-gel method to synthesize carbon-silica composite as presoma usually earlier, and presoma is through the synthetic SiC of pyrocarbon thermal reduction reaction; The particle of the mesoporous SiC material that this method obtains is little; Specific surface area is bigger, like people (Chem.Mater.2010,22 such as Nicholas Leventis; 2790-2803) a kind of method of utilizing the mesoporous SiC of sol-gel method and carbo-thermal process preparation of report; Median size is at 7 ~ 17nm, but its specific surface area is lower, is no more than 100m
2/ g.In addition, the preparation technology of the present SiC presoma of reporting is more complicated, needs the carbon sol and the SiO that will prepare respectively mostly
2Colloidal sol mixes.
Summary of the invention
The objective of the invention is to provide a kind of preparation method of mesoporous silicon carbide material for the deficiency of improving the prior art existence; This method technology is simple; Directly with adopting a step sol-gel method to prepare the silicon carbide precursor body after the raw materials mix, can prepare high-specific surface area, mesoporous silicon carbide material that particle diameter is little.
Technical scheme of the present invention is: a kind of preparation method of mesoporous silicon carbide material, and its concrete steps are following:
(1) Resorcinol, formaldehyde, positive tetraethyl orthosilicate, an acidic catalyst, soda ash light, deionized water, absolute ethyl alcohol are 1:2 in molar ratio: (0.25 ~ 2): (0.04 ~ 0.15): (0.003 ~ 0.01): (1 ~ 8): (20 ~ 160) mix; Stirred 30 ~ 90 minutes down at 50 ~ 70 ℃; Adding ammoniacal liquor adjusting pH value is 7.8 ~ 9.5; Under 50 ~ 70 ° of C, carry out sol gel reaction and obtain wet gel, wet gel obtains the silicon carbide precursor body through the laggard capable constant pressure and dry of overaging;
(2) the silicon carbide precursor body that obtains in the step (1) temperature rise rate with 2 ~ 4 ° of C/min under protection of inert gas is heated to 1450 ~ 1600 ° of C, is incubated 3 ~ 10 hours, cool the temperature to 500 ~ 700 ° of C then; And rare gas element is replaced by air, and be incubated 2 ~ 4 hours to remove residual charcoal, be chilled to room temperature; Take out sample; In hydrofluoric acid, soak then and remove silicon-dioxide, after washing, filtration, oven dry, obtain the light green mesoporous silicon carbide.
An acidic catalyst described in the preferred steps (1) is a kind of in hydrochloric acid or the nitric acid.
Preferred steps (1) the sol gel reaction time is 10 ~ 30 minutes; Aging condition is in the step (1): 50 ~ 75 ° of C wore out 1 ~ 7 day down; Drying conditions is in the step (1): drying is 24 ~ 48 hours under 40 ~ 60 ° of C.
Rare gas element described in the preferred steps (2) is a kind of in helium or the argon gas.The massfraction of the hydrofluoric acid described in the preferred steps (2) is 10 ~ 30%, and soak time is 1 ~ 3 hour.
The mesoporous silicon carbide material of the present invention's preparation can be used for fields such as catalystic material, ceramic composite, high-abrasive material, photoelectron material and high temperature insulating material.
Beneficial effect:
The mesoporous silicon carbide material of the inventive method preparation has following characteristics:
(1) low in raw material cost is easy to get, and equipment is simple, realizes scale prodn easily.
(2) silicon-carbide particle size be evenly distributed, have typical meso-hole structure characteristic.
Description of drawings
The XRD figure spectrum of the mesoporous silicon carbide material that Fig. 1 makes for instance 2.
The HRTEM photo of the mesoporous silicon carbide material that Fig. 2 makes for instance 2.
The SEM photo of the mesoporous silicon carbide material that Fig. 3 makes for instance 2.
The nitrogen adsorption desorption curve of the mesoporous silicon carbide material that Fig. 4 makes for instance 2, wherein ● with zero be respectively adsorption curve and desorption curve.
Embodiment
Instance 1
(1) Resorcinol, formaldehyde, positive tetraethyl orthosilicate, hydrochloric acid, soda ash light, deionized water, absolute ethyl alcohol are mixed for 1:2:1.5:0.06:0.008:6:100 in molar ratio; Under 50 ° of C, stirred 90 minutes; Adding ammoniacal liquor adjusting pH value is 7.8; Carry out sol gel reaction at 60 ° of C and obtained wet gel in 20 minutes, wet gel wore out 3 days under 70 ° of C, and drying obtained the silicon carbide precursor body in 36 hours in 50 ° of C baking ovens then.
