CN114940759B - Fluorine-containing polyimide film, preparation method thereof and supercapacitor - Google Patents
Fluorine-containing polyimide film, preparation method thereof and supercapacitor Download PDFInfo
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- CN114940759B CN114940759B CN202210757565.9A CN202210757565A CN114940759B CN 114940759 B CN114940759 B CN 114940759B CN 202210757565 A CN202210757565 A CN 202210757565A CN 114940759 B CN114940759 B CN 114940759B
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 34
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 31
- 239000011737 fluorine Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000003792 electrolyte Substances 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 13
- 150000004985 diamines Chemical class 0.000 claims abstract description 9
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005266 casting Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000012716 precipitator Substances 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 3
- 238000007790 scraping Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-methyl-PhOH Natural products CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 claims description 12
- AWJUIBRHMBBTKR-UHFFFAOYSA-N iso-quinoline Natural products C1=NC=CC2=CC=CC=C21 AWJUIBRHMBBTKR-UHFFFAOYSA-N 0.000 claims description 8
- 238000005530 etching Methods 0.000 claims description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical group CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 4
- 239000003990 capacitor Substances 0.000 claims description 4
- FJVIHKKXPLPDSV-UHFFFAOYSA-N 4-phenoxybenzene-1,2-diamine Chemical group C1=C(N)C(N)=CC=C1OC1=CC=CC=C1 FJVIHKKXPLPDSV-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 125000002183 isoquinolinyl group Chemical group C1(=NC=CC2=CC=CC=C12)* 0.000 claims description 2
- 125000003717 m-cresyl group Chemical group [H]C1=C([H])C(O*)=C([H])C(=C1[H])C([H])([H])[H] 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 12
- 239000002244 precipitate Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 4
- PBKONEOXTCPAFI-UHFFFAOYSA-N 1,2,4-trichlorobenzene Chemical compound ClC1=CC=C(Cl)C(Cl)=C1 PBKONEOXTCPAFI-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- RFFLAFLAYFXFSW-UHFFFAOYSA-N 1,2-dichlorobenzene Chemical compound ClC1=CC=CC=C1Cl RFFLAFLAYFXFSW-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 150000008064 anhydrides Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 2
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000000010 aprotic solvent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000010329 laser etching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
- C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1039—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors comprising halogen-containing substituents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/04—Hybrid capacitors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a fluorine-containing polyimide film, a preparation method thereof and a supercapacitor, wherein the preparation method of the fluorine-containing polyimide film comprises the following steps: stirring diamine and a first solvent uniformly under the protection of nitrogen, adding dianhydride and a catalyst, and heating until the reaction is complete to obtain a viscous solution; stirring the viscous solution and the precipitator uniformly, washing for a plurality of times, carrying out suction filtration, drying the solid obtained by suction filtration, dissolving the solid in a second solvent to obtain a casting solution, scraping the casting solution on a template, drying, and stripping to obtain the required fluorine-containing polyimide film. The fluorine-containing polyimide film of the invention uses the fluorine-containing polyimide film containing-CF in the preparation process 3 Is etched with CHF 2 、CH 2 F and COF 2 The gaseous form is released, so that more micropore structures are generated in the fluorine-containing polyimide film, the electrolyte is facilitated to be immersed, and the performance of the prepared supercapacitor is improved.
Description
Technical Field
The invention belongs to the field of chemical synthesis, and particularly relates to a fluorine-containing polyimide film, a preparation method thereof and a supercapacitor.
Background
Recently, the demand for miniature electronic devices has grown rapidly. In particular, transparent devices in wearable device applications have received great attention. Thus, this trend has led to active research into small, flexible and transparent energy storage devices.
Super capacitors have long cycle life and high power density, are one of the strongest candidates most likely to replace traditional batteries, which are generally opaque and inflexible miniature energy devices; recently, various organic materials, such as human hair and polyimide, have been used as carbon precursors from which porous carbon materials are derived by pyrolysis. However, the commercial polyimide film has small and few pores after laser etching, which is unfavorable for the full infiltration of electrolyte, so the electrochemical performance of the super capacitor is not good.
