A method for preparing a supercapacitor diaphragm material
By combining graphene composite materials and silica aerogel with non-covalent bonds and high-temperature heat treatment, a porous carbon network is formed, which solves the problems of insufficient tensile strength and low porosity and air permeability of membrane materials in the prior art, and realizes the performance improvement of membrane materials.
Patent Information
- Application Number
- CN202510347801.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-24
- Publication Date
- 2025-11-14
- Estimated Expiration
- 2045-03-24
AI Technical Summary
Existing supercapacitor membrane materials require the use of hydrofluoric acid during preparation, and their tensile strength is insufficient, while their porosity and permeability need to be improved.
Graphene composite material and silica aerogel were used as raw materials. They were bonded by non-covalent bonds and formed into a porous carbon network after high-temperature heat treatment. Then, they were coated with cellulose slurry to prepare supercapacitor membrane material.
It effectively improves the tensile strength and porosity of the diaphragm material, enhances air permeability, and meets the application requirements of high-temperature environments while avoiding the use of hydrofluoric acid.
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Figure BDA0005325197320000101
Abstract
Description
Technical Field
[0001] This invention belongs to the field of supercapacitor technology, and specifically relates to a method for preparing a supercapacitor separator material. Background Technology
[0002] Supercapacitors combine the rapid charging and discharging characteristics of capacitors with the energy storage features of electrochemical batteries. They store and release energy through the polarization of the electrolyte and the bilayer effect at the electrode / electrolyte interface. The charging and discharging process is a physical process involving the release of energy via an electrostatic field. The energy storage process is reversible and can be repeatedly charged and discharged hundreds of thousands of times. The separator, as a crucial component of the supercapacitor, directly affects its performance. Its main functions in a supercapacitor are: separating the positive and negative electrodes to prevent short circuits caused by electrode contact; and forming ion circulation channels to ensure the normal passage of electrolyte ions, enabling the supercapacitor to charge and discharge rapidly.
[0003] Chinese patent (publication number CN111508732B) discloses a composite separator for supercapacitors and its preparation method. This invention introduces silica to prepare a porous graphene film, ensuring the normal movement of anions and cations in the electrolyte during charging and discharging. By combining the high tensile strength of graphene with a fibrous binder introduced into cellulose slurry, the processed composite separator is ensured to have good tensile strength, uniform thickness and pore size. This facilitates its application in high-temperature environments when assembled into a supercapacitor. Furthermore, the preparation method is simple and suitable for continuous production. However, this patent requires the use of the hazardous chemical hydrofluoric acid to etch silica during the preparation of the porous graphene film. Simultaneously, the resulting separator material has insufficient tensile strength, and its porosity and air permeability need improvement, affecting its application and promotion.
[0004] Therefore, how to prepare supercapacitor membrane materials by modifying the membrane material components without using hydrofluoric acid, effectively improving the tensile strength of the material, and obtaining better porosity and air permeability, has become a key area that needs to be addressed. Summary of the Invention
[0005] To address the shortcomings of existing technologies, the present invention aims to provide a method for preparing supercapacitor membrane materials, thereby solving problems such as the need for hydrofluoric acid in the preparation process of membrane materials, insufficient tensile strength, and the need to improve porosity and air permeability.
[0006] This invention uses graphene composite material and silica aerogel as raw materials. The polymers in both are bonded by non-covalent bonds and undergo carbonization during subsequent high-temperature heat treatment to form a graphene porous membrane with a porous carbon network. Combined with the coating treatment of cellulose slurry, a supercapacitor membrane material is prepared, which effectively improves the tensile strength of the material and obtains better porosity and air permeability.
[0007] The technical solution adopted by the present invention to solve the above-mentioned technical problems is as follows:
[0008] This invention provides a method for preparing a supercapacitor separator material, comprising the following steps:
[0009] S1: By weight, 90-100 parts of graphene composite material and 40-50 parts of silica are mixed evenly at high speed, and 500-600 parts of deionized water are added and stirred to disperse to obtain a slurry;
[0010] S2: The slurry is coated onto a PET substrate, dried, the PET substrate is peeled off, and heat-treated to obtain a graphene porous membrane.
[0011] S3: Mix 40-50 parts of cellulose, 5-10 parts of binder and 45-50 parts of deionized water to obtain a coating solution. Coat both sides of the graphene porous membrane with the coating solution and dry to obtain a supercapacitor membrane material.