(2) silicon carbide precursor body temperature rise rate with 4 ° of C/min under argon shield is heated to 1600 ° of C, is incubated 3 hours, cools the temperature to 500 ° of C then; And argon gas is replaced by air, and be incubated 4 hours to remove residual charcoal, be chilled to room temperature; Take out sample, in 30% hydrofluoric acid aqueous solution, soaked 1 hour then, remove the silicon-dioxide in the silit; After washing, filtration, oven dry, obtain the light green mesoporous silicon carbide.
The pore size distribution of the mesoporous silicon carbide material that makes is 5 ~ 26nm, and specific surface area is 196m
2/ g, median size is 6.5nm.
Instance 2
(1) Resorcinol, formaldehyde, positive tetraethyl orthosilicate, hydrochloric acid, soda ash light, deionized water, absolute ethyl alcohol are mixed for 1:2:1:0.09:0.01:4:120 in molar ratio; Under 60 ° of C, stirred 60 minutes; Adding ammoniacal liquor adjusting pH value is 8.5; Carry out sol gel reaction at 60 ° of C and obtained wet gel in 30 minutes, wet gel wore out 5 days under 75 ° of C, and drying obtained the silicon carbide precursor body in 48 hours in 40 ° of C baking ovens then.
(2) silicon carbide precursor body temperature rise rate with 2 ° of C/min under argon shield is heated to 1500 ° of C, is incubated 6 hours, cools the temperature to 600 ° of C then; And argon gas is replaced by air, and be incubated 3 hours to remove residual charcoal, be chilled to room temperature; Take out sample, in 20% hydrofluoric acid aqueous solution, soaked 2 hours then, remove the silicon-dioxide in the silit; After washing, filtration, oven dry, obtain the light green mesoporous silicon carbide.
The pore size distribution of the mesoporous silicon carbide material that makes is 4 ~ 13nm, and the BET specific surface area is 366m
2/ g, median size is 5.2nm.
The XRD figure spectrum of the prepared silit mesoporous material of this instance is as shown in Figure 1.XRD analysis carries out on the ARLX'TRA of Arl Inc. of Thermo Electron Corp. type X-ray diffraction appearance; Adopt CuK α diffraction, λ=0.15406nm, scanning speed 2 (°)/min, scanning angle 10 ~ 80 degree.Can know that from Fig. 1 the mesoporous silicon carbide of preparation is β-SiC, can calculate corresponding median size according to the Scherrer formula is 5.2nm.
The HRTEM photo of the prepared silit mesoporous material of this instance is as shown in Figure 2.Tem analysis adopts the JEM-2010 of company of NEC type transmission electron microscope.Can find out that from the HRTEM photo of sample the mesoporous silicon carbide of preparation has the spacing of 0.252nm, consistent with the spacing of (111) crystal face of β-SiC, this shows that also the silit of preparation is β-SiC.
The SEM photo of the prepared silit mesoporous material of this instance is as shown in Figure 3.The German LEO-1530VP of Carl Zeiss Inc. field emission scanning electron microscope is adopted in the SEM test.From the SEM photo, can find out, the silit mesoporous material particle size of the present invention preparation, be evenly distributed.
The nitrogen adsorption desorption curve of the prepared silit mesoporous material of this instance is as shown in Figure 4.The full-automatic specific surface area analysis appearance of the U.S. ASAP2020 of Micromeritics company type is adopted in the test of nitrogen adsorption desorption.As can be seen from the figure, the carbofrax material of preparation has typical meso-hole structure characteristic, and the BET specific surface area that the data through the adsorption desorption curve can calculate sample is 366m
2/ g.
(1) Resorcinol, formaldehyde, positive tetraethyl orthosilicate, nitric acid, soda ash light, deionized water, absolute ethyl alcohol are mixed for 1:2:0.5:0.04:0.003:1:20 in molar ratio; Under 60 ° of C, stirred 30 minutes; Adding ammoniacal liquor adjusting pH value is 8.5; Carry out sol gel reaction at 50 ° of C and obtained wet gel in 10 minutes, wet gel wore out 3 days under 50 ° of C, and drying obtained the silicon carbide precursor body in 36 hours in 50 ° of C baking ovens then.
