Carbon-silicon composite chiral mesoporous heterojunction film MCSC / AAO and preparation method thereof
By preparing a carbon-silicon composite chiral mesoporous heterojunction membrane MCSC/AAO, the problems of irregular pore structure and pore size adjustment in nanochannel membrane materials were solved, enabling rapid transport and energy conversion of ions and molecules.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-01-16
- Publication Date
- 2026-04-14
AI Technical Summary
Existing nanochannel membrane materials suffer from low pore structure regularity and difficulty in adjusting pore size, which hinders the transport of ions and molecules.
A carbon-silicon composite chiral mesoporous heterojunction membrane MCSC/AAO was used to prepare a membrane material with regular nanopores and adjustable thickness by combining a chiral template with an anodic aluminum oxide membrane through interfacial superassembly. The carbon-silicon composite chiral mesoporous material was prepared by hydrothermal method and calcination process.
It enables rapid and selective transport of ions and molecules, and provides membrane materials with regular channels, controllable thickness and asymmetric charge distribution, supporting the application of nanofluidic membrane devices in energy capture.
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Figure CN116036884B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of membrane science and technology, specifically relating to a carbon silicon composite chiral mesoporous heterojunction membrane MCSC / AAO and its preparation method. Background Technology
[0002] Learning from nature is a perpetual theme in the development of intelligent new materials and systems. Drawing inspiration from the energy conversion principles of biological ion channels (such as electric eel discharge), and mimicking the efficient energy conversion in living systems in both principle and structure, this research utilizes a comprehensive approach combining nanotechnology, molecular biology, and interface chemistry. Through the design of energy-producing materials and the assembly of conversion devices, the conversion between different energy forms—salinity gradient energy and electrical energy—is achieved, providing new ideas, methods, and theories for future energy development technologies. However, currently reported nanochannels still face many challenges, such as low pore structure regularity and difficulty in adjusting pore size, both of which hinder the transport of ions and molecules to some extent. Addressing the current bottlenecks in the field of nanochannel membrane materials, there is an urgent need to develop membrane materials with regular nanopores and adjustable thickness for the rapid and selective transport of specific ions and molecules. Summary of the Invention
[0003] This invention is made to solve the above-mentioned problems, and its purpose is to provide a carbon silicon composite chiral mesoporous heterojunction film MCSC / AAO and its preparation method.
[0004] The present invention provides a silicon carbide composite chiral mesoporous heterojunction membrane MCSC / AAO, characterized by comprising: an anodic aluminum oxide film and a silicon carbide composite chiral mesoporous thin film layer covering the anodic aluminum oxide film, wherein the anodic aluminum oxide film is positively charged in water, and the silicon carbide composite chiral mesoporous thin film layer is negatively charged in water.
[0005] The present invention also provides a carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO, which has the following features: uniformly dispersing the carbon-silicon composite chiral mesoporous nanocomposite material in an aqueous solution, using interfacial superassembly to tightly bond it with an anodic aluminum oxide array at the interface, removing the solvent by filtration and drying to obtain the carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO.
[0006] The carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO provided by the present invention may also have the following characteristics: wherein the carbon-silicon composite chiral mesoporous nanocomposite material is prepared by hydrothermal method using guanylic acid as a template agent.
[0007] The carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO provided by the present invention may also have the following characteristics: the preparation process of the carbon-silicon composite chiral mesoporous nanocomposite material includes: carrying out a hydrothermal reaction of a mixed solution of guanylic acid, potassium chloride, 3-aminopropyltriethoxysilane, concentrated hydrochloric acid, tetraethyl orthosilicate and soluble phenolic resin in a hydrothermal reactor, and then calcining it in an inert atmosphere to obtain the carbon-silicon composite chiral mesoporous nanocomposite material.