[0012] As a preferred embodiment of the present invention, the graphene composite material may be in the following weight proportions: 90 parts, 92 parts, 94 parts, 96 parts, 98 parts, or 100 parts.
[0013] As a preferred embodiment of the present invention, the weight parts of the silicon dioxide may be 40 parts, 42 parts, 44 parts, 46 parts, 48 parts, or 50 parts, etc.
[0014] As a preferred embodiment of the present invention, the weight parts of the cellulose may be 40 parts, 42 parts, 44 parts, 46 parts, 48 parts, or 50 parts, etc.
[0015] As a preferred embodiment of the present invention, the adhesive may be expressed in parts by weight of 5, 6, 7, 8, 9, or 10 parts, etc.
[0016] As a preferred technical solution of the present invention, the preparation method of the graphene composite material includes: dispersing 4-6 parts by weight of commercially available graphene oxide in 400-500 parts by weight of deionized water, then adding 10-16 parts by weight of 1 mol / L hydrochloric acid solution and 2-4 parts by weight of ferric chloride and stirring evenly to obtain solution A; dissolving 16-20 parts by weight of aniline in 400-500 parts by weight of carbon tetrachloride to form solution B; and slowly pouring 400-500 parts by weight of solution A onto the top of 400-500 parts by weight of solution B for in-situ polymerization to obtain the graphene composite material.
[0017] As a preferred technical solution of the present invention, the conditions for in-situ polymerization include: first, letting it stand for 40 to 48 hours, then centrifuging and washing the composite material generated in the aqueous phase, drying it at 30 to 40°C for 30 to 40 hours, and then pulverizing it.
[0018] During high-temperature heat treatment, nitrogen atoms in polyaniline migrate into the graphene lattice, forming nitrogen-doped graphene. Nitrogen doping can repair some defects in graphene and increase the interaction force between layers, thereby improving the overall mechanical strength of the composite material and effectively enhancing its tensile strength.
[0019] As a preferred embodiment of the present invention, the silica is silica aerogel;
[0020] The method for preparing the silica aerogel includes: mixing 30-40 parts by weight of formaldehyde and 450-500 parts by weight of isopropanol evenly, then adding 40-50 parts by weight of resorcinol and stirring thoroughly, then adding 50-60 parts by weight of deionized water and 200-220 parts by weight of 3-aminopropyltriethoxysilane for gelation treatment to obtain silica aerogel.
[0021] As a preferred embodiment of the present invention, the gelation treatment conditions include: first stirring at a speed of 80-100 r / min for 50-60 min, then keeping warm at 60-65°C for 40-48 h to obtain a wet gel, and then replacing it with ethanol at 60-65°C and freeze-drying.
[0022] Silica aerogel is an ultralight nanoporous material composed of silica. It is a nanoporous material with ultra-high porosity and low density. Its unique three-dimensional network structure can effectively improve the porosity of membrane materials.
[0023] As a preferred embodiment of the present invention, the cellulose is modified cellulose;
[0024] The method for preparing the modified cellulose includes: adding 4-6 parts by weight of cellulose to 240-250 parts by weight of deionized water for pretreatment, then adding 0.4-0.8 parts by weight of carbon nanotubes and dispersing them evenly, and finally adding 40-50 parts by weight of 8-10% polyvinyl alcohol aqueous solution and stirring for 1-3 hours, freeze-drying, and pulverizing to obtain modified cellulose.
[0025] As a preferred technical solution of the present invention, the pretreatment conditions include: stirring at a speed of 200-240 r / min for 30-40 min, and then sonicating for 50-60 min.
[0026] The carbon nanotubes introduced into the modified cellulose have a high aspect ratio and good dispersibility, and can form a three-dimensional network structure in the cellulose matrix, optimizing the pore size and distribution on the surface, thereby improving the air permeability of the membrane material.
[0027] As a preferred embodiment of the present invention, the adhesive is selected from polytetrafluoroethylene or ethylene-tetrafluoroethylene copolymer.
[0028] As a preferred embodiment of the present invention, the drying temperature in step S2 is 40-60°C and the drying time is 6-8 hours.
[0029] As a preferred technical solution of the present invention, the heat treatment conditions in step S2 include: first, hot rolling at 180-220°C, and then calcining at 600-650°C for 2-4 hours under argon protection.
[0030] As a preferred embodiment of the present invention, the drying conditions in step S3 include: a temperature of 70-90°C and a time of 8-10 minutes.
