CN112216523A - Preparation method of flame-retardant polymer gel electrolyte with ultrahigh specific capacitance - Google Patents
Preparation method of flame-retardant polymer gel electrolyte with ultrahigh specific capacitance Download PDFInfo
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- 239000011245 gel electrolyte Substances 0.000 title claims abstract description 29
- 229920000642 polymer Polymers 0.000 title claims abstract description 23
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000003063 flame retardant Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229920001817 Agar Polymers 0.000 claims abstract description 17
- 239000008272 agar Substances 0.000 claims abstract description 17
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000000499 gel Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 25
- 239000012528 membrane Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000002485 combustion reaction Methods 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000003792 electrolyte Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007772 electrode material Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000003990 capacitor Substances 0.000 abstract description 13
- 239000007784 solid electrolyte Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000007787 solid Substances 0.000 abstract description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 description 10
- 238000001035 drying Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 241000206572 Rhodophyta Species 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- HVHRDXFMIUHSJZ-WNFIKIDCSA-N (2s,3r,4s,5s,6r)-6-(hydroxymethyl)oxane-2,3,4,5-tetrol;sulfuric acid Chemical compound OS(O)(=O)=O.OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@@H]1O HVHRDXFMIUHSJZ-WNFIKIDCSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WQZGKKKJIJFFOK-FPRJBGLDSA-N beta-D-galactose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-FPRJBGLDSA-N 0.000 description 1
- 239000000679 carrageenan Substances 0.000 description 1
- 229920001525 carrageenan Polymers 0.000 description 1
- 229940113118 carrageenan Drugs 0.000 description 1
- 235000010418 carrageenan Nutrition 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000416 hydrocolloid Substances 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
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- 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
- H01G11/54—Electrolytes
- H01G11/56—Solid electrolytes, e.g. gels; Additives therein
-
- 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
- H01G11/84—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
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- 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
- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
-
- 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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/12—Agar-agar; Derivatives thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a preparation method of a flame-retardant polymer gel electrolyte with ultrahigh specific capacitance, belonging to the field of solid supercapacitors. The polymer gel electrolyte for the super capacitor is successfully prepared by adopting agar, PVA and lithium acetate as raw materials. The gel electrolyte has ultrahigh specific capacitance (701mF cm) compared with the traditional pure PVA gel electrolyte‑2Current density 5mA cm‑2) And good cycle stability(the specific capacitance of the material after 8000 times of continuous charge and discharge was maintained at the initial 90.17%), and excellent flame retardancy was exhibited. The specific capacitance of the traditional gel electrolyte is generally limited to 400mF cm‑2And cannot have flame retardant properties while having high specific capacitance. Therefore, the preparation of the solid electrolyte with higher specific capacitance by using the safe gel polymer with flame retardant property has important significance. In the invention, the agar is rich in source and environment-friendly, and the obtained polymer gel electrolyte with the ultrahigh specific capacitance is excellent in performance when used in a super capacitor, and is an energy material with great prospect.
Description
Technical Field
The invention belongs to the field of super capacitors, and particularly relates to a preparation method of a flame-retardant polymer gel electrolyte with ultrahigh specific capacitance.
Background
With the consumption of fossil energy and the destruction of environmental pollution, there is an urgent need for a green energy storage device. The super capacitor is a novel green energy storage device between a secondary battery and a physical capacitor. Because the traditional super capacitor has a series of problems of high electrolyte toxicity, liquid leakage, difficult packaging and the like, the research and development of the solid super capacitor are urgent and important. The polymer gel electrolyte can solve the problem, and the commonly used polymers are polyvinyl alcohol (PVA), polyethylene oxide (PEO), Polyacrylonitrile (PAN), Polyacrylate (PAA) and polymethyl methacrylate (PMMA). None of these polymers is flame retardant, thus presenting safety issues; and the crystallinity of the polymers is generally higher, which is not beneficial to ion diffusion and makes the specific capacitance difficult to improve. Therefore, the safety problem of the solid-state supercapacitor can be solved by preparing the flame-retardant polymer gel electrolyte with the ultrahigh specific capacitance.
Agar is a hydrocolloid extracted from the class Rhodophyceae. The structure is that chains are formed among beta-D-galactose through 1, 3-glycosidic bonds. At the end of the chain is linked to alpha-D-glucose sulphate by a 1, 4-glycosidic bond. Agar is dissolved in hot water and becomes a gel after cooling. Firstly, because agar molecular chains and water have the function of hydrogen bonds, gel can be formed at low concentration, the water retention rate is high, the conductivity is favorably improved, and the high specific capacitance is obtained; secondly, the agar has a special six-membered ring structure, and the large steric hindrance can reduce the percolation threshold of PVA, improve the conductivity and obtain high specific capacitance; thirdly, a large amount of C-O-C and-OH in the agar can form hydrogen bonds with a large amount of hydroxyl in the PVA, so that the crystallinity of the PVA is reduced, and the conductivity is improved; fourth step ofSince the agar molecule also has a large number of C-O-C in its backbone and many-OH groups, on the one hand, it burns to produce a large amount of H2O and CO2The contact with combustible gas is obstructed, so that the purpose of flame retardance is achieved, and on the other hand, the oxide generated by the lithium ions in the combustion process protects the body of the lithium ion battery, so that the contact of oxygen and the spread of fire are prevented, and further combustion is prevented.