(2) silicon carbide precursor body temperature rise rate with 2 ° of C/min under argon shield is heated to 1450 ° of C, is incubated 10 hours, cools the temperature to 600 ° of C then; And argon gas is replaced by air, and be incubated 3 hours to remove residual charcoal, be chilled to room temperature; Take out sample, in 10% hydrofluoric acid aqueous solution, soaked 3 hours then, remove the silicon-dioxide in the silit; After washing, filtration, oven dry, obtain the light green mesoporous silicon carbide.
The pore size distribution of the mesoporous silicon carbide material that makes is 25 ~ 35nm, and specific surface area is 173m
2/ g, median size is 6.9nm.
Instance 4
(1) Resorcinol, formaldehyde, positive tetraethyl orthosilicate, hydrochloric acid, soda ash light, deionized water, absolute ethyl alcohol are mixed for 1:2:1:0.15:0.004:2:160 in molar ratio; Under 70 ° of C, stirred 30 minutes; Adding ammoniacal liquor adjusting pH value is 9.5; Carry out sol gel reaction at 70 ° of C and obtained wet gel in 30 minutes, wet gel wore out 7 days under 75 ° of C, and drying obtained the silicon carbide precursor body in 24 hours in 60 ° of C baking ovens then.
(2) silicon carbide precursor body temperature rise rate with 2 ° of C/min under argon shield is heated to 1500 ° of C, is incubated 4 hours, cools the temperature to 500 ° of C then; And argon gas is replaced by air, and be incubated 4 hours to remove residual charcoal, be chilled to room temperature; Take out sample, in 20% hydrofluoric acid aqueous solution, soaked 2 hours then, remove the silicon-dioxide in the silit; After washing, filtration, oven dry, obtain the light green mesoporous silicon carbide.
The pore size distribution of the mesoporous silicon carbide material that makes is 5 ~ 25nm, and specific surface area is 298m
2/ g, median size is 4.7nm.
(1) Resorcinol, formaldehyde, positive tetraethyl orthosilicate, nitric acid, soda ash light, deionized water, absolute ethyl alcohol are mixed for 1:2:1:0.1:0.006:2:40 in molar ratio; Under 50 ° of C, stirred 60 minutes; Adding ammoniacal liquor adjusting pH value is 8.2; Carry out sol gel reaction at 50 ° of C and obtained wet gel in 25 minutes, wet gel wore out 1 day under 60 ° of C, and drying obtained the silicon carbide precursor body in 36 hours in 50 ° of C baking ovens then.
(2) silicon carbide precursor body temperature rise rate with 3 ° of C/min under argon shield is heated to 1550 ° of C, is incubated 6 hours, cools the temperature to 700 ° of C then; And argon gas is replaced by air, and be incubated 2 hours to remove residual charcoal, be chilled to room temperature; Take out sample, in 10% hydrofluoric acid aqueous solution, soaked 3 hours then, remove the silicon-dioxide in the silit; After washing, filtration, oven dry, obtain the light green mesoporous silicon carbide.
The pore size distribution of the mesoporous silicon carbide material that makes is 10 ~ 30nm, and specific surface area is 221m
2/ g, median size is 5.6nm.
Instance 6
(1) Resorcinol, formaldehyde, positive tetraethyl orthosilicate, hydrochloric acid, soda ash light, deionized water, absolute ethyl alcohol are mixed for 1:2:1.5:0.13:0.005:8:80 in molar ratio; Under 60 ° of C, stirred 50 minutes; Adding ammoniacal liquor adjusting pH value is 8.8; Carry out sol gel reaction at 60 ° of C and obtained wet gel in 20 minutes, wet gel wore out 5 days under 70 ° of C, and drying obtained the silicon carbide precursor body in 48 hours in 40 ° of C baking ovens then.
(2) silicon carbide precursor body temperature rise rate with 2 ° of C/min under argon shield is heated to 1500 ° of C, is incubated 8 hours, cools the temperature to 600 ° of C then; And argon gas is replaced by air, and be incubated 3 hours to remove residual charcoal, be chilled to room temperature; Take out sample, in 30% hydrofluoric acid aqueous solution, soaked 1 hour then, remove the silicon-dioxide in the silit; After washing, filtration, oven dry, obtain the light green mesoporous silicon carbide.
The pore size distribution of the mesoporous silicon carbide material that makes is 5 ~ 35nm, and specific surface area is 177m
2/ g, median size is 7nm.
