CN119039039A - Preparation method of three-dimensional ordered porous SiC/C with double-layer pore wall structure - Google Patents
Preparation method of three-dimensional ordered porous SiC/C with double-layer pore wall structure Download PDFInfo
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- 239000011148 porous material Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 239000000919 ceramic Substances 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000012298 atmosphere Substances 0.000 claims abstract description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- 238000004132 cross linking Methods 0.000 claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000007598 dipping method Methods 0.000 claims abstract description 4
- 239000010410 layer Substances 0.000 claims description 48
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 238000005530 etching Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002344 surface layer Substances 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 238000007669 thermal treatment Methods 0.000 claims 2
- 238000005516 engineering process Methods 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 238000000151 deposition Methods 0.000 abstract description 7
- 239000002243 precursor Substances 0.000 abstract description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 abstract description 3
- 229910000077 silane Inorganic materials 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 16
- 230000000694 effects Effects 0.000 description 11
- 239000011521 glass Substances 0.000 description 6
- 239000004005 microsphere Substances 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 238000005470 impregnation Methods 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000002077 nanosphere Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021401 carbide-derived carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 239000012229 microporous material Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 239000011225 non-oxide ceramic Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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Abstract
The preparation method of the three-dimensional ordered porous SiC/C with the double-layer pore wall structure comprises the following steps of depositing SiO 2 nanospheres with uniform diameters into a template in a solvent, pouring polymethyl silane dispersion liquid into the template for dipping, thermally crosslinking in inert atmosphere, performing ceramic heat treatment, dipping in hydrofluoric acid, and performing heat treatment in active atmosphere to obtain the three-dimensional ordered porous SiC/C with the double-layer pore wall structure. Compared with the prior art, the preparation method combines the precursor conversion technology, the template technology and the in-situ generation technology of the microporous carbon layer for the first time to prepare the three-dimensional ordered porous material, prepares the three-dimensional ordered porous SiC/C ceramic with a double-layer pore wall structure for the first time, has the advantages of being high in pore wall strength, high in hardness, good in high temperature resistance, large in specific surface area and the like, and is simple in process, convenient to implement and suitable for batch preparation.
Description
Technical Field
The invention relates to a preparation method of three-dimensional ordered porous SiC/C, in particular to a preparation method of three-dimensional ordered porous SiC/C with a double-layer pore wall structure.
Background
If the density of a material is lower than its theoretical density and if the density difference is due to the presence of pores, then the material should be a porous (or apertured) material in a broad sense. The definition of the opening of the pores can be divided into open pore (or through hole) materials and closed pore materials, and the definition of the size of the pores can be divided into macroporous materials (> 50 nm), mesoporous materials (2-50 nm) and microporous materials (< 2 nm). Porous materials have been widely used in daily life and industrial fields, such as molecular sieves, foams, sponges, etc., because of their light weight, heat insulation, adsorption, etc.
Since the nineties of the last century, porous materials have been rapidly developed, and techniques for preparing three-dimensional ordered porous carbon with various pore types and different pore diameters have been successively developed. The material has a three-dimensional ordered pore structure, so that the material has the advantages of super-large specific surface area and super-strong adsorption capacity, and excellent performances in the fields of adsorption, catalysis, hydrogen storage, filtration, separation and the like, but the material has the problems of insufficient temperature resistance and corrosion resistance, weak pore wall strength, small pore diameter, easiness in collapse and blockage of pores and the like, so that the application field and application range of the material are limited. Meanwhile, how to prepare ordered macroporous non-oxide ceramic with larger specific surface area is still a research target of research hotspots and related scientific researchers in the related field.
At present, a plurality of technical methods for preparing holes, such as a foaming method, a template method, a high-energy ion beam or electron beam etching method, an active atmosphere etching method and the like, are established in the field of materials, wherein the active atmosphere etching method is mainly applied to the preparation (Carbide Derived carbon, CDC) of a carbide conversion carbon layer, namely an in-situ generation technology of a microporous carbon layer, for less than twenty years. The limitation of this technique is that only micropores can be prepared, but it is not possible to prepare mesopores, especially macropores.
Disclosure of Invention
The invention aims to solve the technical problems and overcome the defects in the prior art, and provides a preparation method of three-dimensional ordered porous SiC/C with a double-layer pore wall structure, wherein the obtained material has a high specific surface area.
