CN102674354B - Preparation method for mesoporous silicon carbide material - Google Patents
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- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 45
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 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 12
- 230000032683 aging Effects 0.000 claims abstract description 11
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- 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
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- 229910052799 carbon Inorganic materials 0.000 claims abstract description 4
- 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
- 239000007789 gas Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
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- 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
- 229960000935 dehydrated alcohol Drugs 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
- 238000003756 stirring Methods 0.000 claims description 8
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- 239000001307 helium Substances 0.000 claims description 2
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
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- 239000013335 mesoporous material Substances 0.000 description 6
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- 229910000029 sodium carbonate Inorganic materials 0.000 description 6
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- 238000002336 sorption--desorption measurement Methods 0.000 description 4
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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
Silicon carbide (SiC) material has many excellent properties such as good thermal conductivity and electroconductibility, resistance to elevated temperatures and chemical stability, shaking property of heat resistanceheat resistant, low thermal coefficient of expansion, high rigidity, in ceramic composite, high-abrasive material, catalyzer and photoelectron material field, has very large application potential.
SiC can be prepared by methods such as traditional Acheson technique, precursor infiltration and pyrolysis method and shape memory synthesis methods, but these synthetic method carbothermic reduction temperature are higher, as the temperature of reaction of Acheson technique at 2000 ° more than C.In addition the porous SiC material granule that, aforesaid method synthesizes and aperture compared with large (generally in micron level), specific surface area is little (is generally no more than 70m
2/ g).Sol-gel method is a kind of effective way of preparing high-specific surface area SiC mesoporous material or nano particle in conjunction with carbo-thermal process, this method first utilizes sol-gel method to synthesize carbon-silica composite as presoma conventionally, 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 larger, as people (Chem.Mater.2010 such as Nicholas Leventis, 22, 2790-2803) a kind of method of utilizing mesoporous SiC prepared by sol-gel method and carbo-thermal process of report, median size is at 7 ~ 17nm, but its specific surface area is lower, be no more than 100m
2/ g.In addition, the preparation technology of current reported SiC presoma is more complicated, mostly need to be by carbon sol and the SiO of preparation respectively
2colloidal sol mixes.
Summary of the invention
The object of the invention is to provide in order to improve the deficiency of prior art existence a kind of preparation method of mesoporous silicon carbide material, the method technique is simple, after directly raw material being mixed, adopt a step sol-gel method to prepare silicon carbide precursor body, 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 as follows:
(1) by Resorcinol, formaldehyde, tetraethyl orthosilicate, an acidic catalyst, anhydrous sodium carbonate, deionized water, dehydrated alcohol, be 1:2:(0.25 ~ 2 in molar ratio): (0.04 ~ 0.15): (0.003 ~ 0.01): (1 ~ 8): (20 ~ 160) mix, at 50 ~ 70 ℃, stir 30 ~ 90 minutes, adding ammoniacal liquor to regulate pH value is 7.8 ~ 9.5, under 50 ~ 70 ° of C, carry out sol gel reaction and obtain wet gel, wet gel obtains silicon carbide precursor body through the laggard row constant pressure and dry of overaging;
(2) the silicon carbide precursor body obtaining in step (1) temperature rise rate with 2 ~ 4 ° of C/min under protection of inert gas is heated to 1450 ~ 1600 ° of C; be incubated 3 ~ 10 hours; then cool the temperature to 500 ~ 700 ° of C; 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; then in hydrofluoric acid, soak and remove silicon-dioxide, after washing, filtration, drying, obtain light green mesoporous silicon carbide.
An acidic catalyst described in preferred steps (1) is a kind of in hydrochloric acid or nitric acid.
Preferred steps (1) the sol gel reaction time is 10 ~ 30 minutes; Aging condition is in step (1): under 50 ~ 75 ° of C aging 1 ~ 7 day; In step (1), drying conditions is: under 40 ~ 60 ° of C, be dried 24 ~ 48 hours.
