CN113096963A - Gel electrolyte aluminum electrolytic capacitor and preparation method thereof - Google Patents
Gel electrolyte aluminum electrolytic capacitor and preparation method thereof Download PDFInfo
- Publication number
- CN113096963A CN113096963A CN202110381406.9A CN202110381406A CN113096963A CN 113096963 A CN113096963 A CN 113096963A CN 202110381406 A CN202110381406 A CN 202110381406A CN 113096963 A CN113096963 A CN 113096963A
- Authority
- CN
- China
- Prior art keywords
- electrolyte
- hydrogel
- capacitor
- gel
- capacitor core
- Prior art date
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- Granted
Links
- 239000003990 capacitor Substances 0.000 title claims abstract description 247
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 122
- 239000011245 gel electrolyte Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000003792 electrolyte Substances 0.000 claims abstract description 129
- 239000000178 monomer Substances 0.000 claims abstract description 67
- 239000007788 liquid Substances 0.000 claims abstract description 64
- 239000003999 initiator Substances 0.000 claims abstract description 40
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 33
- 229920000642 polymer Polymers 0.000 claims abstract description 21
- 239000000017 hydrogel Substances 0.000 claims description 99
- 229920001940 conductive polymer Polymers 0.000 claims description 53
- 239000011888 foil Substances 0.000 claims description 44
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 33
- 239000000654 additive Substances 0.000 claims description 29
- 150000001875 compounds Chemical class 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 29
- 239000002904 solvent Substances 0.000 claims description 29
- 230000000996 additive effect Effects 0.000 claims description 27
- 239000000499 gel Substances 0.000 claims description 26
- 238000001723 curing Methods 0.000 claims description 21
- 239000002202 Polyethylene glycol Substances 0.000 claims description 18
- 229920001223 polyethylene glycol Polymers 0.000 claims description 18
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 17
- 238000004806 packaging method and process Methods 0.000 claims description 16
- -1 r-butyrolactone Chemical compound 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 238000004804 winding Methods 0.000 claims description 14
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000002955 isolation Methods 0.000 claims description 12
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052698 phosphorus Inorganic materials 0.000 claims description 11
- 239000011574 phosphorus Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 9
- 239000004815 dispersion polymer Substances 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- SBVKVAIECGDBTC-UHFFFAOYSA-N 4-hydroxy-2-methylidenebutanamide Chemical compound NC(=O)C(=C)CCO SBVKVAIECGDBTC-UHFFFAOYSA-N 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 7
- 239000005543 nano-size silicon particle Substances 0.000 claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims description 7
- LEJBBGNFPAFPKQ-UHFFFAOYSA-N 2-(2-prop-2-enoyloxyethoxy)ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOC(=O)C=C LEJBBGNFPAFPKQ-UHFFFAOYSA-N 0.000 claims description 6
- KUDUQBURMYMBIJ-UHFFFAOYSA-N 2-prop-2-enoyloxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC(=O)C=C KUDUQBURMYMBIJ-UHFFFAOYSA-N 0.000 claims description 6
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 6
- 150000003863 ammonium salts Chemical class 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
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- 230000000379 polymerizing effect Effects 0.000 claims description 5
- 238000001029 thermal curing Methods 0.000 claims description 5
- CCJAYIGMMRQRAO-UHFFFAOYSA-N 2-[4-[(2-hydroxyphenyl)methylideneamino]butyliminomethyl]phenol Chemical compound OC1=CC=CC=C1C=NCCCCN=CC1=CC=CC=C1O CCJAYIGMMRQRAO-UHFFFAOYSA-N 0.000 claims description 4
- 239000003963 antioxidant agent Substances 0.000 claims description 4
- 230000003078 antioxidant effect Effects 0.000 claims description 4
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- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 239000004642 Polyimide Substances 0.000 claims description 3
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- UUORTJUPDJJXST-UHFFFAOYSA-N n-(2-hydroxyethyl)prop-2-enamide Chemical compound OCCNC(=O)C=C UUORTJUPDJJXST-UHFFFAOYSA-N 0.000 claims description 3
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 claims description 3
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- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims 8
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- 238000011056 performance test Methods 0.000 description 9
- 230000001066 destructive effect Effects 0.000 description 8
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 6
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- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 5
- 229930195725 Mannitol Natural products 0.000 description 5
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 5
- GJYJYFHBOBUTBY-UHFFFAOYSA-N alpha-camphorene Chemical group CC(C)=CCCC(=C)C1CCC(CCC=C(C)C)=CC1 GJYJYFHBOBUTBY-UHFFFAOYSA-N 0.000 description 5
- 239000000594 mannitol Substances 0.000 description 5
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- 238000000926 separation method Methods 0.000 description 5
- FLDCSPABIQBYKP-UHFFFAOYSA-N 5-chloro-1,2-dimethylbenzimidazole Chemical compound ClC1=CC=C2N(C)C(C)=NC2=C1 FLDCSPABIQBYKP-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- 239000001741 Ammonium adipate Substances 0.000 description 4
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical compound NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 4
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 4
- 235000019293 ammonium adipate Nutrition 0.000 description 4
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 4
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 4
- 239000013065 commercial product Substances 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 235000019837 monoammonium phosphate Nutrition 0.000 description 4
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 4
- 150000007524 organic acids Chemical class 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000009658 destructive testing Methods 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 125000003703 phosphorus containing inorganic group Chemical group 0.000 description 3
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- 125000006850 spacer group Chemical group 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
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- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 2
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- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
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- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
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- 229910052739 hydrogen Inorganic materials 0.000 description 2
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- 239000012535 impurity Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
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- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
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- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
- H01G9/045—Electrodes or formation of dielectric layers thereon characterised by the material based on aluminium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/0029—Processes of manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
- H01G9/028—Organic semiconducting electrolytes, e.g. TCNQ
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention relates to the technical field of capacitors, and provides a gel electrolyte aluminum electrolytic capacitor and a preparation method thereof. According to the invention, a monomer, an initiator and a cross-linking agent are utilized to form gel, and an electrolyte is coated in a three-dimensional polymer gel network, so that a gel electrolyte is formed; according to the invention, the gel electrolyte is used for replacing the traditional liquid electrolyte, the gel electrolyte has two properties of liquid and solid, the solid shape can be maintained unchanged, the free passing of ions in the gel is not influenced, and the three-dimensional polymer gel network has high liquid absorption property, so that the liquid leakage is not caused, and the safety of the capacitor can be obviously improved. The gel electrolyte aluminum electrolytic capacitor provided by the invention has the advantages of no liquid leakage of a solid aluminum electrolytic capacitor, generation and repair of an oxide film of a liquid capacitor, strong overvoltage resistance, low failure rate and good reliability and safety of the capacitor.
Description
Technical Field
The invention relates to the technical field of capacitors, in particular to a gel electrolyte aluminum electrolytic capacitor and a preparation method thereof.