The technical scheme adopted for solving the technical problems is as follows, the preparation method of the three-dimensional ordered porous SiC/C with a double-layer pore wall structure is characterized by comprising the following steps:
(1) Uniformly dispersing SiO 2 nanospheres with uniform diameters in a solvent, self-assembling the naturally deposited SiO 2 nanospheres into a three-dimensional ordered template, removing the solvent and drying, wherein the deposition process can be carried out in a container with a specific shape, the naturally deposited SiO 2 nanospheres form a shape related to the shape of the container, the obtained template is influenced by the shape of the container when the naturally deposited SiO 2 nanospheres are positioned on the macroscopic shape of the finally obtained material, and the shape of the container can be selected according to actual needs;
(2) Pouring polymethyl silane (PMS) dispersion liquid into a container where the template is located, dipping, and removing solvent, wherein when the volume of PMS is equal to that of the template, the production efficiency is the highest, when the volume of PMS is large, the non-pore-forming part exceeding the template can be removed by cutting, grinding and other modes after the material is formed, so that an ideal structure is obtained, and when the volume of PMS is small, the template is not fully utilized, but the obtained material still has the expected structure;
(3) Performing heat crosslinking on the product obtained in the step (2) in an inert atmosphere, and performing heat treatment to ceramic the product;
(4) Soaking the product obtained in the step (3) in hydrofluoric acid, etching the template, and cleaning to obtain 3DOM SiC ceramic, wherein the meaning of 3DOM is a three-dimensional ordered macroporous structure, and the ceramic obtained in the step (4) has the structure, so that the ceramic is named as 3DOM SiC;
(5) And carrying out heat treatment on the 3DOM SiC ceramic under an active atmosphere to remove silicon atoms on the surface layer of the pore wall, and generating a porous carbon layer in situ to obtain the three-dimensional ordered porous SiC/C with a double-layer pore wall structure.
The solvent can be removed by distillation under reduced pressure, and other means of removing the solvent are possible.
By adopting the technical scheme, the three-dimensional ordered porous SiC/C with the double-layer pore wall structure is prepared.
Preferably, in the step (1), ultrasound-assisted SiO 2 nanosphere dispersion is adopted.
By adopting the technical scheme, the SiO 2 nanospheres can be dispersed.
Preferably, in the step (1), the weight ratio of the SiO 2 nanospheres to the solvent is 5-30:100.
By adopting the technical scheme, the method has good dispersing and depositing effects.
Preferably, in step (1), the solvent is absolute ethanol.
The SiO 2 nanospheres in the absolute ethyl alcohol have good dispersibility, the dispersion and natural deposition of the SiO 2 nanospheres are facilitated by adopting the technical scheme, the absolute ethyl alcohol is easy to remove, and other solvents with similar properties can be used.
Preferably, in the step (1), the particle size of the SiO 2 nanospheres is 1000nm or less, more preferably 10 to 800nm.
By adopting the technical scheme, the obtained material has a reasonable pore structure.
Preferably, in step (2), the solvent in the PMS dispersion is Tetrahydrofuran (THF).
The solvent plays a role in dispersing the PMS, the PMS can be dispersed in the dispersion liquid by adopting the technical scheme, and other solvents with similar properties can be used.
Preferably, in step (2), the concentration of PMS dispersion is 10 to 80% (g/g), more preferably 25 to 70% (g/g).
By adopting the technical scheme, the method has a good impregnation effect.
Preferably, in the step (2), the time for impregnation is 5 to 30 hours, more preferably 10 to 25 hours.
By adopting the technical scheme, the method has a good impregnation effect.
Preferably, in the step (3), the temperature at the time of thermal crosslinking is 150-300 ℃, more preferably 160-280 ℃, and the crosslinking time is 2-30 h, more preferably 5-25 h.
By adopting the technical scheme, the PMS can be crosslinked and molded.
Preferably, in the step (3), the temperature of the heat treatment is 800-1650 ℃, more preferably 1000-1600 ℃, and the heat is preserved for 0.5-5 hours, more preferably 0.5-3 hours at the temperature.
By adopting the technical scheme, the ceramic material has a good ceramic effect.