Disclosure of Invention
The invention utilizes agar which is rich in source and can be regenerated as one of raw materials to prepare the flame-retardant polymer hydrogel with ultrahigh specific capacitance which can be used as a solid electrolyte material of a safe super capacitor.
The preparation method is simple in preparation process, does not need expensive equipment, and has good product quality stability and bright prospect in future large-scale application of the solid-state super capacitor.
A preparation method of a flame-retardant polymer gel electrolyte with ultrahigh specific capacitance comprises the following steps:
1) adding 4% agar powder into 1-4M lithium acetate water solution, heating to 90-100 deg.C, dissolving, and making into agar-lithium acetate solution.
2) PVA with the mass fraction of 10 percent is added into 1-4M aqueous solution of lithium acetate, and the mixture is heated to 90-100 ℃ to be dissolved, so that PVA-lithium acetate solution is prepared.
3) Uniformly blending the agar-lithium acetate solution and the PVA-lithium acetate solution at a volume ratio of 1: 1 at high temperature to obtain an agar-PVA-lithium acetate blended solution;
4) pouring the agar-PVA-lithium acetate blended solution on a smooth flat plate, uniformly troweling to the thickness of 2mm, cooling and standing to obtain a gel electrolyte membrane;
5) drying the flame-retardant polymer gel electrolyte membrane with ultrahigh specific capacitance, and then performing combustion test by using an alcohol burner;
6) the active carbon is used as an electrode material, the flame-retardant polymer gel with ultrahigh specific capacitance is used as a solid electrolyte to assemble a super capacitor, and the electrochemical performance of the super capacitor is tested in an electrochemical workstation and a blue-electricity battery testing system.
The invention has the following advantages:
the raw material used by the invention is mainly agar, and the carrageenan is extracted from red algae, so that the raw material has wide sources, is environment-friendly and green, and has high safety.
The flame-retardant polymer gel electrolyte with ultrahigh specific capacitance prepared by the method can be used as a solid electrolyte material of a super capacitor, and has good safety.
The flame-retardant polymer gel electrolyte with ultrahigh specific capacitance prepared by the method can be synthesized in a large quantity, does not need expensive equipment, and can be widely used in solid-state supercapacitors.
Drawings
Fig. 1 is a flowchart for preparing a flame-retardant gel electrolyte membrane with ultra-high specific capacitance of specific example 1.
FIG. 2 is an experimental photograph (group a) of the flame retardant gel electrolyte membrane with ultra-high specific capacitance after drying for various times of combustion in specific example 1, and the inset is a photograph of the electrolyte membrane with the flame removed; and the group b is a comparative picture of the conventional PVA electrolyte membrane.
Fig. 3 is a constant current charge and discharge curve of a supercapacitor made of the flame-retardant gel electrolyte with ultra-high specific capacitance of the specific example 1 at different current densities.
FIG. 4 shows a solid-state supercapacitor made of the flame-retardant gel electrolyte with ultra-high specific capacitance according to example 1 at a current density of 10mA cm-2The cycling stability of the test (voltage 1.8V) was tested.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
1) Adding 4% agar powder into 2M lithium acetate water solution, heating to 95 deg.C, dissolving, and making into agar-lithium acetate solution.
2) PVA with the mass fraction of 10 percent is added into a 2M aqueous solution of lithium acetate, and the mixture is heated to 95 ℃ to be dissolved to prepare a PVA-lithium acetate solution.
3) Uniformly blending the agar-lithium acetate solution and the PVA-lithium acetate solution at a volume ratio of 1: 1 at high temperature to obtain an agar-PVA-lithium acetate blended solution;
4) pouring the agar-PVA-lithium acetate blended solution on a smooth flat plate, uniformly troweling to the thickness of 2mm, cooling and standing to obtain a gel electrolyte membrane;
5) after drying the polymer gel electrolyte membrane, a combustion test was performed using an alcohol burner
6) The electrochemical performance of the gel electrolyte membrane is tested in an electrochemical workstation and a blue-electricity battery testing system by using active carbon as an electrode material and a gel electrolyte membrane as a solid electrolyte to assemble a super capacitor.
Example 2
1) The solubility of the aqueous lithium acetate solution was changed to 1M, and the procedure was otherwise the same as in example 1.
Example 3
1) The solubility of the aqueous lithium acetate solution was changed to 3M, and the procedure was otherwise the same as in example 1.
Example 4
1) The solubility of the aqueous lithium acetate solution was changed to 4M, and the procedure was otherwise the same as in example 1.