Background
In an electronic circuit, a capacitor is an essential basic component as a rectifying or filtering element. The liquid capacitor is a capacitor in which a capacitor core is impregnated with an electrolyte, and the solid-liquid hybrid capacitor is a capacitor in which a solid conductive polymer is attached to a capacitor core, and the capacitor core is impregnated with an electrolyte. The liquid capacitor and the solid-liquid mixed capacitor contain electrolyte, so that a large amount of ion-repaired anode oxide films can be provided, and the product has low leakage current, strong anti-overvoltage capacity and low cost.
However, the liquid capacitor has liquid inside, which is easy to leak, and the safety of the capacitor is low. Although the solid-liquid mixed capacitor has the advantages of solid and liquid capacitors, when the explosion-proof valve of the capacitor is opened under extreme working conditions, liquid electrolyte still has the risk of leakage, can cause the damage of electronic products, and can cause safety accidents seriously.
Disclosure of Invention
In view of the above, the present invention provides a gel electrolyte aluminum electrolytic capacitor and a method for manufacturing the same. The invention provides a gel electrolyte which is used for replacing the traditional liquid electrolyte, the obtained gel electrolyte capacitor does not leak liquid, and has high safety, strong pressure resistance and good high temperature resistance.
In order to achieve the above object, the present invention provides the following technical solutions:
a preparation method of a gel electrolyte aluminum electrolytic capacitor comprises the following steps:
(1) placing the isolation paper between the positive aluminum foil and the negative foil, and then winding the isolation paper into a capacitor core;
(2) impregnating the capacitor core in hydrogel electrolyte, and curing and packaging the impregnated capacitor core to obtain a gel electrolyte aluminum electrolytic capacitor; the components of the hydrogel electrolyte comprise a solvent, a solute, an additive, a monomer, an initiator and a cross-linking agent, and the hydrogel electrolyte does not comprise a compound containing a benzene ring structure;
or, the capacitor core is cured and dried after being impregnated in the hydrogel solution, then the capacitor core is impregnated in the electrolyte, and the impregnated capacitor core is packaged to obtain the gel electrolyte aluminum electrolytic capacitor; the components of the hydrogel solution comprise a solvent, a monomer, an initiator and a cross-linking agent; the electrolyte comprises a solvent, a solute and an additive;
wherein the monomer is a monomer capable of polymerizing into a gel compound.
Preferably, the method further comprises the step of impregnating the capacitor core in the conductive polymer dispersion liquid and then drying the impregnated capacitor core after winding the capacitor core.
Preferably, the components of the hydrogel electrolyte and the hydrogel solution independently further comprise a conductive polymer.
Preferably, the monomers in the hydrogel electrolyte and the hydrogel solution independently comprise one or more of epoxy resin, acrylic resin, dimethylacetamide, dimethylformamide, hydroxyethyl acrylamide, N-hydroxymethyl acrylamide, N-hydroxyethyl acrylamide, monovinyl ether, methyl methacrylate, ethyl methacrylate, hydroxyethyl acrylate and diacetone acrylamide;
the initiators in the hydrogel electrolyte and the hydrogel solution independently comprise one or more of polyamide, polyimide, hydrogen peroxide and azo initiators;
the cross-linking agent in the hydrogel electrolyte and the hydrogel solution independently comprises one or more of polyurethane, ethylene glycol diacrylate, diethylene glycol diacrylate, polyethylene glycol acrylate and polyethylene glycol acrylate.
Preferably, the hydrogel electrolyte, the hydrogel solution and the solvent in the electrolyte independently comprise one or more of ethylene glycol, diethylene glycol, glycerol, polyethylene glycol, r-butyrolactone, sulfolane and water;
the hydrogel electrolyte and the solute in the electrolyte independently comprise one or more of boric acid, borate, organic acid salt, amine salt and ammonium salt;
the additive in the hydrogel electrolyte comprises one or more of a phosphorus-containing compound, a high molecular polymer, nano silicon dioxide and borate;
the additive in the electrolyte comprises one or more of a phosphorus-containing compound, a high molecular polymer, nano silicon dioxide, borate and a compound containing a benzene ring structure.
Preferably, the additives in the hydrogel electrolyte and the electrolyte independently further comprise an antioxidant and/or a chelating agent.
Preferably, in the hydrogel electrolyte and the hydrogel solution, the mass of the cross-linking agent is 5-50% of the mass of the monomer independently, and the mass of the initiator is 0.1-15% of the mass of the monomer independently.
Preferably, in the hydrogel electrolyte, the total mass of the solvent, the solute and the additive is 100%, the mass fraction of the solute is 3-30%, the mass fraction of the additive is 0.1-15%, and the mass fraction of the solvent is 50-95%;
in the hydrogel electrolyte, the mass of a monomer is 5-50% of the total mass of the solvent, the solute and the additive.
Preferably, the curing is thermal curing or photo curing.
The invention also provides the gel electrolyte aluminum electrolytic capacitor prepared by the preparation method of the scheme, which comprises a shell, a capacitor core packaged in the shell and gel electrolyte attached to the capacitor core.
The invention provides a preparation method of a gel electrolyte aluminum electrolytic capacitor, which comprises the following steps: winding an anode aluminum foil, a cathode foil and an isolating paper into a capacitor core, and then impregnating the capacitor core, wherein the impregnation method comprises two impregnation methods, namely one impregnation method is one-time impregnation, namely, the capacitor core is directly impregnated in gel electrolyte, and the gel electrolyte capacitor can be obtained after curing and packaging; the other method is secondary impregnation, namely, the capacitor core is impregnated in a hydrogel solution, the impregnation is carried out in an electrolyte after the curing and drying, and then the gel electrolyte capacitor can be obtained after the encapsulation. The gel electrolyte is used for replacing the traditional liquid electrolyte, is composed of a three-dimensional polymer gel network and an electrolyte, has the properties of liquid and solid, can maintain the shape of the solid unchanged, and does not influence the free passing of ions in the gel; meanwhile, as the three-dimensional polymer gel network is attached to the isolation paper, the density and the thickness of the isolation paper are increased, and the voltage resistance of the capacitor is further improved; in addition, the three-dimensional polymer gel network coats the electrolyte, so that the saturated air pressure in the capacitor can be successfully reduced, the service temperature of the capacitor is improved, the three-dimensional polymer gel network has high liquid absorption performance, liquid leakage cannot be caused, and the safety of the capacitor can be remarkably improved.
In addition, when the one-time impregnation method is adopted, the gel electrolyte does not contain a compound containing a benzene ring structure, the compound containing the benzene ring structure has polymerization inhibition effect on gel polymerization, and the gel electrolyte does not contain the compound containing the benzene ring structure, so that the smooth proceeding of the gel polymerization can be ensured. When the secondary impregnation method is adopted, the hydrogel solution is impregnated firstly, and then the electrolyte is impregnated, and because the gel is polymerized when the electrolyte is impregnated, a compound containing a benzene ring structure can be added into the electrolyte.