Preferably, in the step (3), the temperature rising rate in the heat treatment is 5 to 50 ℃ per minute, more preferably 10 to 30 ℃.
By adopting the technical scheme, the ceramic material has a good ceramic effect.
Preferably, in step (3), the inert atmosphere is a nitrogen atmosphere. Inert atmospheres are used to provide an environment that does not participate in chemical reactions (particularly oxygen-free), and by employing the above-described techniques, suitable reaction environments can be provided, as well as other atmospheres that achieve this effect are possible.
Preferably, in step (4), the concentration of hydrofluoric acid is 10 to 50% (g/g), more preferably 15 to 30% (g/g).
By adopting the technical scheme, the etching effect is better.
Preferably, in the step (4), the time of the impregnation is 3 to 50 hours, more preferably 10 to 30 hours.
By adopting the technical scheme, the etching effect is better.
Preferably, in the step (5), the temperature of the heat treatment is 400-900 ℃, more preferably 450-800 ℃.
By adopting the technical scheme, the method has a good reaction effect.
Preferably, in the step (5), the time of the heat treatment is 0.1 to 5 hours, more preferably 0.15 to 3 hours.
By adopting the technical scheme, the method has a good reaction effect.
Preferably, in the step (5), the active atmosphere is an atmosphere containing one or more of Cl 2, HCl or F 2.
By adopting the technical scheme, the method has a good reaction effect.
The method comprises the steps of self-assembling silicon dioxide (SiO 2) nanospheres into a three-dimensional ordered microsphere template by adopting a natural deposition technology, impregnating and filling polymethyl silane (PMS) into gaps in the microsphere template under the assistance of a solvent, performing thermal crosslinking and high-temperature inorganic conversion, removing the microsphere template to obtain three-dimensional ordered porous (3 DOM) SiC ceramic, removing silicon atoms on the surface layer of a pore wall by heat treatment of the 3DOM SiC ceramic in an active atmosphere, and simultaneously generating a microporous carbon layer in situ, so as to prepare the three-dimensional ordered porous SiC/C with a double-layer pore wall structure. The method combines a precursor conversion technology, a template technology and an in-situ generation technology of the microporous carbon layer to prepare the 3DOM non-oxidized ceramic material with the double-layer pore wall structure for the first time. The method has the advantages of simple process, convenient implementation and lower cost, and provides a new method and a new technical path for preparing the 3DOM non-oxidized ceramic with large specific surface area.
The invention relates to a double-layer hole wall structure, which is characterized in that a spherical hole wall consists of a SiC layer and a C layer. The SiC layer is derived from the inorganization of the PMS precursor, and Si is removed from the surface of the SiC pore wall by the action of the active gas to form a C layer.
Compared with the prior art, the preparation method has the characteristics and advantages that (1) a precursor conversion technology, a template technology and an in-situ generation technology of a microporous carbon layer are combined for the first time to prepare the three-dimensional ordered porous material, (2) the three-dimensional ordered porous SiC/C ceramic with a double-layer pore wall structure is prepared for the first time, and (3) the material has the advantages of being high in pore wall strength, high in hardness, good in high temperature resistance, large in specific surface area and the like, and the preparation method is simple in process, convenient to implement and suitable for batch preparation.
Drawings
FIG. 1 is a TEM photograph of three-dimensional ordered porous SiC/C with a double-layer pore wall structure obtained in example 2 of the present invention.
FIG. 2 is a TEM photograph of three-dimensional ordered porous SiC/C with a double-layer pore wall structure obtained in example 3 of the present invention.
Detailed Description
The invention is further described below with reference to examples and figures.
The starting materials used in the examples of the present invention were all obtained by conventional commercial means.