Disclosure of Invention
In view of the above, the present invention aims to provide a fluorine-containing polyimide film, a preparation method thereof and a supercapacitor, so as to prepare a polyimide film suitable for the supercapacitor, facilitate the immersion of electrolyte, and improve the performance of the supercapacitor.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
a method for preparing a fluorine-containing polyimide film, comprising the following steps:
s1: diamine and a first solvent are placed into a container, stirred uniformly at normal temperature for a certain time under the protection of nitrogen, dianhydride and a catalyst with certain mass are added to prepare a mixed solution, and the mixed solution is heated until the reaction is complete, so that a viscous solution is obtained; preferably, the solid content of the mixed solution is 15% -20%;
s2: stirring the viscous solution and a precipitator uniformly to generate solid precipitate, flushing the solid precipitate for a plurality of times by using the precipitator, carrying out suction filtration, drying the solid obtained by suction filtration in a vacuum oven to obtain dry solid, dissolving the dry solid in a second solvent to obtain casting solution, scraping the casting solution on a template, putting the template in the vacuum oven for drying, cooling to room temperature, putting the template in deionized water for stripping and drying to obtain the required fluorine-containing polyimide film; preferably, the drying temperature of the solid obtained by suction filtration in the vacuum oven is 100 ℃, the drying time is 12 hours, the drying temperature of the casting film liquid in the vacuum oven is 180 ℃, and the drying time is 12 hours.
Further, the diamine is 3, 4-diaminodiphenyl ether and the dianhydride is hexafluorodianhydride.
Further, the molar ratio of diamine to dianhydride is 1:1.
Further, the first solvent is a high boiling point solvent; preferably, the first solvent comprises one of phenol, cresol, m-cresol, o-dichlorobenzene, 1,2, 4-trichlorobenzene; further preferably, the first solvent is m-cresol.
Further, the catalyst is one of pyridine, isoquinoline and triethylamine; preferably, the catalyst is isoquinoline.
Further, the reaction conditions in step S1 are, in order, 1h at 40 ℃, 1h at 80 ℃, 2h at 120 ℃, 2h at 140 ℃, 2h at 160 ℃, and 1h at 180 ℃.
Further, the second solvent is an aprotic solvent; preferably, the second solvent is N, N-dimethylacetamide.
Further, the precipitating agent is ethanol.
The fluorine-containing polyimide film prepared by the preparation method is provided.
The preparation method of the supercapacitor, which is applied to the preparation method or the fluorine-containing polyimide film, comprises the following steps of:
etching the fluorine-containing polyimide film into interdigital electrodes through laser, and coating electrolyte on the electrodes to obtain a supercapacitor; preferably, the laser power is 100%, and the etching depth is 10-15; preferably, the electrolyte is PVA/H 2 SO 4 An electrolyte.
Compared with the prior art, the fluorine-containing polyimide film, the preparation method thereof and the supercapacitor have the following advantages:
the fluorine-containing polyimide film of the invention uses the fluorine-containing polyimide film containing-CF in the preparation process 3 Is etched with CHF 2 、CH 2 F and COF 2 The gaseous form is released, so that more micropore structures are generated in the fluorine-containing polyimide film, the electrolyte is facilitated to be immersed, and the performance of the prepared supercapacitor is improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
FIG. 1 is a schematic diagram of a sample of a fluorine-containing polyimide film produced in example 1 of the present invention;
FIG. 2 is a schematic diagram of a supercapacitor made according to example 1 of the present invention;
FIG. 3 is an electron microscopic view of the fluorine-containing polyimide film produced in example 1 of the present invention;
fig. 4 is an electron microscope image of a commercial film of the prior art.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention pertains. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to the following examples and drawings.
Example 1
(1) Diamine 3,4-ODA (1.20142 g,15mL of m-cresol) was added to the three-necked flask, and the mixture was stirred at room temperature under a nitrogen atmosphere for 1 hour.
(2) Further, 6FDA diacid anhydride, 2.66542g,2 drops of isoquinoline was added.
(3) Then heating to 40 ℃ for 1h,80 ℃ for 1h,120 ℃ for 2h,140 ℃ for 2h,160 ℃ for 2h,180 ℃ for 1h respectively, and stopping the reaction to obtain a viscous solution. 5mL of m-cresol was added during the procedure.
(4) The viscous solution was poured into ethanol to give a solid precipitate. Washing with ethanol for several times, suction filtering, and oven drying at 100deg.C.
(5) 1g of precipitate, 4ml of DMAc was prepared as a 20% solution, the solution was spread on a clean glass plate, placed in an oven, baked at 180℃for 12 hours, and peeled off to obtain a fluorine-containing polyimide film, as shown in FIG. 1.
(6) Etching the commercial film and the dried fluorine-containing polyimide film by laser to obtain the shape of an interdigital electrode with the depth of 10, and coating PVA/H on the electrode 2 SO 4 Electrolyte, and the like, dried for several hours, and performance test was performed after drying.
Example 2
(1) Diamine 3,4-ODA (1.20142 g,15mL of m-cresol) was added to the three-necked flask, and the mixture was stirred at room temperature under a nitrogen atmosphere for 1 hour.
(2) Further, 6FDA diacid anhydride, 2.66542g,2 drops of isoquinoline was added.