Furthermore, conductive polymers can be added into the gel electrolyte or the hydrogel solution, and after the gel is solidified, the conductive polymers are wound in a three-dimensional polymer gel network to form a double-layer conductive electrolyte layer, so that the internal resistance of the capacitor is reduced.
Furthermore, the invention also comprises a step of dipping the capacitor core in the conductive polymer dispersion liquid and then drying after the capacitor core is obtained by winding, so that the conductive polymer is attached to the capacitor core, and then the subsequent dipping of the gel electrolyte is carried out, and the conductive polymer is attached to the capacitor core in a solid state, thereby further reducing the internal resistance of the capacitor.
The invention also provides the gel electrolyte aluminum electrolytic capacitor prepared by the preparation method of the scheme. The gel electrolyte aluminum electrolytic capacitor provided by the invention has the advantages of no liquid leakage of a solid aluminum electrolytic capacitor, generation and repair of an oxide film of a liquid capacitor, strong overvoltage resistance, low failure rate and good reliability and safety of the capacitor.
Detailed Description
The invention provides a preparation method of a gel electrolyte aluminum electrolytic capacitor, which comprises the following steps:
(1) placing the isolation paper between the positive aluminum foil and the negative foil, and then winding the isolation paper into a capacitor core;
(2) impregnating the capacitor core in hydrogel electrolyte, and curing and packaging the impregnated capacitor core to obtain a gel electrolyte aluminum electrolytic capacitor; the components of the hydrogel electrolyte comprise a solvent, a solute, an additive, a monomer, an initiator and a cross-linking agent, and the hydrogel electrolyte does not comprise a compound containing a benzene ring structure;
or, the capacitor core is cured and dried after being impregnated in the hydrogel solution, then the capacitor core is impregnated in the electrolyte, and the impregnated capacitor core is packaged to obtain the gel electrolyte aluminum electrolytic capacitor; the components of the hydrogel solution comprise a solvent, a monomer, an initiator and a cross-linking agent; the electrolyte comprises a solvent, a solute and an additive;
wherein the monomer is a monomer capable of polymerizing into a gel compound.
The invention arranges the isolation paper between the anode aluminum foil and the cathode foil, and then the isolation paper is wound into the capacitor core. In the present invention, the negative electrode foil is preferably an aluminum foil or a carbon foil; in a specific embodiment of the present invention, the positive aluminum foil and the negative aluminum foil are selected according to the specification of the aluminum electrolytic capacitor to be manufactured, using the conventional positive aluminum foil and negative aluminum foil on the market for manufacturing the aluminum electrolytic capacitor.
In the invention, the material of the release paper is preferably fiber or resin, and the fiber is preferably one or more of manila hemp, Spanish grass or artificial fiber; the resin is preferably one or more of polyester resin, polyamide resin, polyimide resin, polypropylene resin and polyethylene resin; in a particular embodiment of the invention, the release paper is preferably kraft paper.
The invention has no special requirement on the winding method, and the winding method known by the technicians in the field can be used, specifically, the separator paper is clamped between the positive aluminum foil and the negative foil, and the tail end is stuck after winding, so that the capacitor core is obtained. In the embodiment of the present invention, before winding, it is preferable to further cut the positive electrode aluminum foil, the negative electrode foil, and the separator paper according to the size of the target capacitor.
After the capacitor core is obtained, the capacitor core is impregnated with the gel electrolyte by two methods, specifically, a one-time impregnation method and a two-time impregnation method, which are respectively described as follows:
in the present invention, the one-time impregnation method comprises the steps of: and impregnating the capacitor core in hydrogel electrolyte, and curing and packaging the impregnated capacitor core to obtain the gel electrolyte aluminum electrolytic capacitor. In the present invention, the components of the hydrogel electrolyte include a solvent, a solute, an additive, a monomer, an initiator, and a crosslinking agent, and the hydrogel electrolyte does not include a compound containing a benzene ring structure.
In the present invention, the solvent in the hydrogel electrolyte preferably includes one or more of ethylene glycol, diethylene glycol, glycerol, polyethylene glycol, r-butyrolactone, sulfolane and water.
In the present invention, the solute in the hydrogel electrolyte preferably includes one or more of boric acid, borate, organic acid salt, amine salt and ammonium salt; the organic acid preferably comprises one or more of formic acid, adipic acid, benzoic acid, azelaic acid, sebacic acid, dodecanedioic acid, 1, 6-decanedicarboxylic acid and 1, 7-sebacic acid, and the organic acid salt is preferably ammonium salt of the organic acid; the amine preferably comprises diethylamine and/or triethylamine; the amine salt preferably comprises triethylammonium maleate; the ammonium salt preferably comprises one or more of ammonium 1, 4-dodecadicarboxylate, ammonium 1, 6-dodecadicarboxylate, tetramethylammonium phthalate and ammonium tetramethylammonium maleate.
In the invention, the additive in the hydrogel electrolyte preferably comprises one or more of a phosphorus-containing compound, a high molecular polymer, nano silicon dioxide and borate; the phosphorus-containing compound preferably comprises one or more of phosphorus-containing organic acid and salt thereof, phosphorus-containing inorganic acid and salt thereof and phosphate ester compounds, the phosphorus-containing organic acid preferably comprises one or more of polyamine polyether phosphonic acid, diethylenetriamine pentamethylene phosphonic acid and hydroxyl ethylidene diphosphonic acid, and the phosphorus-containing organic acid salt is preferably guanylurea phosphate; the phosphorus-containing inorganic acid preferably comprises phosphoric acid and/or hypophosphorous acid, and the phosphorus-containing inorganic acid salt is preferably ammonium hypophosphite. In the present invention, the high molecular polymer preferably includes one or more of polyvinyl alcohol, polyvinylpyrrolidone, mannitol, a polymer of boric acid and polysaccharides, and a polymer of boric acid and alcohols. In the invention, the high molecular polymer and the nano silicon dioxide can improve the sparking voltage of the electrolyte.
In the invention, the additive preferably further comprises an antioxidant and/or a chelating agent, wherein the antioxidant preferably comprises one or more of hydroquinone, allantoin, ferulic acid and cyanuric acid; the chelating agent preferably comprises one or more of aminocarboxylic acid and salt thereof; the aminocarboxylic acid preferably comprises one or more of Ethylene Diamine Tetraacetic Acid (EDTA), diethylenetriamine pentaacetic acid (DTPA) and nitrilotriacetic acid (NTA), and the aminocarboxylate is preferably a sodium salt of an aminocarboxylic acid of the above kind; in the invention, the chelating agent can generate a chelate with the impurity ions, so that the impurity ions are prevented from damaging the generation of an oxide film on the anode aluminum foil, and the service life of the capacitor is prolonged.
In the present invention, the additive in the hydrogel electrolyte cannot be a compound containing a benzene ring structure, which would prevent polymerization of monomers, thereby affecting the formation of a gel. In particular embodiments of the present invention, the compound containing a benzene ring structure may be added after polymerization to form a gel or before encapsulation, or the compound containing a benzene ring structure may be added to the aluminum shell for encapsulation.