Rare gas element described in preferred steps (2) is a kind of in helium or argon gas.The massfraction of the hydrofluoric acid described in preferred steps (2) is 10 ~ 30%, and soak time is 1 ~ 3 hour.
Mesoporous silicon carbide material prepared by the present invention can be for fields such as catalystic material, ceramic composite, high-abrasive material, photoelectron material and high temperature insulating materials.
Beneficial effect:
Mesoporous silicon carbide material prepared by the inventive method has following features:
(1) raw material is cheap and easy to get, and equipment is simple, easily realizes scale production.
(2) silicon-carbide particle size and being evenly distributed, has typical meso-hole structure feature.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the mesoporous silicon carbide material that makes of example 2.
Fig. 2 is the HRTEM photo of the mesoporous silicon carbide material that makes of example 2.
Fig. 3 is the SEM photo of the mesoporous silicon carbide material that makes of example 2.
Fig. 4 is the nitrogen adsorption desorption curve of the mesoporous silicon carbide material that makes of example 2, wherein ● and zero be respectively adsorption curve and desorption curve.
Embodiment
Example 1
(1) by Resorcinol, formaldehyde, tetraethyl orthosilicate, hydrochloric acid, anhydrous sodium carbonate, deionized water, dehydrated alcohol in molar ratio for 1:2:1.5:0.06:0.008:6:100 mixes, under 50 ° of C, stir 90 minutes, adding ammoniacal liquor to regulate pH value is 7.8, at 60 ° of C, carry out sol gel reaction and within 20 minutes, obtain wet gel, wet gel under 70 ° of C aging 3 days, the then dry silicon carbide precursor body that obtains for 36 hours in 50 ° of C baking ovens.
(2) silicon carbide precursor body temperature rise rate with 4 ° of C/min under argon shield is heated to 1600 ° of C; be incubated 3 hours; then cool the temperature to 500 ° of C, and argon gas is replaced by air, be incubated 4 hours to remove residual charcoal; be chilled to room temperature; take out sample, then in 30% hydrofluoric acid aqueous solution, soak 1 hour, remove the silicon-dioxide in silicon carbide; after washing, filtration, drying, obtain light green mesoporous silicon carbide.
The pore size distribution of the mesoporous silicon carbide material making is 5 ~ 26nm, and specific surface area is 196m
2/ g, median size is 6.5nm.
Example 2
(1) by Resorcinol, formaldehyde, tetraethyl orthosilicate, hydrochloric acid, anhydrous sodium carbonate, deionized water, dehydrated alcohol in molar ratio for 1:2:1:0.09:0.01:4:120 mixes, under 60 ° of C, stir 60 minutes, adding ammoniacal liquor to regulate pH value is 8.5, at 60 ° of C, carry out sol gel reaction and within 30 minutes, obtain wet gel, wet gel under 75 ° of C aging 5 days, the then dry silicon carbide precursor body that obtains for 48 hours in 40 ° of C baking ovens.
(2) silicon carbide precursor body temperature rise rate with 2 ° of C/min under argon shield is heated to 1500 ° of C; be incubated 6 hours; then cool the temperature to 600 ° of C, and argon gas is replaced by air, be incubated 3 hours to remove residual charcoal; be chilled to room temperature; take out sample, then in 20% hydrofluoric acid aqueous solution, soak 2 hours, remove the silicon-dioxide in silicon carbide; after washing, filtration, drying, obtain light green mesoporous silicon carbide.
The pore size distribution of the mesoporous silicon carbide material making is 4 ~ 13nm, and BET specific surface area is 366m
2/ g, median size is 5.2nm.
The XRD figure spectrum of the prepared silicon carbide mesoporous material of this example as shown in Figure 1.XRD analysis is carried out on the ARLX'TRA of Arl Inc. of Thermo Electron Corp. type X-ray diffraction instrument; Adopt CuK α diffraction, λ=0.15406nm, scanning speed 2 (°)/min, scanning angle 10 ~ 80 degree.As can be seen from Figure 1, the mesoporous silicon carbide of preparation is β-SiC, and according to Scherrer formula, can calculate corresponding median size is 5.2nm.