[0008] The carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO provided by this invention may also have the following characteristics: the preparation process of the carbon-silicon composite chiral mesoporous nanomaterial specifically includes the following steps: Step 1, guanylic acid and potassium chloride are simultaneously dispersed or dissolved in deionized water, 37% concentrated hydrochloric acid and 3-aminopropyltriethoxysilane are added under stirring conditions, stirring is continued, and tetraethyl orthosilicate and soluble phenolic resin are added dropwise, and stirring is carried out at room temperature for a period of time; Step 2, the mixed solution obtained in Step 1 is transferred to a hydrothermal reactor for hydrothermal reaction, and then filtered and dried to obtain a chiral carbon-silicon composite material with a template; Step 3, the chiral carbon-silicon composite material with the template is added to a mixed solution of concentrated hydrochloric acid and anhydrous ethanol and heated, and then filtered and dried to obtain a chiral carbon-silicon composite mesoporous material with the template removed and the amino-modified inner surface removed; Step 4, the chiral carbon-silicon composite mesoporous material obtained in Step 3 is calcined in an inert gas to obtain the carbon-silicon composite chiral mesoporous nanomaterial.
[0009] The carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO provided by this invention may also have the following characteristics: in step 1, the molar ratio of tetraethyl orthosilicate to soluble phenolic resin is 1:0.75, the mass-to-volume ratio of guanylic acid to 3-aminopropyltriethoxysilane is (0.4-0.7) g:(0.70-1.00) ml, the mass-to-volume ratio of guanylic acid to tetraethyl orthosilicate is (0.4-0.7) g:(0.79-1.12) ml, and the mass-to-volume ratio of guanylic acid to concentrated hydrochloric acid is (0.4-0.7) g:(0.12-0.26) ml.
[0010] The carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO provided by the present invention may also have the following characteristics: in step 3, the concentrated hydrochloric acid and anhydrous ethanol mixed solution is 37% concentrated hydrochloric acid, and the volume ratio of concentrated hydrochloric acid to anhydrous ethanol is 3:7.
[0011] The carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO provided by the present invention may also have the following characteristics: wherein, in step 2, the hydrothermal reaction temperature is 80℃~120℃ and the reaction time is 24h~120h.
[0012] The carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO provided by the present invention may also have the following characteristics: wherein, in step 4, the calcination temperature is 500℃~1000℃ and the calcination time is 3h~5h.
[0013] The carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO provided by the present invention may also have the following characteristics: wherein the process of uniformly dispersing the carbon-silicon composite chiral mesoporous nanomaterial in a deionized aqueous solution includes: ultrasonically dispersing the carbon-silicon composite chiral mesoporous nanomaterial in an ethanol mixture of anhydrous ethanol and deionized water.
[0014] The role and effect of invention
[0015] The present invention relates to a carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO and its preparation method. Firstly, a chiral template is transcribed onto the inner surface of carbon-silicon composite nanopores via self-assembly and co-assembly. The chiral template is then removed through acid washing and high-temperature calcination, yielding a chiral mesoporous material with a chiral pore inner surface. Next, using an interfacial superassembly method, the material is filtered onto the AAO surface via fluid-directed induction, resulting in a carbon-silicon composite chiral mesoporous heterojunction membrane with an ordered pore structure and adjustable thickness. This heterojunction membrane possesses an asymmetric chemical composition, an asymmetric pore structure, an asymmetric pore surface charge distribution, and a carbon-silicon composite component that enhances electrical properties. These asymmetric elements and composite components endow the heterojunction membrane with considerable application potential in the fields of chiral recognition and sieving.
[0016] Furthermore, the MCSC / AAO heterojunction membrane with adjustable pore size, controllable thickness, typical surface enhancement, and regular channels prepared by the interfacial super-assembly strategy of this invention provides reliable technical support for the development of membrane science and also provides a new material for energy capture in nanofluidic membrane devices. Attached Figure Description
[0017] Figure 1 This is a transmission electron microscope (TEM) image of the carbon-silicon composite chiral mesoporous nanocomposite material prepared in Example 1 of the present invention;
[0018] Figure 2 The nitrogen adsorption-desorption curve of the carbon-silicon composite chiral mesoporous nanocomposite material prepared in Example 1 of the present invention is shown.