In the invention, the monomer in the hydrogel electrolyte is a monomer capable of polymerizing into a gel compound, and preferably comprises one or more of epoxy resin, acrylic resin, dimethylacetamide, dimethylformamide, hydroxyethyl acrylamide, N-hydroxymethyl acrylamide, N-hydroxyethyl acrylamide, monovinyl ether, methyl methacrylate, ethyl methacrylate, hydroxyethyl acrylate and diacetone acrylamide; when the number of the monomers in the hydrogel electrolyte is multiple, the dosage ratio of each monomer is not particularly required, any proportion can be adopted, and in the specific embodiment of the invention, the dosage of each monomer is preferably equal.
In the invention, the initiator in the hydrogel electrolyte preferably comprises one or more of polyamide, polyimide, hydrogen peroxide and azo initiators; the azo initiator is preferably 2, 2-azobis (N-2-hydroxyethyl) -2-methylpropionamide.
In the invention, the cross-linking agent in the hydrogel electrolyte preferably comprises one or more of polyurethane, ethylene glycol diacrylate, diethylene glycol diacrylate, polyethylene glycol acrylate and polyethylene glycol acrylate.
In the invention, the mass fraction of the solute is preferably 3-30%, more preferably 5-25%, the mass fraction of the additive is preferably 0.1-15%, more preferably 1-10%, and the mass fraction of the solvent is preferably 50-95%, more preferably 60-85%, based on 100% of the total mass of the solvent, the solute and the additive in the hydrogel electrolyte; in the hydrogel electrolyte, the mass of the monomer is preferably 5-50% of the total mass of the solvent, the solute and the additive, and more preferably 8-40%; the mass of the cross-linking agent is preferably 5-50%, more preferably 8-40% of the mass of the monomer, and the mass of the initiator is preferably 0.1-15%, more preferably 3-10% of the mass of the monomer. In the embodiment of the present invention, it is preferable that the electrolyte is prepared by using a solvent, a solute and an additive, and then the monomer, the crosslinking agent and the initiator are added to the electrolyte to obtain the hydrogel electrolyte.
In the invention, the components of the hydrogel electrolyte preferably further comprise a conductive polymer, and the conductive polymer preferably comprises one or more of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid (PEDOT/PSS), polyaniline-polystyrene sulfonic acid and polypyrrole-polystyrene sulfonic acid; in the present invention, the conductive polymer is preferably used in the form of an aqueous conductive polymer dispersion, specifically, an aqueous poly-3, 4-ethylenedioxythiophene-polystyrenesulfonic acid dispersion, an aqueous polyaniline-polystyrenesulfonic acid dispersion, or an aqueous polypyrrole-polystyrenesulfonic acid dispersion; the invention has no special requirement on the source of the conductive polymer aqueous dispersion liquid, and can adopt a commercial product; in a specific embodiment of the present invention, the aqueous dispersion of poly 3, 4-ethylenedioxythiophene-polystyrene sulfonic acid is preferably an aqueous dispersion of Shenzhen New aegis corporation model number PEDT 201.
In the invention, the mass fraction of the conductive polymer in the conductive polymer aqueous dispersion liquid is preferably 0.5-5%; according to the invention, the conductive polymer aqueous dispersion liquid is preferably directly added into the gel electrolyte; the addition amount of the conductive polymer aqueous dispersion liquid is preferably 20-50% of the total mass of the solvent, the solute and the additive in the hydrogel electrolyte, and is preferably 30%.
The capacitor core is impregnated in the hydrogel electrolyte, and then the impregnated capacitor core is cured and packaged to obtain the hydrogel electrolyte capacitor. In the invention, the impregnation is specifically to soak the capacitor core in the hydrogel electrolyte, and the invention has no special requirement on the soaking time and is suitable for full soaking; the hydrogel electrolyte is absorbed in the release paper by impregnation.
In the present invention, the curing is preferably thermal curing or photo curing, and the specific curing conditions are preferably determined according to the kind of the initiator. In the specific embodiment of the invention, when the initiator is a thermal initiator, the curing method is thermal curing, the thermal curing temperature is preferably 75-120 ℃, and the curing time is preferably 0.1-2 h; when the initiator is a photoinitiator, the curing method is photocuring, the photocuring condition is preferably 0.1-2 hours of illumination, and the invention has no special requirement on a light source for illumination as long as polymerization can be initiated; in the present invention, a light source known to those skilled in the art may be used, specifically, a high-pressure mercury lamp, an LED lamp, an ultraviolet lamp, and the like. During the curing process, the monomers polymerize under the action of the initiator and the crosslinking agent to form a gel.
The packaging method has no special requirement, and the capacitor core is packaged by a method known by the technical personnel in the field, specifically, the capacitor core impregnated with electrolyte is placed in an aluminum shell, and then the capacitor core is packaged by a rubber plug.
The invention has no requirement on the sequence of curing and packaging, can be cured firstly and then packaged, and can also be packaged firstly and then cured, and the invention does not have specific requirements.
In the present invention, the secondary impregnation method includes the steps of: and (3) impregnating the capacitor core in a hydrogel solution, curing and drying, then impregnating in an electrolyte, and packaging the impregnated capacitor core to obtain the gel electrolyte aluminum electrolytic capacitor.
In the invention, the components of the hydrogel solution comprise a solvent, a monomer, an initiator and a cross-linking agent, and the selectable types of the solvent, the monomer, the initiator and the cross-linking agent are consistent with the selectable types of the solvent, the monomer, the initiator and the cross-linking agent in the hydrogel electrolyte in the scheme, and are not described again; in the hydrogel solution, the mass of the cross-linking agent is preferably 5-50% of the mass of the monomer, more preferably 8-40%, and the mass of the initiator is preferably 0.1-15% of the mass of the monomer, more preferably 3-10%; the mass fraction of the monomers in the hydrogel solution is preferably 8-30%.
In the present invention, the components of the hydrogel solution preferably further include a conductive polymer; the types of the conductive macromolecules are consistent with the scheme, and are not described again; the conductive polymer is preferably used in the form of conductive polymer aqueous dispersion liquid, the type and concentration of the conductive polymer aqueous dispersion liquid are consistent with the scheme, and the description is omitted; in a specific embodiment of the present invention, when the hydrogel electrolyte includes a conductive polymer, it is preferable to directly add a monomer, a crosslinking agent, and an initiator to the aqueous dispersion of the conductive polymer, so as to obtain a hydrogel solution including the conductive polymer; the addition amount of the monomer is preferably 15-25% of the mass of the conductive polymer aqueous dispersion liquid, and more preferably 20%.
The capacitor core is impregnated in the hydrogel solution and then cured and dried. In the present invention, the impregnation operation method is preferably consistent with the above scheme, and is not described herein again; the curing method and conditions are consistent with the scheme, and are not described again; the invention has no special requirements on the drying condition, and can remove the moisture in the solidified gel.