The HRTEM photo of the prepared silicon carbide mesoporous material of this example as shown in Figure 2.Tem analysis adopts the JEM-2010 of NEC company type transmission electron microscope.From the HRTEM photo of sample, can find out, the mesoporous silicon carbide of preparation has the spacing of 0.252nm, consistent with the spacing of (111) crystal face of β-SiC, and this silicon carbide that also shows preparation is β-SiC.
The SEM photo of the prepared silicon carbide mesoporous material of this example as shown in Figure 3.SEM test adopts the German LEO-1530VP of Carl Zeiss Inc. field emission scanning electron microscope.From SEM photo, can find out, silicon carbide mesoporous material granular size prepared by the present invention, be evenly distributed.
The nitrogen adsorption desorption curve of the prepared silicon carbide mesoporous material of this example as shown in Figure 4.The test of nitrogen adsorption desorption adopts the full-automatic specific surface area analysis instrument of the U.S. ASAP2020 of Micromeritics company type.As can be seen from the figure, the carbofrax material of preparation has typical meso-hole structure feature, and the BET specific surface area that the data by adsorption desorption curve can calculate sample is 366m
2/ g.
Example 3
(1) by Resorcinol, formaldehyde, tetraethyl orthosilicate, nitric acid, anhydrous sodium carbonate, deionized water, dehydrated alcohol in molar ratio for 1:2:0.5:0.04:0.003:1:20 mixes, under 60 ° of C, stir 30 minutes, adding ammoniacal liquor to regulate pH value is 8.5, at 50 ° of C, carry out sol gel reaction and within 10 minutes, obtain wet gel, wet gel under 50 ° of C aging 3 days, the then dry silicon carbide precursor body that obtains for 36 hours in 50 ° of C baking ovens.
(2) silicon carbide precursor body temperature rise rate with 2 ° of C/min under argon shield is heated to 1450 ° of C; be incubated 10 hours; then cool the temperature to 600 ° of C, and argon gas is replaced by air, be incubated 3 hours to remove residual charcoal; be chilled to room temperature; take out sample, then in 10% hydrofluoric acid aqueous solution, soak 3 hours, remove the silicon-dioxide in silicon carbide; after washing, filtration, drying, obtain light green mesoporous silicon carbide.
The pore size distribution of the mesoporous silicon carbide material making is 25 ~ 35nm, and specific surface area is 173m
2/ g, median size is 6.9nm.
Example 4
(1) by Resorcinol, formaldehyde, tetraethyl orthosilicate, hydrochloric acid, anhydrous sodium carbonate, deionized water, dehydrated alcohol in molar ratio for 1:2:1:0.15:0.004:2:160 mixes, under 70 ° of C, stir 30 minutes, adding ammoniacal liquor to regulate pH value is 9.5, at 70 ° of C, carry out sol gel reaction and within 30 minutes, obtain wet gel, wet gel under 75 ° of C aging 7 days, the then dry silicon carbide precursor body that obtains for 24 hours in 60 ° of C baking ovens.
(2) silicon carbide precursor body temperature rise rate with 2 ° of C/min under argon shield is heated to 1500 ° of C; be incubated 4 hours; then cool the temperature to 500 ° of C, and argon gas is replaced by air, be incubated 4 hours to remove residual charcoal; be chilled to room temperature; take out sample, then in 20% hydrofluoric acid aqueous solution, soak 2 hours, remove the silicon-dioxide in silicon carbide; after washing, filtration, drying, obtain light green mesoporous silicon carbide.
The pore size distribution of the mesoporous silicon carbide material making is 5 ~ 25nm, and specific surface area is 298m
2/ g, median size is 4.7nm.