[0019] Figure 3 This is the pore size distribution curve of the carbon-silicon composite chiral mesoporous nanocomposite material prepared in Example 1 of the present invention;
[0020] Figure 4This is a surface scanning electron microscope (SEM) image of the carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO prepared in Example 1 of the present invention;
[0021] Figure 5 This is a cross-sectional scanning electron microscope (SEM) image of the carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO prepared in Example 1 of the present invention;
[0022] Figure 6 This is a graph showing the variation of the salinity gradient power generation performance of a carbon-silicon composite chiral mesoporous heterojunction membrane (MCSC / AAO) with carbon-silicon composite chiral mesoporous thin film layers of different thicknesses in Embodiment 1 of the present invention.
[0023] Figure 7 Fourier transform infrared absorption spectra of the chiral carbon-silicon composite mesoporous material and the carbon-silicon composite chiral mesoporous nanocomposite material prepared in Example 1 of the present invention.
[0024] Figure 8 This is a contact angle test diagram of the carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO prepared in Example 1 of the present invention. Detailed Implementation
[0025] To make the technical means, creative features, objectives and effects of the present invention easy to understand, the following embodiments, in conjunction with the accompanying drawings, specifically illustrate the carbon silicon composite chiral mesoporous heterojunction membrane MCSC / AAO and its preparation method.
[0026] <Example 1>
[0027] Example 1 provides a carbon silicon composite chiral mesoporous heterojunction membrane MCSC / AAO and its preparation method.
[0028] The preparation method of silicon carbide composite chiral mesoporous heterojunction film MCSC / AAO specifically includes the following steps:
[0029] 1) Weigh 0.6g of guanylic acid white powder and 0.22g of potassium chloride solid powder using an analytical balance, then disperse or dissolve them in about 21ml of deionized water solution, and stir at 300 rpm for about 1 hour on a magnetic stirrer to obtain the first mixed solution;
[0030] 2) Measure 0.24 mL of 37% concentrated hydrochloric acid and add it to the first mixed solution above, which is stirred continuously, to obtain the second mixed solution;
[0031] 3) Measure 0.95 ml of 3-aminopropyltriethoxysilane (APTES) and add it to the second mixed solution above while stirring continuously to obtain the third mixed solution;
[0032] 4) Then measure 1.11 ml of tetraethyl orthosilicate (TEOS), slowly add TEOS dropwise to the above third mixed solution, stir at room temperature for 30 min to obtain the fourth mixed solution;
[0033] 5) Measure 0.83 mL of soluble phenolic resin and add it to the fourth mixed solution above. Stir at room temperature for 12 h to obtain the fifth mixed solution.
[0034] 6) Transfer the above fifth mixed solution to a hydrothermal reactor and place it in an oven at 100°C for hydrothermal reaction for 48 hours to obtain the sixth mixed solution;
[0035] 7) Filter the above sixth mixed solution through a Buchner funnel;
[0036] 8) Place the sample filtered in step 7) in a room temperature environment for 24 hours to allow the sample to dry naturally, and obtain the first dried sample;
[0037] 9) Prepare a mixed solution of 37% concentrated hydrochloric acid and anhydrous ethanol in a 3:7 ratio, and set aside for later use;
[0038] 10) Weigh 0.5g of the first dried sample and add it to the above-prepared mixed solution of concentrated hydrochloric acid and anhydrous ethanol according to the ratio (add 10ml of mixed solution for every 0.1g of sample) to obtain the seventh mixed solution;
[0039] 11) Transfer the above seventh mixed solution to an oil bath and incubate at 60°C for 12 hours to obtain the eighth mixed solution;
[0040] 12) Filter the above eighth mixed solution through a Buchner funnel;
[0041] 13) Place the sample filtered in step 12) in a room temperature environment for 24 hours to allow the sample to dry naturally, and obtain a second dried sample. The second dried sample is a chiral carbon silicon composite mesoporous material with the amino-modified inner surface removed from the template.
[0042] 14) The second dried sample was calcined at 800°C for 3 hours under a nitrogen atmosphere to obtain a carbon-silicon composite chiral mesoporous nanocomposite material.