Example 5
1) The agar dissolution temperature and PVA dissolution temperature were changed to 90 ℃ and the other operations were the same as in example 1.
Example 6
1) The agar dissolution temperature and PVA dissolution temperature were changed to 100 ℃ and the other operations were the same as in example 1.
Claims (7)
1. A method for preparing a flame-retardant polymer gel electrolyte with ultrahigh specific capacitance is characterized by comprising the following steps:
1) adding appropriate amount of agar powder into aqueous solution of lithium acetate, heating to dissolve, and preparing into agar-lithium acetate solution.
2) Adding a proper amount of PVA into an aqueous solution of lithium acetate, heating and dissolving to prepare a PVA-lithium acetate solution.
3) Uniformly blending the agar-lithium acetate solution and the PVA-lithium acetate solution at high temperature to obtain an agar-PVA-lithium acetate blended solution;
4) pouring the agar-PVA-lithium acetate blended solution on a smooth flat plate, uniformly floating, cooling and standing to obtain the flame-retardant gel electrolyte membrane with ultrahigh specific capacitance;
5) carrying out combustion test on the flame-retardant polymer gel electrolyte membrane with ultrahigh specific capacitance;
6) and testing the electrochemical performance of the flame-retardant gel electrolyte membrane with the ultrahigh specific capacitance by using an electrochemical workstation and a blue battery testing system.
2. The preparation method according to claim 1, wherein the concentration of the agar aqueous solution in the step 1) is 4% by mass, the dissolution temperature is 90-100 ℃, and the concentration of the lithium acetate aqueous solution is 1M, 2M, 3M, or 4M.
3. The method according to claim 1, wherein the concentration of the aqueous solution of PVA in step 2) is 10% by mass, the dissolution temperature is 90-100 ℃, and the concentration of the aqueous solution of lithium acetate is 1M, 2M, 3M, or 4M.
4. The method according to claim 1, wherein the volume ratio of the agar-lithium acetate solution to the PVA-lithium acetate solution in step 3) is 1: 1, the temperature is 90-100 ℃, and the time is 15 min.
5. The preparation method according to claim 1, wherein in the step 4), the gel is uniformly coated to a thickness of about 2mm, and the gel polymer is solidified into a film by hydrogen bonds formed by water molecules and polymer molecular chains and by hydrogen bonds formed by agar molecular chains and PVA molecular chains in the cooling and standing process.
6. The production method according to claim 1, wherein after the gel electrolyte is dried in step 5), a burning test is performed using an alcohol burner.
7. The method according to claim 1, wherein the solid-state supercapacitor is assembled by using activated carbon as an electrode material and a gel electrolyte membrane as an electrolyte in step 6).
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11214037A (en) * | 1998-01-23 | 1999-08-06 | Sony Corp | Gel electrolyte and battery using the same |
| CN107481869A (en) * | 2017-08-11 | 2017-12-15 | 北京大学 | A kind of double-network hydrogel electrolyte and its preparation and application |
| CN108364803A (en) * | 2018-01-10 | 2018-08-03 | 青岛大学 | A kind of fire-retardant method for preparing gel polymer electrolyte of all-solid-state supercapacitor based on lithium alginate |
| CN108546333A (en) * | 2018-03-26 | 2018-09-18 | 中国林业科学研究院林产化学工业研究所 | A kind of preparation of high-mechanical property dual network composite hydrogel |
| CN108598567A (en) * | 2018-04-26 | 2018-09-28 | 吉林大学 | A kind of fire-retardant gel electrolyte, preparation method and its application in lithium ion battery and ultracapacitor |
| CN109994322A (en) * | 2019-03-27 | 2019-07-09 | 中国科学院福建物质结构研究所 | A kind of cell type supercapacitor and application thereof |
-
2020
- 2020-09-02 CN CN202010914302.5A patent/CN112216523A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11214037A (en) * | 1998-01-23 | 1999-08-06 | Sony Corp | Gel electrolyte and battery using the same |
| CN107481869A (en) * | 2017-08-11 | 2017-12-15 | 北京大学 | A kind of double-network hydrogel electrolyte and its preparation and application |
| CN108364803A (en) * | 2018-01-10 | 2018-08-03 | 青岛大学 | A kind of fire-retardant method for preparing gel polymer electrolyte of all-solid-state supercapacitor based on lithium alginate |
| CN108546333A (en) * | 2018-03-26 | 2018-09-18 | 中国林业科学研究院林产化学工业研究所 | A kind of preparation of high-mechanical property dual network composite hydrogel |
| CN108598567A (en) * | 2018-04-26 | 2018-09-28 | 吉林大学 | A kind of fire-retardant gel electrolyte, preparation method and its application in lithium ion battery and ultracapacitor |
| CN109994322A (en) * | 2019-03-27 | 2019-07-09 | 中国科学院福建物质结构研究所 | A kind of cell type supercapacitor and application thereof |
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