Example 5
(1) by Resorcinol, formaldehyde, tetraethyl orthosilicate, nitric acid, anhydrous sodium carbonate, deionized water, dehydrated alcohol in molar ratio for 1:2:1:0.1:0.006:2:40 mixes, under 50 ° of C, stir 60 minutes, adding ammoniacal liquor to regulate pH value is 8.2, at 50 ° of C, carry out sol gel reaction and within 25 minutes, obtain wet gel, wet gel under 60 ° of C aging 1 day, the then dry silicon carbide precursor body that obtains for 36 hours in 50 ° of C baking ovens.
(2) silicon carbide precursor body temperature rise rate with 3 ° of C/min under argon shield is heated to 1550 ° of C; be incubated 6 hours; then cool the temperature to 700 ° of C, and argon gas is replaced by air, be incubated 2 hours to remove residual charcoal; be chilled to room temperature; take out sample, then in 10% hydrofluoric acid aqueous solution, soak 3 hours, remove the silicon-dioxide in silicon carbide; after washing, filtration, drying, obtain light green mesoporous silicon carbide.
The pore size distribution of the mesoporous silicon carbide material making is 10 ~ 30nm, and specific surface area is 221m
2/ g, median size is 5.6nm.
Example 6
(1) by Resorcinol, formaldehyde, tetraethyl orthosilicate, hydrochloric acid, anhydrous sodium carbonate, deionized water, dehydrated alcohol in molar ratio for 1:2:1.5:0.13:0.005:8:80 mixes, under 60 ° of C, stir 50 minutes, adding ammoniacal liquor to regulate pH value is 8.8, at 60 ° of C, carry out sol gel reaction and within 20 minutes, obtain wet gel, wet gel under 70 ° of C aging 5 days, the then dry silicon carbide precursor body that obtains for 48 hours in 40 ° of C baking ovens.
(2) silicon carbide precursor body temperature rise rate with 2 ° of C/min under argon shield is heated to 1500 ° of C; be incubated 8 hours; then cool the temperature to 600 ° of C, and argon gas is replaced by air, be incubated 3 hours to remove residual charcoal; be chilled to room temperature; take out sample, then in 30% hydrofluoric acid aqueous solution, soak 1 hour, remove the silicon-dioxide in silicon carbide; after washing, filtration, drying, obtain light green mesoporous silicon carbide.
The pore size distribution of the mesoporous silicon carbide material making is 5 ~ 35nm, and specific surface area is 177m
2/ g, median size is 7nm.
Claims (7)
1. a preparation method for mesoporous silicon carbide material, its concrete steps are as follows:
(1) by Resorcinol, formaldehyde, tetraethyl orthosilicate, an acidic catalyst, anhydrous sodium carbonate, deionized water, dehydrated alcohol, be 1:2:(0.25～2 in molar ratio): (0.04～0.15): (0.003～0.01): (1～8): (20～160) mix, at 50～70 ℃, stir 30～90 minutes, adding ammoniacal liquor to regulate pH value is 7.8～9.5, at 50～70 ℃, carry out sol gel reaction and obtain wet gel, wet gel is through the dry silicon carbide precursor body that obtains of the laggard row of overaging;
(2) the silicon carbide precursor body obtaining in step (1) temperature rise rate with 2～4 ℃/min under protection of inert gas is heated to 1450～1600 ℃; be incubated 3～10 hours; then cool the temperature to 500～700 ℃; and rare gas element is replaced by air, and be incubated 2～4 hours to remove residual charcoal, be cooled to room temperature; take out sample; then in hydrofluoric acid, soak, after washing, filtration, drying, obtain light green mesoporous silicon carbide.
2. preparation method according to claim 1, is characterized in that an acidic catalyst described in step (1) is a kind of in hydrochloric acid or 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 in step (1), aging condition is: at 50～75 ℃ aging 1～7 day.
5. preparation method according to claim 1, is characterized in that in step (1), drying conditions is: at 40～60 ℃, be dried 24～48 hours.
6. preparation method according to claim 1, is characterized in that the rare gas element described in step (2) is a kind of in helium or argon gas.
7. preparation method according to claim 1, the massfraction that it is characterized in that the hydrofluoric acid described in step (2) is 10～30%, soak time is 1～3 hour.
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