Example 1
The preparation method of the three-dimensional ordered porous SiC/C with the double-layer pore wall structure comprises the following steps:
(1) Under the assistance of ultrasound, uniformly dispersing 5g of SiO 2 nanospheres with the particle size of 500nm in 20g of absolute ethyl alcohol (the weight ratio of SiO 2 nanospheres is 25%), then placing the dispersion liquid in a flat-bottom vertical glass tube, self-assembling the SiO 2 nanospheres into a three-dimensional ordered microsphere template through natural deposition, removing a solvent and drying;
(2) 5g of PMS is dissolved in 15g of THF, poured into a glass tube where a small sphere template is located, immersed for 12 hours, and then distilled under reduced pressure to remove the solvent;
(3) Under the protection of high-purity N 2, thermally crosslinking a PMS-impregnated small sphere template at 200 ℃ for 10 hours, heating to 1400 ℃ at a heating rate of 30 ℃ per minute, and preserving heat for 1 hour;
(4) Etching the obtained product in 30% (g/g) hydrofluoric acid for 10 hours to remove the SiO 2 template, cleaning and drying to obtain the 3DOM SiC ceramic, wherein the spherical pore diameter of the ceramic is 470nm, and the BET specific surface area of the ceramic is 235m 2/g;
(5) And (3) carrying out heat treatment on the prepared 3DOM SiC for 10min at 650 ℃ in the Cl 2 atmosphere, removing silicon atoms on the surface layer of the porous SiC pore wall, and generating a porous carbon layer in situ to finally prepare the three-dimensional ordered porous SiC/C with a double-layer pore wall structure.
Through detection, the spherical aperture of the prepared porous SiC/C is 470nm, the aperture of the microporous carbon layer is 0.7nm, and the BET specific surface area is 1206m 2/g.
Example 2
The preparation method of the three-dimensional ordered porous SiC/C with the double-layer pore wall structure comprises the following steps:
(1) Under the assistance of ultrasound, uniformly dispersing 5g of SiO 2 nanospheres with the particle size of 500nm in 20g of absolute ethyl alcohol (the weight ratio of SiO 2 nanospheres is 25%), then placing the dispersion liquid in a flat-bottom vertical glass tube, self-assembling the SiO 2 nanospheres into a three-dimensional ordered microsphere template through natural deposition, removing a solvent and drying;
(2) 5g of PMS is dissolved in 15g of THF, poured into a glass tube where a small sphere template is located, immersed for 12 hours, and then distilled under reduced pressure to remove the solvent;
(3) Under the protection of high-purity N 2, thermally crosslinking a PMS-impregnated small sphere template at 200 ℃ for 10 hours, heating to 1400 ℃ at a heating rate of 30 ℃ per minute, and preserving heat for 1 hour;
(4) Etching the obtained product in 30% (g/g) hydrofluoric acid for 10 hours to remove the SiO 2 template, cleaning and drying to obtain the 3DOM SiC ceramic, wherein the spherical aperture of the ceramic is 470nm;
(5) And (3) carrying out heat treatment on the prepared 3DOM SiC for 15min at 650 ℃ in the Cl 2 atmosphere, removing silicon atoms on the surface layer of the porous SiC pore wall, generating a porous carbon layer in situ, and finally preparing the three-dimensional ordered porous SiC/C with a double-layer pore wall structure.
The electron microscope photograph of the obtained three-dimensional ordered porous SiC/C with the double-layer pore wall structure is shown in figure 1, and the spherical pore diameter is 470nm, the pore diameter of the microporous carbon layer is about 0.7nm, and the BET specific surface area is 1283m 2/g in the prepared porous SiC/C through detection.
Example 3
The preparation method of the three-dimensional ordered porous SiC/C with the double-layer pore wall structure comprises the following steps:
(1) Under the assistance of ultrasound, uniformly dispersing 5g of SiO 2 nanospheres with the particle size of 230nm in 20g of absolute ethyl alcohol (the weight ratio of SiO 2 nanospheres is 25%), then placing the dispersion liquid in a flat-bottom vertical glass tube, self-assembling the SiO 2 nanospheres into a three-dimensional ordered microsphere template through natural deposition, removing a solvent and drying;
(2) 5g of PMS is dissolved in 15g of THF, poured into a glass tube where a small sphere template is located, immersed for 12 hours, and then distilled under reduced pressure to remove the solvent;
(3) Under the protection of high-purity N 2, thermally crosslinking a PMS-impregnated small sphere template at 200 ℃ for 10 hours, heating to 1400 ℃ at a heating rate of 30 ℃ per minute, and preserving heat for 1 hour;
(4) Etching the obtained product in 30% (g/g) hydrofluoric acid for 10 hours to remove the SiO 2 template, cleaning and drying to obtain the 3DOM SiC ceramic, wherein the spherical aperture of the ceramic is 210nm;
(5) And (3) carrying out heat treatment on the prepared 3DOM SiC for 15min at 650 ℃ in the Cl 2 atmosphere, removing silicon atoms on the surface layer of the porous SiC pore wall, generating a porous carbon layer in situ, and finally preparing the three-dimensional ordered porous SiC/C with a double-layer pore wall structure.