[0031] Compared with the prior art, the present invention has the following beneficial effects:
[0032] (1) In this invention, graphene composite material and silica aerogel are first mixed. The resorcinol in the silica aerogel contains benzene rings, which can undergo π-π stacking with the polyaniline in the graphene composite material. Non-covalent bonds are formed through the interaction of π electron clouds. During the subsequent high-temperature heat treatment, carbonization occurs to form a graphene porous membrane with a porous carbon network. The network structure of the graphene porous membrane, together with silica, can improve the tensile strength of the membrane material, while the porous structure can effectively improve the porosity and air permeability of the material. Then, cellulose slurry is coated on the graphene porous membrane. The carbon nanotubes of the modified cellulose in the cellulose slurry and the graphene surface are both made of sp 2The hybrid carbon atoms have a conjugated electron system. The two are stacked face-to-face or offset, and the electron clouds overlap to form a stable interaction, thereby ensuring a good bond between cellulose and graphene porous membranes and improving the mechanical properties and air permeability of the membrane material.
[0033] (2) When the graphene composite material of the present invention is subjected to high-temperature heat treatment, nitrogen atoms in polyaniline will migrate into the graphene lattice to form nitrogen-doped graphene. Nitrogen doping can repair some defects of graphene and increase the interaction force between the layers, thereby improving the overall mechanical strength of the composite material and effectively enhancing the tensile strength.
[0034] (3) The silica aerogel of the present invention is an ultralight nanoporous material composed of silica. It is a nanoporous material with ultra-high porosity and low density. Its unique three-dimensional network structure can effectively improve the porosity of the membrane material.
[0035] (4) The carbon nanotubes introduced into the modified cellulose of this invention have a high aspect ratio and good dispersibility, and can form a three-dimensional network structure in the cellulose matrix, optimizing the pore size and distribution on the surface, thereby improving the air permeability of the membrane material. Detailed Implementation
[0036] To facilitate understanding of the present invention, the following embodiments are provided. Those skilled in the art should understand that these embodiments are merely illustrative and should not be construed as limiting the scope of the invention.
[0037] The sources of some components in the examples and comparative examples are as follows:
[0038] Commercially available graphene oxide, product number G139803, was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.
[0039] Commercially available silica, product number S433666, was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.
[0040] Commercially available cellulose, product number C104841, was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.
[0041] Polytetrafluoroethylene, item number P434338, was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.
[0042] Ethylene-tetrafluoroethylene copolymer, model LC031, purchased from Ganzhou Lichang New Materials Co., Ltd.
[0043] Aniline, CAS No. 62-53-3, was purchased from Sinopharm Chemical Reagent Co., Ltd.
[0044] Carbon tetrachloride, CAS No. 56-23-5, was purchased from Shanghai Maclean Biochemical Technology Co., Ltd.
[0045] Ferric chloride, CAS No. 7705-08-0, was purchased from Shanghai Maclean Biochemical Technology Co., Ltd.
[0046] Formaldehyde, CAS No. 50-00-0, purchased from Sinopharm Chemical Reagent Co., Ltd.
[0047] Isopropanol, CAS 67-63-0, purchased from Sinopharm Chemical Reagent Co., Ltd.
[0048] Resorcinol, CAS108-46-3, purchased from Shanghai Maclean Biochemical Technology Co., Ltd.
[0049] 3-Aminopropyltriethoxysilane, CAS919-30-2, purchased from Shanghai Maclean Biochemical Technology Co., Ltd.
[0050] Carbon nanotubes, item number C313046, were purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.
[0051] Polyvinyl alcohol, product number P139543, was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.
[0052] Example 1
[0053] This embodiment provides a method for preparing a supercapacitor separator material, including the following steps:
[0054] S1: By weight, 100 parts of graphene composite material and 50 parts of silica aerogel are mixed evenly at high speed, and 600 parts of deionized water are added and stirred to disperse to obtain a slurry;
[0055] S2: The slurry is coated on a PET substrate and dried (drying temperature is 60℃, drying time is 8h). The PET substrate is peeled off and heat-treated. First, it is hot-calcined at 220℃, and then placed under argon protection and calcined at 650℃ for 2h to obtain a graphene porous membrane.
[0056] S3: Mix 50 parts of modified cellulose, 5 parts of binder polytetrafluoroethylene and 45 parts of deionized water to obtain a coating solution. Coat both sides of the graphene porous membrane with the coating solution and dry (temperature 90℃, time 8min) to obtain a supercapacitor membrane material.