After drying, the capacitor core adhered with the xerogel is impregnated in the electrolyte, and the impregnated capacitor core is packaged to obtain the gel electrolyte aluminum electrolytic capacitor. In the invention, the components of the electrolyte comprise a solvent, a solute and an additive; the types of the solvent and the solute in the electrolyte are preferably consistent with those of the hydrogel electrolyte in the scheme, and are not repeated herein; the additive in the electrolyte preferably comprises one or more of a phosphorus-containing compound, a high molecular polymer, nano silicon dioxide, borate and a compound containing a benzene ring structure; the types of the phosphorus-containing compound and the high molecular polymer are preferably consistent with the scheme, and are not described again; the compound containing the benzene ring structure preferably comprises one or more of p-nitrobenzoic acid, p-nitrophenol, p-nitrobenzol and m-nitrophenol; in the invention, the compound containing the benzene ring structure has a hydrogen absorption function, so that the internal pressure of the capacitor can be reduced, the safety of the capacitor is improved, and the service life of the capacitor is prolonged. In the secondary impregnation method of the present invention, the gel is prepared first, and then the electrolyte is adsorbed by utilizing the adsorption swelling property of the gel, and since the gel is already polymerized, a compound containing a benzene ring structure may be added to the electrolyte.
In the present invention, the impregnation method is consistent with the above scheme, and is not described herein again, and during the impregnation process, the electrolyte is adsorbed by using the good adsorption swelling property of the gel. In the present invention, the encapsulation method is preferably consistent with the above scheme, and is not described herein again.
In the present invention, it is preferable that the capacitor element is impregnated with the gel electrolyte, and the wound capacitor element is impregnated with the conductive polymer dispersion and then dried. In the present invention, the conductive polymer dispersion is specifically the conductive polymer aqueous dispersion according to the above-mentioned scheme, and is not described herein again; the invention has no special requirement on the impregnation, and the capacitor core can be fully soaked in the conductive polymer dispersion liquid.
In the present invention, the number of impregnation and drying is preferably 2 or more, preferably 2 to 5, and more preferably 2 to 3, and the two impregnation and drying are exemplified as follows: the capacitor core is firstly impregnated in the conductive polymer solution for the first time and then dried, and the dried capacitor core is impregnated in the conductive polymer solution for the second time and then dried again. The invention improves the adhesion amount of the conductive polymer on the capacitor core through multiple impregnation drying, and obtains the capacitor core with lower internal resistance.
The invention also provides the gel electrolyte aluminum electrolytic capacitor prepared by the preparation method of the scheme. In the invention, the gel electrolyte aluminum electrolytic capacitor comprises a shell, a capacitor core encapsulated in the shell and gel electrolyte attached on the capacitor core; the capacitor core comprises an anode aluminum foil, a cathode foil and isolation paper arranged between the anode aluminum foil and the cathode foil, and the gel electrolyte is specifically attached to the isolation paper of the capacitor core; the gel electrolyte consists of a three-dimensional polymer gel network and electrolyte absorbed in the gel network; the three-dimensional polymer gel network is formed by polymerizing monomers; further, when the hydrogel electrolyte or the hydrogel solution further comprises a conductive polymer, the three-dimensional polymer gel network skeleton is further doped with the conductive polymer, so that a capacitor with lower internal resistance is obtained; furthermore, a conductive polymer layer is attached to the surface of the capacitor core, so that the internal resistance of the capacitor is further reduced.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
The gel electrolyte aluminum electrolytic capacitor prepared in this example had a rated capacitance/rated voltage of 1000UF/10V, a size (diameter) of 8mm by 14mm, a commercially available aluminum foil for the positive electrode, a type of 14VF, and a specific volume of 130UF/cm2The negative foil is commercially available negative foil with a model of 1V and a specific volume of 350UF/cm2The spacer between the aluminum foils of the positive and negative electrodes was a commercial electrolytic paper (Kane corporation, model MJ255-40), the size of the aluminum package was 8mm 14.5mm, and the thickness of the rubber plug was 3.0 mm.
The preparation steps are as follows:
(1) and (3) placing the separation paper between the positive aluminum foil and the negative foil, and then winding the separation paper into a capacitor core with the specification of 1000 UF/10V.
(2) Impregnating the capacitor core with hydrogel electrolyte, wherein the hydrogel electrolyte is prepared from electrolyte, a monomer, a cross-linking agent and an initiator, and the electrolyte comprises the following components in percentage by mass: 50% of ethylene glycol, 41% of pure water, 8% of ammonium adipate, 0.5% of ammonium dihydrogen phosphate and 0.5% of EDTA; the electrolyte is added with polymerized monomer hydroxyethyl acrylate (the addition amount of the hydroxyethyl acrylate is 20% of the mass of the electrolyte), crosslinking agent polyethylene glycol bisacrylamide (the addition amount is 20% of the mass of the monomer), and initiator hydrogen peroxide (the addition amount is 3% of the mass of the monomer).
(3) And packaging the capacitor core impregnated with the hydrogel electrolyte by using an aluminum shell and a rubber plug, and thermally curing at 95 ℃ for 1h to obtain the gel electrolyte aluminum electrolytic capacitor.
Preparing 100 gel electrolyte aluminum electrolytic capacitors, aging the obtained capacitors, and randomly selecting 10 capacitors for electrical performance test, wherein the capacity, the loss and the performance are tested by using an LCR digital bridge; impedance is tested using an LCR bridge; testing the leakage current by using a leakage current tester; the service life is characterized by the capacity of the capacitor after 2000 hours of load at the rated voltage and the temperature of 105 ℃; destructive testing was performed by rapid reverse charging to see if leakage occurred.
The test results are shown in table 1:
TABLE 1 random test results of electrical properties of gel electrolyte aluminum electrolytic capacitors
According to the data in the table 1, the gel electrolyte aluminum electrolytic capacitor prepared by the invention has low loss, small leakage current and small impedance, the capacity can reach over 900UF after being loaded for 2000 hours at 10V and 105 ℃, which shows that the gel electrolyte aluminum electrolytic capacitor has longer service life, no leakage phenomenon exists after destructive test, which shows that the gel electrolyte aluminum electrolytic capacitor is not easy to leak liquid and has better safety.
Example 2
Other conditions were the same as in example 1 except that only the monomer was polymerized, and the monomer polymerized in example 1, hydroxyethyl acrylate, was changed to hydroxyethyl acrylamide.
Preparing 100 gel electrolyte aluminum electrolytic capacitors, aging the obtained capacitors, and randomly selecting 10 capacitors for electrical performance test, wherein the capacity, the loss and the performance are tested by using an LCR digital bridge; impedance is tested using an LCR bridge; testing the leakage current by using a leakage current tester; the service life is characterized by the capacity of the capacitor after 2000 hours of load at the rated voltage and the temperature of 105 ℃; destructive testing was performed by rapid reverse charging to see if leakage occurred.