[0043] 15) Prepare an ethanol mixture of anhydrous ethanol and deionized water in a 2:5 ratio;
[0044] 16) Tightly adhere the anodized aluminum oxide membrane (AAO substrate) to the surface of the filtration device and set up the filtration device;
[0045] 17) The carbon-silicon composite chiral mesoporous nanocomposite material was dispersed in the above ethanol mixed solution to obtain the ninth mixed solution;
[0046] 18) The above ninth mixed solution is ultrasonically vibrated to uniformly disperse the nanomaterials in the solution, thus obtaining a dispersion solution;
[0047] 19) The above dispersion solution is filtered onto the AAO substrate through the above filtration device to obtain the final carbon silicon composite chiral mesoporous heterojunction membrane MCSC / AAO with a carbon silicon composite chiral channel structure.
[0048] Figure 1 This is a transmission electron microscope (TEM) image of the carbon-silicon composite chiral mesoporous nanocomposite material prepared in Example 1 of the present invention. As can be seen from the TEM image, the carbon-silicon composite chiral mesoporous nanocomposite material prepared in Example 1 has a regular mesoporous channel structure.
[0049] Figure 2 This is the nitrogen adsorption-desorption curve of the carbon-silicon composite chiral mesoporous nanocomposite material prepared in Example 1 of the present invention. Figure 2 The nitrogen adsorption-desorption curves show that the adsorption and desorption curves almost overlap within a narrow pressure range, indicating that the carbon-silicon composite chiral mesoporous nanocomposite material prepared in Example 1 has a narrow pore size distribution structure.
[0050] Figure 3 This is the pore size distribution curve of the carbon-silicon composite chiral mesoporous nanocomposite material prepared in Example 1 of the present invention. The pore size distribution curve is obtained through the desorption value ( Figure 3 It can be seen that the pore size of the carbon-silicon composite chiral mesoporous nanocomposite is approximately 2.4 nm.
[0051] Figure 4 This is a surface scanning electron microscope (SEM) image of the carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO prepared in Example 1 of the present invention; Figure 5 This is a cross-sectional scanning electron microscope (SEM) image of the carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO prepared in Example 1 of this invention. Figure 4 As can be seen, the carbon-silicon composite chiral mesoporous nanocomposite material is flat and completely covered on the AAO substrate, from Figure 5 As can be seen, the carbon-silicon composite chiral mesoporous nanocomposite material is tightly adsorbed on the upper layer of AAO, forming a carbon-silicon composite chiral mesoporous thin film layer with a thickness of about 70 μm.
[0052] Figure 6 This is a graph showing the variation in MCSC / AAO salinity gradient power generation performance of carbon-silicon composite chiral mesoporous heterojunction films with different thicknesses of carbon-silicon composite chiral mesoporous thin film layers in Embodiment 1 of the present invention. Figure 6As shown, this embodiment also investigated the variation of salinity gradient power generation performance of carbon-silicon composite chiral mesoporous heterojunction films (MCSC / AAO) prepared by loading carbon-silicon composite chiral mesoporous nanocomposites of different thicknesses. Figure 6 As can be seen, with the increase of filtration loading, the thickness of the silicon carbide composite chiral mesoporous film layer increases, and the salinity gradient of the silicon carbide composite chiral mesoporous heterojunction membrane MCSC / AAO first gradually increases and then slowly decreases. Therefore, in the final optimized scheme, the silicon carbide composite chiral mesoporous heterojunction membrane MCSC / AAO includes a 60 μm thick positively charged AAO layer and a 70 μm thick negatively charged silicon carbide composite chiral mesoporous material.
[0053] Figure 7 These are the Fourier transform infrared absorption spectra of the chiral carbon-silicon composite mesoporous material and the carbon-silicon composite chiral mesoporous nanocomposite material prepared in Example 1 of this invention. Figure 7 As can be seen, the chiral silicon carbide composite mesoporous material (MCSC in the figure) obtained in step 13) has a pore size of 1480 cm⁻¹. -1 and 687cm -1 The peaks at the points correspond to the bands of NH stretching and bending vibrations, respectively, indicating that -NH2 groups exist in the inner wall of the pores of the synthesized material. However, the carbon-silicon composite chiral mesoporous nanocomposite material (asy MCSC in the figure) obtained after calcination in step 14) does not have the above two peaks, indicating that calcination can completely remove APTES and guanylic acid template.