[0057] Preparation of the graphene composite material: By weight, 6 parts of commercially available graphene oxide were dispersed in 500 parts of deionized water, and then 16 parts of 1 mol / L hydrochloric acid solution and 4 parts of ferric chloride were added and stirred evenly to obtain solution A. 20 parts of aniline were dissolved in 500 parts of carbon tetrachloride to form solution B. 500 parts of solution A were slowly poured on top of 500 parts of solution B for in-situ polymerization. The mixture was allowed to stand for 48 hours, and then the composite material generated in the aqueous phase was centrifuged and washed. It was dried at 40°C for 30 hours and then pulverized to obtain the graphene composite material.
[0058] Preparation of the silica aerogel: By weight, 40 parts of formaldehyde and 500 parts of isopropanol are mixed evenly, then 50 parts of resorcinol are added and stirred thoroughly, then 60 parts of deionized water and 220 parts of 3-aminopropyltriethoxysilane are added for gelation treatment. First, the mixture is stirred at 100 r / min for 50 min, then kept at 65℃ for 40 h to obtain a wet gel, then replaced with ethanol at 65℃ and freeze-dried to obtain silica aerogel.
[0059] Preparation of the modified cellulose: By weight, 6 parts of cellulose were added to 250 parts of deionized water for pretreatment. The mixture was first stirred at 240 r / min for 30 min, then sonicated for 60 min, then 0.8 parts of carbon nanotubes were added and dispersed evenly. Finally, 50 parts of 10% polyvinyl alcohol aqueous solution were added and stirred for 3 h. The mixture was then freeze-dried and pulverized to obtain the modified cellulose.
[0060] Example 2
[0061] This embodiment provides a method for preparing a supercapacitor separator material, including the following steps:
[0062] S1: By weight, 90 parts of graphene composite material and 40 parts of silica aerogel are mixed evenly at high speed, and 500 parts of deionized water are added and stirred to disperse to obtain a slurry;
[0063] S2: The slurry is coated on a PET substrate and dried (drying temperature is 40℃, drying time is 8h). The PET substrate is peeled off and heat-treated. First, it is hot-calcined at 180℃, and then placed under argon protection and calcined at 600℃ for 4h to obtain a graphene porous membrane.
[0064] S3: Mix 40 parts of modified cellulose, 10 parts of binder ethylene-tetrafluoroethylene copolymer and 50 parts of deionized water to obtain a coating solution. Coat both sides of the graphene porous membrane with the coating solution and dry (temperature 70℃, time 10min) to obtain a supercapacitor membrane material.
[0065] Preparation of the graphene composite material: By weight, 4 parts of commercially available graphene oxide were dispersed in 400 parts of deionized water, then 10 parts of 1 mol / L hydrochloric acid solution and 2 parts of ferric chloride were added and stirred evenly to obtain solution A. 16 parts of aniline were dissolved in 400 parts of carbon tetrachloride to form solution B. 400 parts of solution A were slowly poured on top of 400 parts of solution B for in-situ polymerization. The mixture was allowed to stand for 40 hours, then the composite material generated in the aqueous phase was centrifuged and washed, dried at 30°C for 40 hours, and pulverized to obtain the graphene composite material.
[0066] Preparation of the silica aerogel: 30 parts by weight of formaldehyde and 450 parts by weight of isopropanol are mixed evenly, then 40 parts by weight of resorcinol are added and stirred thoroughly, then 50 parts by weight of deionized water and 200 parts by weight of 3-aminopropyltriethoxysilane are added for gelation treatment. First, the mixture is stirred at 80 r / min for 60 min, then kept at 60℃ for 48 h to obtain a wet gel, then replaced with ethanol at 60℃ and freeze-dried to obtain silica aerogel.
[0067] Preparation of the modified cellulose: By weight, 4 parts of cellulose were added to 240 parts of deionized water for pretreatment. The mixture was first stirred at 200 r / min for 40 min, then sonicated for 50 min, then 0.4 parts of carbon nanotubes were added and dispersed evenly. Finally, 40 parts of 8% polyvinyl alcohol aqueous solution were added and stirred for 3 h. The mixture was then freeze-dried and pulverized to obtain the modified cellulose.
[0068] Example 3
[0069] This embodiment provides a method for preparing a supercapacitor separator material, including the following steps:
[0070] S1: By weight, 95 parts of graphene composite material and 45 parts of silica aerogel are mixed evenly at high speed, and 550 parts of deionized water are added and stirred to disperse to obtain a slurry.