The test results are shown in table 2:
TABLE 2 random test results of electrical properties of gel electrolyte aluminum electrolytic capacitors
According to the data in the table 2, the gel electrolyte aluminum electrolytic capacitor prepared by the invention has low loss, small leakage current and small impedance, the capacity can reach over 900UF after being loaded for 2000 hours at 10V and 105 ℃, which shows that the gel electrolyte aluminum electrolytic capacitor has longer service life, no leakage phenomenon exists after destructive test, which shows that the gel electrolyte aluminum electrolytic capacitor is not easy to leak liquid and has better safety.
Example 3
Other conditions were the same as in example 1, except that only the monomers were polymerized, the hydroxyethyl acrylate in example 1 was changed to hydroxyethyl acrylamide and ethyl methacrylate, the total weight of the mixture of hydroxyethyl acrylamide and ethyl methacrylate was the same as that of the hydroxyethyl acrylate in example 1, and the weight ratio of hydroxyethyl acrylamide to ethyl methacrylate was 1: 1.
Preparing 100 gel electrolyte aluminum electrolytic capacitors, aging the obtained capacitors, and randomly selecting 10 capacitors for electrical performance test, wherein the capacity, the loss and the performance are tested by using an LCR digital bridge; impedance is tested using an LCR bridge; testing the leakage current by using a leakage current tester; the service life is characterized by the capacity of the capacitor after 2000 hours of load at the rated voltage and the temperature of 105 ℃; destructive testing was performed by rapid reverse charging to see if leakage occurred.
The test results are shown in table 3:
TABLE 3 random test results of electrical properties of gel electrolyte aluminum electrolytic capacitors
According to the data in the table 3, the gel electrolyte aluminum electrolytic capacitor prepared by the invention has low loss, small leakage current and small impedance, the capacity can reach over 900UF after being loaded for 2000 hours at 10V and 105 ℃, which shows that the gel electrolyte aluminum electrolytic capacitor has longer service life, no leakage phenomenon exists after destructive test, which shows that the gel electrolyte aluminum electrolytic capacitor is not easy to leak liquid and has better safety.
Comparative example 1
The other steps are the same as those of the embodiment 1, and only the step (2) is changed into the following steps: the capacitor core is impregnated with electrolyte, and the electrolyte comprises the following components: 50% of ethylene glycol, 41% of pure water, 8% of ammonium adipate, 0.5% of ammonium dihydrogen phosphate and 0.5% of EDTA, and packaging the impregnated capacitor core by using an aluminum shell and a rubber plug; namely, the monomer, the initiator and the crosslinking agent in example 1 were omitted, and the obtained capacitor was a general liquid aluminum electrolytic capacitor.
Totally 100 liquid aluminum electrolytic capacitors are prepared, 10 capacitors are randomly selected after aging for electrical performance test, and the test method is consistent with that of the embodiment 1.
The results are shown in Table 4.
TABLE 4 random test results of electrical properties of liquid aluminum electrolytic capacitor
According to the data in table 4, it can be seen that the liquid aluminum electrolytic capacitor obtained in comparative example 1 has low loss, small leakage current, small impedance and long service life, but the leakage occurs after destructive test, and the safety of the capacitor is low.
Example 4
The gel electrolyte aluminum electrolytic capacitor prepared in this example had a rated capacitance/rated voltage of 10UF/400V, a size (diameter) of 10mm by 16mm, a commercially available aluminum foil for the positive electrode, a model of 560VF, and a specific volume of 0.7UF/cm2The negative foil is commercially available negative foil with a model of 3V and a specific volume of 100UF/cm2The spacer between the positive and negative aluminum foils was made of commercially available electrolytic paper (Kene corporation, model Ws280-60), the size of the aluminum casing was 10mm 16.5mm, and the thickness of the rubber plug was 3.0 mm.
The preparation steps are as follows:
(1) and (3) placing the separation paper between the positive aluminum foil and the negative foil, and then winding the separation paper into a capacitor core with the specification of 10 UF/400V.
(2) Impregnating the capacitor core with hydrogel electrolyte, wherein the hydrogel electrolyte is prepared from electrolyte, a monomer, a cross-linking agent and an initiator, and the electrolyte comprises the following components in percentage by mass: 80% of ethylene glycol, 5% of pure water, 4.9% of polyethylene glycol, 8% of 1, 6-dodecanedioic acid ammonium, 2% of mannitol and 0.1% of ammonium hypophosphite; the electrolyte is added with polymerized monomer hydroxyethyl acrylate (the addition amount of the hydroxyethyl acrylate is 20% of the mass of the electrolyte), crosslinking agent polyethylene glycol bisacrylamide (the addition amount is 20% of the mass of the monomer), and initiator 2, 2-azo bis (N-2-hydroxyethyl) -2-methacrylamide (the addition amount is 3% of the mass of the monomer).
(3) And (3) thermally curing the capacitor core impregnated with the hydrogel electrolyte at 95 ℃ for 1h, and then packaging with an aluminum shell (the aluminum shell is added with a hydrogen absorbing agent p-nitrobenzol) and a rubber plug to obtain the gel electrolyte aluminum electrolytic capacitor.
Totally 100 gel electrolyte aluminum electrolytic capacitors are prepared, 10 capacitors are randomly selected after aging for electrical performance test, and the test method is consistent with that of the embodiment 1.
The test results are shown in table 5:
TABLE 5 random test results of electrical properties of gel electrolyte aluminum electrolytic capacitors
According to the data in table 5, the gel electrolyte aluminum electrolytic capacitor prepared by the invention has low loss, small leakage current and small impedance, and the capacity can reach over 9.0UF after being loaded for 2000 hours at 400V and 105 ℃, which shows that the gel electrolyte aluminum electrolytic capacitor has longer service life, no leakage phenomenon after destructive test, and better safety.
Example 5
(1) The specification and the manufacturing method of the capacitor core were the same as those of example 4, and a capacitor core having a size of 10mm by 16mm and 10UF/400V was obtained.
(2) The capacitor core is firstly impregnated with a hydrogel solution containing conductive macromolecules, the hydrogel solution is prepared from conductive macromolecule aqueous dispersion, a monomer, an initiator and a cross-linking agent, the conductive polymer aqueous dispersion liquid adopts 3, 4-ethylenedioxythiophene-polystyrene sulfonic acid aqueous dispersion liquid (a commercial product, purchased from Shenzhen New Zealand company, model number is PEDT201, the mass fraction of the conductive polymer in the dispersion liquid is 1.5%), polymerized monomer hydroxyethyl acrylate (the addition amount is 20% of the mass of the conductive polymer aqueous dispersion liquid), cross-linking agent polyethylene glycol bisacrylamide (the addition amount is 20% of the mass of the monomer), and initiator 2, 2-azobis (N-2-hydroxyethyl) -2-methacrylamide (the addition amount is 3% of the mass of the monomer) are added into the conductive polymer aqueous dispersion liquid. The impregnated capacitor core was thermally cured at 95 ℃ for 1 hour, and then dried and dehydrated.