Claims (7)
1. the preparation method of a mesoporous silicon carbide material, its concrete steps are following:
(1) Resorcinol, formaldehyde, positive tetraethyl orthosilicate, an acidic catalyst, soda ash light, deionized water, absolute ethyl alcohol are 1:2 in molar ratio: (0.25 ~ 2): (0.04 ~ 0.15): (0.003 ~ 0.01): (1 ~ 8): (20 ~ 160) mix; Stirred 30 ~ 90 minutes down at 50 ~ 70 ℃; Adding ammoniacal liquor adjusting pH value is 7.8 ~ 9.5; Under 50 ~ 70 ° of C, carry out sol gel reaction and obtain wet gel, wet gel obtains the silicon carbide precursor body through the laggard capable drying of overaging;
(2) the silicon carbide precursor body that obtains in the step (1) temperature rise rate with 2 ~ 4 ° of C/min under protection of inert gas is heated to 1450 ~ 1600 ° of C, is incubated 3 ~ 10 hours, cool the temperature to 500 ~ 700 ° of C then; And rare gas element is replaced by air, and be incubated 2 ~ 4 hours to remove residual charcoal, be chilled to; Take out sample; In hydrofluoric acid, soak then, after washing, filtration, oven dry, obtain the light green mesoporous silicon carbide.
2. preparation method according to claim 1 is characterized in that an acidic catalyst described in the step (1) is a kind of in hydrochloric acid or the nitric acid.
3. preparation method according to claim 1 is characterized in that step (1) the sol gel reaction time is 10 ~ 30 minutes.
4. preparation method according to claim 1 is characterized in that aging condition is in the step (1): 50 ~ 75 ° of C wore out 1 ~ 7 day down.
5. preparation method according to claim 1 is characterized in that drying conditions is in the step (1): drying is 24 ~ 48 hours under 40 ~ 60 ° of C.
6. preparation method according to claim 1 is characterized in that the rare gas element described in the step (2) is a kind of in helium or the argon gas.
7. preparation method according to claim 1, the massfraction that it is characterized in that the hydrofluoric acid described in the step (2) is 10 ~ 30%, soak time is 1 ~ 3 hour.
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| CN102897764A (en) * | 2012-10-22 | 2013-01-30 | 南京工业大学 | Bulk silicon carbide aerogel material and preparation method thereof |
| CN105000562B (en) * | 2015-07-31 | 2018-02-13 | 中国计量学院 | A kind of preparation method of carborundum hollow ball |
| CN105000562A (en) * | 2015-07-31 | 2015-10-28 | 中国计量学院 | Preparation method of silicon carbide hollow sphere |
| CN105110334A (en) * | 2015-07-31 | 2015-12-02 | 中国计量学院 | Preparation method for spherical silicon carbide |
| CN105502403A (en) * | 2016-01-14 | 2016-04-20 | 太原理工大学 | Preparation method of ordered mesoporous silicon carbide |
| CN105502403B (en) * | 2016-01-14 | 2017-05-10 | 太原理工大学 | Preparation method of ordered mesoporous silicon carbide |
| CN107416837A (en) * | 2017-05-09 | 2017-12-01 | 武汉科技大学 | A kind of method that porous nano carborundum is prepared using silicate glass as raw material |
| CN107963631A (en) * | 2017-12-12 | 2018-04-27 | 宁波爱克创威新材料科技有限公司 | Nanometer silicon carbide and preparation method thereof |
| CN113149013A (en) * | 2021-04-30 | 2021-07-23 | 天津理工大学 | Method for preparing silicon carbide micron rod |
| CN113149013B (en) * | 2021-04-30 | 2023-05-23 | 天津理工大学 | Method for preparing silicon carbide micron rod |
| CN113224304A (en) * | 2021-05-10 | 2021-08-06 | 浙江辽江新材料有限公司 | Copper-nickel co-doped silicon carbide lithium ion battery negative electrode material and preparation method thereof |
| CN113224304B (en) * | 2021-05-10 | 2022-07-05 | 江西普瑞森新能源科技有限公司 | Copper-nickel co-doped silicon carbide lithium ion battery negative electrode material and preparation method thereof |
| CN114715897A (en) * | 2022-04-19 | 2022-07-08 | 南京航空航天大学 | Size-adjustable SiC @ C mesoporous hollow sphere and preparation method and application thereof |
| CN115072723A (en) * | 2022-07-18 | 2022-09-20 | 陕西煤业化工技术研究院有限责任公司 | Method for preparing nano silicon carbide by sol-gel method |
| CN115072723B (en) * | 2022-07-18 | 2024-02-27 | 陕西煤业化工技术研究院有限责任公司 | Method for preparing nano silicon carbide by sol-gel method |
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