[0071] S2: The slurry is coated on a PET substrate and dried (drying temperature is 50℃, drying time is 7h). The PET substrate is peeled off and heat-treated. First, it is hot-calcined at 200℃, and then placed under argon protection and calcined at 620℃ for 3h to obtain a graphene porous membrane.
[0072] S3: Mix 45 parts modified cellulose, 8 parts binder polytetrafluoroethylene and 47 parts deionized water to obtain a coating solution. Coat both sides of the graphene porous membrane with the coating solution and dry (temperature 80℃, time 9min) to obtain a supercapacitor membrane material.
[0073] Preparation of the graphene composite material: By weight, 5 parts of commercially available graphene oxide were dispersed in 450 parts of deionized water, then 14 parts of 1 mol / L hydrochloric acid solution and 3 parts of ferric chloride were added and stirred evenly to obtain solution A. 18 parts of aniline were dissolved in 450 parts of carbon tetrachloride to form solution B. 450 parts of solution A were slowly poured on top of 450 parts of solution B for in-situ polymerization. The mixture was first allowed to stand for 44 hours, then the composite material generated in the aqueous phase was centrifuged and washed, dried at 35°C for 35 hours, and pulverized to obtain the graphene composite material.
[0074] Preparation of the silica aerogel: 35 parts by weight of formaldehyde and 480 parts by weight of isopropanol are mixed evenly, then 45 parts by weight of resorcinol are added and stirred thoroughly, then 55 parts by weight of deionized water and 210 parts by weight of 3-aminopropyltriethoxysilane are added for gelation treatment. The mixture is first stirred at 90 r / min for 55 min, then kept at 62℃ for 44 h to obtain a wet gel, then replaced with ethanol at 62℃ and freeze-dried to obtain silica aerogel.
[0075] Preparation of the modified cellulose: by weight, 5 parts of cellulose were added to 245 parts of deionized water for pretreatment. The mixture was first stirred at 220 r / min for 35 min, then sonicated for 55 min, then 0.6 parts of carbon nanotubes were added and dispersed evenly. Finally, 45 parts of 9% polyvinyl alcohol aqueous solution were added and stirred for 2 h. The mixture was then freeze-dried and pulverized to obtain the modified cellulose.
[0076] Example 4
[0077] The difference between this embodiment and Embodiment 1 is that commercially available silica (item number S433666) is used instead of silica aerogel.
[0078] Example 5
[0079] The difference between this embodiment and Embodiment 1 is that commercially available cellulose (product number C104841) is used instead of modified cellulose.
[0080] Comparative Example 1
[0081] The difference between this comparative example and Example 1 is that commercially available graphene oxide (item number G139803) was used instead of the graphene composite material.
[0082] Comparative Example 2
[0083] The difference between this comparative example and Example 1 is that 50 parts of silica aerogel are not added to the slurry in step S1.
[0084] The performance of the diaphragm materials provided in the above embodiments and comparative examples was tested using the following methods:
[0085] (1) Tensile strength test: The test shall be conducted in accordance with the requirements of GB / T 12914-2018 Determination of tensile strength of paper and paperboard by constant speed tensile test (20 mm / min).
[0086] (2) Porosity test: The porosity of the membrane material was tested using a fully automated nitrogen adsorption micropore distribution tester (model QUADRASORB SI, CANTA Corporation, USA).
[0087] (3) Air permeability test: The test shall be conducted in accordance with the requirements of GB / T 458-2008 Determination of air permeability of paper and paperboard.
[0088] The performance test data above are shown in Table 1.
[0089] Table 1 Performance Test Results
[0090]
[0091] As can be seen from the above, the present invention uses graphene composite material and silica aerogel as raw materials. The polymers in both are bonded by non-covalent bonds and undergo carbonization during subsequent high-temperature heat treatment to form a graphene porous membrane with a porous carbon network. Combined with the coating treatment of cellulose slurry, a supercapacitor separator material (Examples 1 to 3) is prepared. It has good comprehensive performance, with a tensile strength of 909 to 914 N / m, a porosity of 77.1 to 77.8%, and an air permeability of 44.7 to 45.2 μm / (Pa·s).
[0092] Compared to Example 1, replacing silica aerogel with commercially available silica (item number S433666) resulted in decreased tensile strength, smaller porosity, and reduced air permeability (Example 4); replacing modified cellulose with commercially available cellulose (item number C104841) resulted in decreased tensile strength, smaller porosity, and reduced air permeability (Example 5); replacing graphene composite material with commercially available graphene oxide (item number G139803) resulted in decreased tensile strength, smaller porosity, and reduced air permeability (Comparative Example 1); and not adding 50 parts of silica aerogel to the slurry in step S1 resulted in decreased tensile strength, smaller porosity, and reduced air permeability (Comparative Example 2).