Impregnating the capacitor core adhered with the xerogel with electrolyte, wherein the electrolyte comprises the following components in percentage by mass: 80% of ethylene glycol, 5% of pure water, 4.3% of polyethylene glycol, 8% of 1, 6-ammonium dodecanedioate, 2% of mannitol, 0.1% of ammonium hypophosphite, 0.5% of p-nitrobenzyl alcohol and 0.1% of hydroquinone.
(3) And packaging the capacitor core impregnated with the electrolyte by using an aluminum shell and a rubber plug to obtain the gel electrolyte aluminum electrolytic capacitor.
Totally 100 gel electrolyte aluminum electrolytic capacitors are prepared, 10 capacitors are randomly selected after aging for electrical performance test, and the test method is consistent with that of the embodiment 1.
The test results are shown in table 6:
TABLE 6 random test results of electrical properties of gel electrolyte aluminum electrolytic capacitors
According to the data in table 6, the gel electrolyte aluminum electrolytic capacitor prepared by the invention has low loss and small leakage current, and the impedance of the obtained capacitor is extremely low due to the addition of the conductive polymer in the embodiment; after the gel electrolyte aluminum electrolytic capacitor is loaded for 2000 hours at 400V and 105 ℃, the capacity of the capacitor can reach over 9.0UF, which shows that the gel electrolyte aluminum electrolytic capacitor has longer service life, no liquid leakage phenomenon exists after destructive tests, and shows that the gel electrolyte aluminum electrolytic capacitor is not easy to cause liquid leakage and has better safety.
Example 6
(1) The specification and the manufacturing method of the capacitor core were the same as those of example 4, and a capacitor core having a size of 10mm by 16mm and 10UF/400V was obtained.
(2) The capacitor core is impregnated with a hydrogel electrolyte added with a conductive polymer, wherein the hydrogel electrolyte is prepared from an electrolyte, a conductive polymer aqueous dispersion, a monomer, a cross-linking agent and an initiator, and the electrolyte comprises the following components in percentage by mass: 80% of ethylene glycol, 5% of pure water, 4.9% of polyethylene glycol, 8% of 1, 6-dodecanedioic acid ammonium, 2% of mannitol and 0.1% of ammonium hypophosphite; the electrolyte is added with polymerized monomer hydroxyethyl acrylate (the addition amount is 20 percent of the mass of the electrolyte), cross-linking agent polyethylene glycol bisacrylamide (the addition amount is 20 percent of the mass of the monomer), and polymerization initiator 2, 2-azo bis (N-2-hydroxyethyl) -2-methacrylamide (the addition amount is 3 percent of the mass of the monomer); the conductive polymer dispersion liquid is poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid aqueous dispersion liquid, the aqueous dispersion liquid adopts a commercial product, is purchased from Shenzhen New Zezhou nation company, and has the model of PEDT201, the mass fraction of the conductive polymer in the dispersion liquid is 1.5%, and the addition amount of the conductive polymer dispersion liquid is 30% of the mass of the electrolyte.
(3) And packaging the impregnated capacitor core by using an aluminum shell and a rubber plug, and thermally curing at 95 ℃ for 1h to obtain the gel electrolyte aluminum electrolytic capacitor.
Totally 100 gel electrolyte aluminum electrolytic capacitors are prepared, 10 capacitors are randomly selected after aging for electrical performance test, and the test method is consistent with that of the embodiment 1.
The test results are shown in table 7:
TABLE 7 random test results of electrical properties of gel electrolyte aluminum electrolytic capacitors
According to the data in table 7, the gel electrolyte aluminum electrolytic capacitor prepared by the invention has low loss and small leakage current, and the impedance of the obtained capacitor is extremely low due to the addition of the conductive polymer in the embodiment, and the capacity of the capacitor can reach over 9.0UF after the capacitor is loaded for 2000 hours at 400V and 105 ℃, which indicates that the gel electrolyte aluminum electrolytic capacitor has a long service life, and no leakage phenomenon exists after destructive tests, which indicates that the gel electrolyte aluminum electrolytic capacitor is not easy to leak, and has better safety.
Comparative example 2
Other conditions were the same as in example 4, except that the step (2) was changed to: impregnating the capacitor core obtained in the step (1) with electrolyte, wherein the electrolyte comprises the following components in percentage by mass: 80% of ethylene glycol, 5% of pure water, 4.9% of polyethylene glycol, 8% of 1, 6-ammonium dodecanedioate, 2% of mannitol and 0.1% of ammonium hypophosphite, and packaging the impregnated capacitor core by using an aluminum shell and a rubber plug. Namely, the step of impregnating the hydrogel solution in example 2 is omitted, and the obtained capacitor is a common liquid aluminum electrolytic capacitor.
Totally 100 liquid aluminum electrolytic capacitors are prepared, 10 capacitors are randomly selected after aging for electrical performance test, and the test method is consistent with that of the embodiment 1.
The results are shown in Table 8.
TABLE 8 random test results of electrical properties of liquid aluminum electrolytic capacitor
As can be seen from the data in Table 8, the liquid aluminum electrolytic capacitor obtained in comparative example 2 has low loss, small leakage current and long service life, but the impedance is increased compared with example 4, leakage occurs after destructive test, and the safety of the capacitor is low.
Example 7
The gel electrolyte aluminum electrolytic capacitor prepared in this example had a rated capacitance/rated voltage of 100UF/35V, a size (diameter) of 6.3mm by 12mm, a commercially available aluminum foil for the positive electrode, a model of 51VF, and a specific volume of 22UF/cm2The negative foil is commercial carbon foil with a model of 0V and a specific volume of 2000UF/cm2The spacer between the positive and negative aluminum foils was a commercially available electrolytic paper (Kene corporation, model SM255-40), the size of the aluminum casing was 6.3mm 12mm, and the plug thickness was 2.0 mm.
The preparation steps are as follows:
(1) and (3) placing the separation paper between the positive aluminum foil and the negative foil, and then winding to obtain the capacitor core with the specification of 100UF/35V and the size of 6.3mm by 12 mm.
(2) And (3) impregnating the capacitor core with a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid dispersion (a commercial product, purchased from Shenzhen New aegium corporation, the model number of which is PED-201), drying, and then impregnating and drying again to obtain the capacitor core attached with the conductive polymer.
(3) Impregnating a capacitor core attached with a conductive polymer with hydrogel electrolyte, wherein the hydrogel electrolyte is prepared from the electrolyte, a monomer, an initiator and a cross-linking agent, and comprises the following components in percentage by mass: 40% of ethylene glycol, 50% of pure water, 8% of ammonium adipate, 1% of ammonium dihydrogen phosphate and 1% of EDTA; the electrolyte is added with N-hydroxymethyl acrylamide monomer (the addition amount is 20% of the mass of the electrolyte), cross-linking agent polyethylene glycol acrylate (the addition amount is 30% of the mass of the monomer), and initiator 2, 2-azo bis (N-2-hydroxyethyl) -2-methacrylamide (the addition amount is 1% of the mass of the monomer).