[0054] Figure 8 This is a contact angle test diagram of the carbon-silicon composite chiral mesoporous heterojunction film MCSC / AAO prepared in Example 1 of the present invention. Figure 8 It can be seen that the synthesized carbon-silicon composite chiral mesoporous heterojunction membrane MCSC / AAO is still a hydrophilic material.
[0055] The carbon-silicon composite chiral mesoporous heterojunction membrane (MCSC / AAO) prepared in this embodiment comprises a 60 μm thick positively charged AAO and a 70 μm thick negatively charged carbon-silicon composite chiral mesoporous nanocomposite material. Compared with other nanochannel membranes, this heterojunction membrane exhibits high mechanical stability, a well-ordered pore structure, adjustable membrane thickness, and uniform composite composition. These advantages significantly reduce the internal resistance of ion transport, which is beneficial for the application of heterojunction membranes in energy conversion.
[0056] <Example 2>
[0057] Example 2 provides a carbon silicon composite chiral mesoporous heterojunction membrane MCSC / AAO and its preparation method.
[0058] The preparation method of silicon carbide composite chiral mesoporous heterojunction film MCSC / AAO specifically includes the following steps:
[0059] 1) Weigh 0.5g of white guanylic acid powder and 0.26g of solid potassium chloride powder using an analytical balance, then disperse or dissolve them in about 21ml of deionized water solution, and stir at 300 rpm for about 1 hour on a magnetic stirrer to obtain the first mixed solution;
[0060] 2) Measure 0.22 mL of 37% concentrated hydrochloric acid and add it to the first mixed solution above, which is stirred continuously, to obtain the second mixed solution;
[0061] 3) Measure 1.00 ml of 3-aminopropyltriethoxysilane (APTES) and add it to the second mixed solution above while stirring continuously to obtain the third mixed solution;
[0062] 4) Then measure 1.30 ml of tetraethyl orthosilicate (TEOS), slowly add TEOS dropwise to the above third mixed solution, stir at room temperature for 1 hour to obtain the fourth mixed solution;
[0063] 5) Measure 1.00 mL of soluble phenolic resin and add it to the fourth mixed solution above. Stir at room temperature for 12 h to obtain the fifth mixed solution.
[0064] 6) Transfer the above fifth mixed solution to a hydrothermal reactor and place it in an oven at 100°C for hydrothermal reaction for 72 hours to obtain the sixth mixed solution;
[0065] 7) Filter the above sixth mixed solution through a Buchner funnel;
[0066] 8) Place the sample filtered in step 7) in a room temperature environment for 24 hours to allow the sample to dry naturally, and obtain the first dried sample;
[0067] 9) Prepare a mixed solution of 37% concentrated hydrochloric acid and anhydrous ethanol in a 3:7 ratio, and set aside for later use;
[0068] 10) Weigh 0.5g of the first dried sample and add it to the above-prepared concentrated hydrochloric acid and anhydrous ethanol mixed solution according to the ratio (add 10ml of mixed solution for every 0.1 sample) to obtain the seventh mixed solution;
[0069] 11) Transfer the above seventh mixed solution to an oil bath and incubate at 60°C for 12 hours to obtain the eighth mixed solution;
[0070] 12) Filter the above eighth mixed solution through a Buchner funnel;
[0071] 13) Place the sample filtered in step 12) in a room temperature environment for 24 hours to allow the sample to dry naturally, and obtain a second dried sample. The second dried sample is a chiral carbon silicon composite mesoporous material with the amino-modified inner surface removed from the template.
[0072] 14) The second dried sample was calcined at 900°C for 3 hours under a nitrogen atmosphere to obtain a carbon-silicon composite chiral mesoporous nanocomposite material.
[0073] 15) Prepare an ethanol mixture of anhydrous ethanol and deionized water in a 2:5 ratio;
[0074] 16) Fit the AAO substrate tightly onto the surface of the filtration device and set up the filtration device.
[0075] 17) The carbon-silicon composite chiral mesoporous nanocomposite material was dispersed in the above ethanol mixed solution to obtain the ninth mixed solution;
[0076] 18) The above ninth mixed solution is ultrasonically vibrated to uniformly disperse the nanomaterials in the solution, thus obtaining a dispersion solution;
[0077] 19) The above dispersion solution is filtered onto the AAO substrate through the above filtration device to obtain the final carbon silicon composite chiral mesoporous heterojunction membrane MCSC / AAO with a carbon silicon composite chiral channel structure.