[0093] In summary, this invention uses graphene composite material and silica aerogel as raw materials. The polymers in both are bonded by non-covalent bonds and undergo carbonization during subsequent high-temperature heat treatment to form a graphene porous membrane with a porous carbon network. Combined with the coating treatment of cellulose slurry, a supercapacitor membrane material is prepared, which effectively improves the tensile strength of the material and obtains better porosity and air permeability.
Claims
1. A method for preparing a supercapacitor diaphragm material, characterized in that, include: S1: By weight, 90-100 parts of graphene composite material and 40-50 parts of silica aerogel are mixed evenly at high speed, and 500-600 parts of deionized water are added and stirred to disperse to obtain a slurry; S2: The slurry is coated onto a PET substrate, dried, the PET substrate is peeled off, and heat-treated to obtain a graphene porous membrane. S3: Mix 40-50 parts of modified cellulose, 5-10 parts of binder and 45-50 parts of deionized water to obtain a coating solution. Coat both sides of the graphene porous membrane with the coating solution and dry to obtain a supercapacitor membrane material. The preparation method of the graphene composite material includes: dispersing 4-6 parts of commercially available graphene oxide in 400-500 parts of deionized water by weight, then adding 10-16 parts of 1mol / L hydrochloric acid solution and 2-4 parts of ferric chloride and stirring evenly to obtain solution A; dissolving 16-20 parts of aniline in 400-500 parts of carbon tetrachloride to form solution B; and slowly pouring 400-500 parts of solution A onto the top of 400-500 parts of solution B for in-situ polymerization to obtain the graphene composite material. The preparation method of the silica aerogel includes: mixing 30-40 parts by weight of formaldehyde and 450-500 parts by weight of isopropanol evenly, then adding 40-50 parts by weight of resorcinol and stirring thoroughly, then adding 50-60 parts by weight of deionized water and 200-220 parts by weight of 3-aminopropyltriethoxysilane for gelation treatment to obtain silica aerogel. The method for preparing the modified cellulose includes: adding 4-6 parts by weight of cellulose to 240-250 parts by weight of deionized water for pretreatment, then adding 0.4-0.8 parts by weight of carbon nanotubes and dispersing them evenly, and finally adding 40-50 parts by weight of 8-10% polyvinyl alcohol aqueous solution and stirring for 1-3 hours, freeze-drying, and pulverizing to obtain modified cellulose.
2. The method for preparing a supercapacitor separator material according to claim 1, characterized in that, The conditions for the in-situ polymerization include: first, letting it stand for 40 to 48 hours, then centrifuging and washing the composite material generated in the aqueous phase, drying it at 30 to 40°C for 30 to 40 hours, and then pulverizing it.
3. The method for preparing a supercapacitor separator material according to claim 1, characterized in that, The gelation treatment conditions include: first stirring at a speed of 80-100 r / min for 50-60 min, then keeping at 60-65℃ for 40-48 h to obtain a wet gel, then replacing it with ethanol at 60-65℃ and freeze-drying.
4. The method for preparing a supercapacitor separator material according to claim 1, characterized in that, The pretreatment conditions include: stirring at 200-240 r / min for 30-40 min, followed by sonication for 50-60 min.
5. The method for preparing a supercapacitor separator material according to claim 1, characterized in that, The adhesive is selected from polytetrafluoroethylene or ethylene-tetrafluoroethylene copolymer.
6. The method for preparing a supercapacitor separator material according to claim 1, characterized in that, In step S2, the drying temperature is 40–60°C and the drying time is 6–8 hours.
7. The method for preparing a supercapacitor separator material according to claim 1, characterized in that, The conditions for heat treatment in step S2 include: first, hot rolling at 180-220°C, and then calcining at 600-650°C for 2-4 hours under argon protection.
8. The method for preparing a supercapacitor separator material according to claim 1, characterized in that, The drying conditions in step S3 include: a temperature of 70–90°C and a time of 8–10 minutes.
Citation Information
Patent Citations
Composite separators for supercapacitors and their preparation methods
CN111508732B
Conductive polymer / graphene composite and preparation method thereof
CN108586737A
Composite diaphragm for supercapacitor and preparation method thereof
CN111508732A