(4) And packaging the impregnated capacitor core with an aluminum shell and a rubber plug, and heating and curing at 110 ℃ for 2h to obtain the gel electrolyte aluminum electrolytic capacitor.
Preparing 100 gel electrolyte aluminum electrolytic capacitors, aging the obtained capacitors, and randomly selecting 10 capacitors for electrical property test; the testing method of the capacity, the loss, the leakage current and the impedance is consistent with that of the embodiment 1, and the service life is characterized by appearance change of the capacitor after being loaded for 1000 hours at the rated voltage and the temperature of 115 ℃; and (4) observing whether liquid leaks or not under the conditions of overpressure and over-temperature (40V and 125 ℃) and load for 500 h.
The test results are shown in table 9:
TABLE 9 random test results of electrical properties of gel electrolyte aluminum electrolytic capacitors
According to the data in table 9, it can be seen that the capacitor prepared in this embodiment has low loss, small leakage current, and extremely low impedance, and has no change in appearance after being loaded for 1000 hours at 35V and 115 ℃, and has no change in appearance and no leakage phenomenon after being loaded for 500 hours under the overvoltage and overtemperature conditions, which indicates that the capacitor prepared in this embodiment has high safety.
Comparative example 3
Other conditions were the same as in example 7 except that step (3) was changed to: impregnating the capacitor core attached with the conductive polymer obtained in the step (2) with electrolyte, wherein the electrolyte comprises the following components in percentage by mass: 40% of ethylene glycol, 50% of pure water, 8% of ammonium adipate, 1% of ammonium dihydrogen phosphate and 1% of EDTA, and packaging the impregnated capacitor core by using an aluminum shell and a rubber plug. Namely, the monomer, the initiator and the crosslinking agent in example 7 were omitted, and the obtained capacitor was a general solid-liquid mixed aluminum electrolytic capacitor.
Totally 100 solid-liquid mixed aluminum electrolytic capacitors are prepared, 10 capacitors are randomly selected after aging for electrical performance test, and the test method is consistent with that of the embodiment 7.
The test results are shown in table 10:
TABLE 10 random test results of electrical properties of solid-liquid mixed aluminum electrolytic capacitor
As can be seen from Table 10, the obtained solid-liquid mixed aluminum electrolytic capacitor has the phenomena of rubber plug protrusion and liquid leakage after being loaded for 500 hours under the conditions of overvoltage and overtemperature.
As can be seen from the above examples and comparative examples, the electrolyte in the capacitor prepared by the examples of the present invention is a gel electrolyte, and no liquid leakage occurs under the condition that the explosion-proof valve is opened, thereby successfully improving the reliability of the product; the aluminum electrolytic capacitors (liquid aluminum electrolytic capacitors and solid-liquid mixed aluminum electrolytic capacitors) without the gel electrolyte have the liquid leakage phenomenon; in addition, the embodiment of adding the conductive polymer into the hydrogel electrolyte (or the hydrogel solution) and the embodiment of attaching the conductive polymer on the capacitor core can prevent the liquid leakage and simultaneously has extremely low internal resistance.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a gel electrolyte aluminum electrolytic capacitor comprises the following steps:
(1) placing the isolation paper between the positive aluminum foil and the negative foil, and then winding the isolation paper into a capacitor core;
(2) impregnating the capacitor core in hydrogel electrolyte, and curing and packaging the impregnated capacitor core to obtain a gel electrolyte aluminum electrolytic capacitor; the components of the hydrogel electrolyte comprise a solvent, a solute, an additive, a monomer, an initiator and a cross-linking agent, and the hydrogel electrolyte does not comprise a compound containing a benzene ring structure;
or, the capacitor core is cured and dried after being impregnated in the hydrogel solution, then the capacitor core is impregnated in the electrolyte, and the impregnated capacitor core is packaged to obtain the gel electrolyte aluminum electrolytic capacitor; the components of the hydrogel solution comprise a solvent, a monomer, an initiator and a cross-linking agent; the electrolyte comprises a solvent, a solute and an additive;
wherein the monomer is a monomer capable of polymerizing into a gel compound.
2. The method according to claim 1, further comprising a step of impregnating the conductive polymer dispersion liquid with the capacitor core and drying the impregnated capacitor core after winding the capacitor core.
3. The method according to claim 1, wherein the components of the hydrogel electrolyte and the hydrogel solution independently further comprise a conductive polymer.
4. The preparation method according to claim 1 or 3, wherein the monomers in the hydrogel electrolyte and the hydrogel solution independently comprise one or more of epoxy resin, acrylic resin, dimethylacetamide, dimethylformamide, hydroxyethyl acrylamide, N-hydroxymethyl acrylamide, N-hydroxyethyl acrylamide, monovinyl ether, methyl methacrylate, ethyl methacrylate, hydroxyethyl acrylate and diacetone acrylamide;
the initiators in the hydrogel electrolyte and the hydrogel solution independently comprise one or more of polyamide, polyimide, hydrogen peroxide and azo initiators;
the cross-linking agent in the hydrogel electrolyte and the hydrogel solution independently comprises one or more of polyurethane, ethylene glycol diacrylate, diethylene glycol diacrylate, polyethylene glycol acrylate and polyethylene glycol acrylate.
5. The method of claim 1, wherein the hydrogel electrolyte, the hydrogel solution and the solvent in the electrolyte independently comprise one or more of ethylene glycol, diethylene glycol, glycerol, polyethylene glycol, r-butyrolactone, sulfolane and water;
the hydrogel electrolyte and the solute in the electrolyte independently comprise one or more of boric acid, borate, organic acid salt, amine salt and ammonium salt;
the additive in the hydrogel electrolyte comprises one or more of a phosphorus-containing compound, a high molecular polymer, nano silicon dioxide and borate;
the additive in the electrolyte comprises one or more of a phosphorus-containing compound, a high molecular polymer, nano silicon dioxide, borate and a compound containing a benzene ring structure.
6. The method according to claim 5, wherein the additives in the hydrogel electrolyte and the electrolyte independently further include an antioxidant and/or a chelating agent.
7. The method according to claim 1, wherein the mass of the crosslinking agent is 5 to 50% of the mass of the monomer and the mass of the initiator is 0.1 to 15% of the mass of the monomer in the hydrogel electrolyte solution and the hydrogel solution.
8. The preparation method according to claim 1, wherein in the hydrogel electrolyte, the mass fraction of the solute is 3 to 30%, the mass fraction of the additive is 0.1 to 15%, and the mass fraction of the solvent is 50 to 95%, based on 100% of the total mass of the solvent, the solute and the additive;
in the hydrogel electrolyte, the mass of a monomer is 5-50% of the total mass of the solvent, the solute and the additive.
9. The method of claim 1, wherein the curing is thermal curing or photo curing.
10. The gel electrolyte aluminum electrolytic capacitor prepared by the preparation method of any one of claims 1 to 9, comprising a housing, a capacitor core encapsulated in the housing, and a gel electrolyte attached to the capacitor core.
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