[0078] <Example 3>
[0079] Example 3 provides a carbon silicon composite chiral mesoporous heterojunction membrane MCSC / AAO and its preparation method.
[0080] The preparation method of silicon carbide composite chiral mesoporous heterojunction film MCSC / AAO specifically includes the following steps:
[0081] 1) Weigh 0.65g of guanylic acid white powder and 0.20g of potassium chloride solid powder using an analytical balance, then disperse or dissolve them in about 21ml of deionized water solution, and stir at 300 rpm for about 1 hour on a magnetic stirrer to obtain the first mixed solution;
[0082] 2) Measure 0.20 mL of 37% concentrated hydrochloric acid and add it to the first mixed solution above, which is stirred continuously, to obtain the second mixed solution;
[0083] 3) Measure 1.10 ml of 3-aminopropyltriethoxysilane (APTES) and add it to the second mixed solution above while stirring continuously to obtain the third mixed solution;
[0084] 4) Then measure 1.30 ml of tetraethyl orthosilicate (TEOS), slowly add TEOS dropwise to the above third mixed solution, stir at room temperature for 1 hour to obtain the fourth mixed solution;
[0085] 5) Measure 1.30 mL of soluble phenolic resin and add it to the fourth mixed solution above. Stir at room temperature for 12 h to obtain the fifth mixed solution.
[0086] 6) Transfer the above fifth mixed solution to a hydrothermal reactor and place it in an oven at 100°C for hydrothermal reaction for 96 hours to obtain the sixth mixed solution;
[0087] 7) Filter the above sixth mixed solution through a Buchner funnel;
[0088] 8) Place the sample filtered in step 7) in a room temperature environment for 24 hours to allow the sample to dry naturally, and obtain the first dried sample;
[0089] 9) Prepare a mixed solution of 37% concentrated hydrochloric acid and anhydrous ethanol in a 3:7 ratio, and set aside for later use;
[0090] 10) Weigh 0.5g of the first dried sample and add it to the above-prepared concentrated hydrochloric acid and anhydrous ethanol mixed solution according to the ratio (add 10ml of mixed solution for every 0.1g of sample) to obtain the seventh mixed solution;
[0091] 11) Transfer the above seventh mixed solution to an oil bath and incubate at 60°C for 12 hours to obtain the eighth mixed solution;
[0092] 12) Filter the above eighth mixed solution through a Buchner funnel;
[0093] 13) Place the sample filtered in step 12) in a room temperature environment for 24 hours to allow the sample to dry naturally, and obtain a second dried sample. The second dried sample is a chiral carbon silicon composite mesoporous material with the amino-modified inner surface removed from the template.
[0094] 14) The second dried sample was calcined at 500°C for 3 hours under a nitrogen atmosphere to obtain a carbon-silicon composite chiral mesoporous nanocomposite material.
[0095] 15) Prepare an ethanol mixture of anhydrous ethanol and deionized water in a 2:5 ratio;
[0096] 16) Fit the AAO substrate tightly onto the surface of the filtration device and set up the filtration device.
[0097] 17) The carbon-silicon composite chiral mesoporous nanocomposite material was dispersed in the above ethanol mixed solution to obtain the ninth mixed solution;
[0098] 18) The above ninth mixed solution is ultrasonically vibrated to uniformly disperse the nanomaterials in the solution, thus obtaining a dispersion solution;
[0099] 19) The above dispersion solution is filtered onto the AAO substrate through the above-mentioned filtration device to obtain the final carbon silicon composite chiral mesoporous heterojunction membrane MCSC / AAO with a carbon silicon composite chiral channel structure.
[0100] The above embodiments are preferred embodiments of the present invention and are not intended to limit the scope of protection of the present invention.