The electron microscope photograph of the obtained three-dimensional ordered porous SiC/C with the double-layer pore wall structure is shown as figure 2, and the spherical pore diameter is 210nm, the pore diameter of the microporous carbon layer is about 0.7nm, and the BET specific surface area is 1396m 2/g in the prepared porous SiC/C through detection.
Claims (10)
1. The preparation method of the three-dimensional ordered porous SiC/C with the double-layer pore wall structure is characterized by comprising the following steps of:
(1) Uniformly dispersing SiO 2 nanospheres with uniform diameters in a solvent, self-assembling the naturally deposited SiO 2 nanospheres into a three-dimensional ordered template, removing the solvent and drying;
(2) Pouring the polymethylsilane dispersion liquid into a container where the template is located, dipping, and removing the solvent;
(3) Performing heat crosslinking on the product obtained in the step (2) in an inert atmosphere, and performing heat treatment to ceramic the product;
(4) Soaking the product obtained in the step (3) in hydrofluoric acid, etching the template, and cleaning to obtain 3DOM SiC ceramic;
(5) And carrying out heat treatment on the 3DOM SiC ceramic under an active atmosphere to remove silicon atoms on the surface layer of the pore wall, and generating a porous carbon layer in situ to obtain the three-dimensional ordered porous SiC/C with a double-layer pore wall structure.
2. The method for preparing the three-dimensional ordered porous SiC/C with the double-layer pore wall structure, which is disclosed in claim 1, is characterized in that in the step (1), ultrasonic-assisted SiO 2 nanospheres are adopted for dispersion, and the weight ratio of SiO 2 nanospheres to solvent is 5-30:100.
3. The method for preparing three-dimensional ordered porous SiC/C with a double-layer pore wall structure according to claim 1 or 2, wherein in the step (1), the solvent is absolute ethyl alcohol, and the particle size of the SiO 2 nanospheres is below 1000 nm.
4. The method for preparing three-dimensional ordered porous SiC/C having a double-layer pore wall structure according to any one of claims 1 to 3, wherein in step (2), the solvent in the polymethylsilane dispersion is tetrahydrofuran.
5. The method for preparing three-dimensional ordered porous SiC/C with a double-layer pore wall structure according to any one of claims 1 to 4, wherein in the step (2), the concentration of the polymethylsilane dispersion is 10 to 80%, the unit is g/g, and the soaking time is 5 to 30 hours.
6. The method for preparing the three-dimensional ordered porous SiC/C with the double-layer pore wall structure according to any one of claims 1 to 5, wherein in the step (3), the temperature during thermal crosslinking is 150 to 300 ℃, the crosslinking time is 2 to 30 hours, the temperature during thermal treatment is 800 to 1650 ℃, the temperature is kept for 0.5 to 5 hours at the temperature, and the heating rate during thermal treatment is 5 to 50 ℃ per minute.
7. The method for preparing three-dimensional ordered porous SiC/C having a double-layer pore wall structure according to any one of claims 1 to 6, wherein in step (3), the inert atmosphere is a nitrogen atmosphere.
8. The method for preparing three-dimensional ordered porous SiC/C with a double-layer pore wall structure according to any one of claims 1 to 7, wherein in the step (4), the soaking time is 3 to 50 hours, the concentration of hydrofluoric acid is 10 to 50%, and the unit is g/g.
9. The method for preparing three-dimensional ordered porous SiC/C with a double-layer pore wall structure according to any one of claims 1 to 8, wherein in the step (5), the temperature of the heat treatment is 400 to 900 ℃, and the time of the heat treatment is 0.1 to 5 hours.
10. The method for preparing three-dimensional ordered porous SiC/C having a double-layer pore wall structure according to any one of claims 1 to 9, wherein in step (5), the active atmosphere is an atmosphere containing one or two or more of Cl 2, HCl or F 2.
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