(3) Then heating to 40 ℃ for 1h,80 ℃ for 1h,120 ℃ for 2h,140 ℃ for 2h,160 ℃ for 2h,180 ℃ for 1h respectively, and stopping the reaction to obtain a viscous solution. 5mL of m-cresol was added during the procedure.
(4) The viscous solution was poured into ethanol to give a solid precipitate. Washing with ethanol for several times, suction filtering, and oven drying at 100deg.C.
(5) 1g of sediment and 4ml of DMAc are taken to prepare 20 percent solution, the solution is spread on a clean glass plate, the clean glass plate is placed in an oven to be dried for 12 hours at 180 ℃, and then the fluorine-containing polyimide film is obtained by stripping.
(6) Etching the dried film into the shape of an interdigital electrode with the depth of 15 by using laser, and coating PVA/H on the electrode 2 SO 4 Electrolyte, and the like, dried for several hours, and performance test was performed after drying.
The test results of examples 1-2 are shown in Table 1.
TABLE 1 area specific capacitance calculation results of fluorine-containing polyimide films and commercial films prepared in examples 1-2
Fig. 3 is an electron microscope image of the fluorine-containing polyimide film prepared in example 1, fig. 4 is an electron microscope image of a commercial film, and it can be seen from the electron microscope image that the self-made film containing trifluoromethyl is more holes after etching than the commercial film not containing trifluoromethyl, so that the immersion of electrolyte is more favorable, the electrochemical performance is improved, and the area ratio capacitance data calculated after the test in table 1 shows that the area ratio capacitance of the fluorine-containing polyimide film prepared in the invention is about 4 times higher than that of the commercial film, and the fluorine-containing polyimide film prepared in the invention has good electrical performance.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (6)
1. The preparation method of the super capacitor is characterized by comprising the following steps of:
the fluorine-containing polyimide film is etched into interdigital electrodes through laser, electrolyte is coated on the electrodes to obtain the super capacitor,
the preparation method of the fluorine-containing polyimide film comprises the following steps:
s1: uniformly stirring diamine and a first solvent under the protection of nitrogen, adding dianhydride and a catalyst, wherein the diamine is 3, 4-diaminodiphenyl ether, the dianhydride is hexafluorodianhydride, the first solvent is m-cresol, the catalyst is isoquinoline, and heating to react completely to obtain a viscous solution, wherein the reaction conditions are that the reaction is carried out at 40 ℃ for 1h, at 80 ℃ for 1h, at 120 ℃ for 2h, at 140 ℃ for 2h, at 160 ℃ for 2h and at 180 ℃ for 1h in sequence;
s2: stirring the viscous solution and the precipitator uniformly, washing for a plurality of times, carrying out suction filtration, drying the solid obtained by suction filtration, dissolving the solid in a second solvent to obtain a casting solution, scraping the casting solution on a template, drying, and stripping to obtain the required fluorine-containing polyimide film.
2. The supercapacitor of claim 1, wherein: the molar ratio of diamine to dianhydride is 1:1.
3. The supercapacitor of claim 1, wherein: the second solvent is N, N-dimethylacetamide.
4. The supercapacitor of claim 1, wherein: the precipitating agent is ethanol.
5. The supercapacitor of claim 1, wherein: the laser power is 100% and the etching depth is 10-15.
6. The supercapacitor of claim 1, wherein: the electrolyte is PVA/H 2 SO 4 An electrolyte.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105348551A (en) * | 2015-12-11 | 2016-02-24 | 桂林电器科学研究院有限公司 | Polyimide porous membrane and preparation method thereof |
| CN111019129A (en) * | 2019-11-22 | 2020-04-17 | 桂林电器科学研究院有限公司 | Low-thermal expansion coefficient soluble polyimide resin powder and preparation method thereof |
| CN112086290A (en) * | 2020-09-11 | 2020-12-15 | 闽江学院 | Flexible extensible supercapacitor array based on mechanical buckling principle and preparation method thereof |
| WO2022079454A1 (en) * | 2020-10-16 | 2022-04-21 | Rd Groupco Limited | Flexible supercapacitor with graphene electrodes embedded in hydrogel electrolyte |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105348551A (en) * | 2015-12-11 | 2016-02-24 | 桂林电器科学研究院有限公司 | Polyimide porous membrane and preparation method thereof |
| CN111019129A (en) * | 2019-11-22 | 2020-04-17 | 桂林电器科学研究院有限公司 | Low-thermal expansion coefficient soluble polyimide resin powder and preparation method thereof |
| CN112086290A (en) * | 2020-09-11 | 2020-12-15 | 闽江学院 | Flexible extensible supercapacitor array based on mechanical buckling principle and preparation method thereof |
| WO2022079454A1 (en) * | 2020-10-16 | 2022-04-21 | Rd Groupco Limited | Flexible supercapacitor with graphene electrodes embedded in hydrogel electrolyte |
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