Claims
1. A method for preparing a carbon-silicon composite chiral mesoporous heterojunction film, characterized in that, Includes the following steps: A carbon-silicon composite chiral mesoporous nanocomposite material was uniformly dispersed in an aqueous solution, and then tightly bonded to an anodic aluminum oxide array at the interface using interfacial superassembly. After removing the solvent by filtration and drying, the carbon-silicon composite chiral mesoporous heterostructure film was obtained. The carbon-silicon composite chiral mesoporous nanocomposite material was prepared by a hydrothermal method using guanylic acid as a template agent. The silicon-carbon composite chiral mesoporous heterojunction membrane includes an anodic aluminum oxide film and a silicon-carbon composite chiral mesoporous thin film layer covering the anodic aluminum oxide film, wherein the anodic aluminum oxide film is positively charged in water, and the silicon-carbon composite chiral mesoporous thin film layer is negatively charged in water.
2. The method for preparing a carbon-silicon composite chiral mesoporous heterojunction film according to claim 1, characterized in that: in, The preparation process of the carbon-silicon composite chiral mesoporous nanocomposite material includes: A mixed solution of guanylic acid, potassium chloride, 3-aminopropyltriethoxysilane, concentrated hydrochloric acid, tetraethyl orthosilicate, and soluble phenolic resin was subjected to a hydrothermal reaction in a hydrothermal reactor, and then calcined in an inert atmosphere to obtain the carbon-silicon composite chiral mesoporous nanocomposite material.
3. The method for preparing a carbon-silicon composite chiral mesoporous heterojunction film according to claim 2, Its features are: The preparation process of the carbon-silicon composite chiral mesoporous nanocomposite material specifically includes the following steps: Step 1: Disperse or dissolve guanylic acid and potassium chloride in deionized water. Add 37% concentrated hydrochloric acid and 3-aminopropyltriethoxysilane under stirring. Continue stirring and add tetraethyl orthosilicate and soluble phenolic resin dropwise. Stir at room temperature for a period of time. Step 2: Transfer the mixed solution obtained in Step 1 into a hydrothermal reactor for hydrothermal reaction, then filter and dry to obtain a chiral carbon silicon composite material with a template. Step 3: Add the chiral carbon silicon composite material with the template to a mixed solution of concentrated hydrochloric acid and anhydrous ethanol and heat it. Then filter and dry it to obtain a chiral carbon silicon composite mesoporous material with the template removed from the amino-modified inner surface. Step 4: The chiral carbon-silicon composite mesoporous material obtained in step 3 is calcined in an inert gas to obtain the carbon-silicon composite chiral mesoporous nanocomposite material.
4. The method for preparing a carbon-silicon composite chiral mesoporous heterojunction film according to claim 3, characterized in that: in, In step 1, the molar ratio of tetraethyl orthosilicate to the soluble phenolic resin is 1:0.
75. The mass-to-volume ratio of the guanylic acid and the 3-aminopropyltriethoxysilane is (0.4-0.7) g : (0.70-1.00) ml. The mass-to-volume ratio of guanylic acid to tetraethyl orthosilicate is (0.4-0.7) g : (0.79-1.12) ml. The mass-to-volume ratio of the guanylic acid to the concentrated hydrochloric acid is (0.4-0.7) g:(0.12-0.26) ml.
5. The method for preparing a carbon-silicon composite chiral mesoporous heterojunction film according to claim 3, characterized in that: in, In step 3, the concentrated hydrochloric acid and anhydrous ethanol mixture contains 37% concentrated hydrochloric acid, and the volume ratio of concentrated hydrochloric acid to anhydrous ethanol is 3:
7.
6. The method for preparing a carbon-silicon composite chiral mesoporous heterojunction film according to claim 3, characterized in that: in, In step 2, the hydrothermal reaction temperature is 80℃~120℃, and the reaction time is 24h~120h.
7. The method for preparing a carbon-silicon composite chiral mesoporous heterojunction film according to claim 3, characterized in that: in, In step 4, the roasting temperature is 500℃~1000℃ and the roasting time is 3h~5h.
8. The method for preparing a carbon-silicon composite chiral mesoporous heterojunction film according to claim 3, characterized in that: in, The process of uniformly dispersing the carbon-silicon composite chiral mesoporous nanomaterial in a deionized aqueous solution includes: ultrasonically dispersing the carbon-silicon composite chiral mesoporous nanomaterial in an ethanol mixture of anhydrous ethanol and deionized water.
Citation Information
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