CN114664568A - Method for reducing equivalent series resistance of laminated capacitor - Google Patents
Method for reducing equivalent series resistance of laminated capacitor Download PDFInfo
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- CN114664568A CN114664568A CN202210482676.3A CN202210482676A CN114664568A CN 114664568 A CN114664568 A CN 114664568A CN 202210482676 A CN202210482676 A CN 202210482676A CN 114664568 A CN114664568 A CN 114664568A
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- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000003990 capacitor Substances 0.000 title claims abstract description 38
- 230000001590 oxidative effect Effects 0.000 claims abstract description 98
- 239000011888 foil Substances 0.000 claims abstract description 94
- 239000000178 monomer Substances 0.000 claims abstract description 66
- 238000001035 drying Methods 0.000 claims abstract description 37
- 238000005470 impregnation Methods 0.000 claims abstract description 27
- 238000007664 blowing Methods 0.000 claims abstract description 23
- 230000003647 oxidation Effects 0.000 claims abstract description 17
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 16
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000007800 oxidant agent Substances 0.000 claims description 14
- 239000002019 doping agent Substances 0.000 claims description 13
- 150000003839 salts Chemical class 0.000 claims description 12
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 12
- 239000012752 auxiliary agent Substances 0.000 claims description 11
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 9
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 claims description 8
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical class OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- HOMQUHGCYPKWEY-UHFFFAOYSA-N 1,3-dioxo-1h,3h-benzo[de]isochromene-6-sulfonic acid Chemical compound O=C1OC(=O)C2=CC=CC3=C2C1=CC=C3S(=O)(=O)O HOMQUHGCYPKWEY-UHFFFAOYSA-N 0.000 claims description 4
- UNDJACIXRKPCJI-UHFFFAOYSA-N 3-carbamoylbenzenesulfonic acid Chemical compound NC(=O)C1=CC=CC(S(O)(=O)=O)=C1 UNDJACIXRKPCJI-UHFFFAOYSA-N 0.000 claims description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- 239000012286 potassium permanganate Substances 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 235000009518 sodium iodide Nutrition 0.000 claims description 4
- 229930192474 thiophene Natural products 0.000 claims description 4
- ICLYJLBTOGPLMC-KVVVOXFISA-N (z)-octadec-9-enoate;tris(2-hydroxyethyl)azanium Chemical compound OCCN(CCO)CCO.CCCCCCCC\C=C/CCCCCCCC(O)=O ICLYJLBTOGPLMC-KVVVOXFISA-N 0.000 claims description 3
- 229920002126 Acrylic acid copolymer Polymers 0.000 claims description 3
- 108010077895 Sarcosine Proteins 0.000 claims description 3
- 125000001931 aliphatic group Chemical group 0.000 claims description 3
- 125000003118 aryl group Chemical group 0.000 claims description 3
- AXZAYXJCENRGIM-UHFFFAOYSA-J dipotassium;tetrabromoplatinum(2-) Chemical compound [K+].[K+].[Br-].[Br-].[Br-].[Br-].[Pt+2] AXZAYXJCENRGIM-UHFFFAOYSA-J 0.000 claims description 3
- FYMCOOOLDFPFPN-UHFFFAOYSA-K iron(3+);4-methylbenzenesulfonate Chemical compound [Fe+3].CC1=CC=C(S([O-])(=O)=O)C=C1.CC1=CC=C(S([O-])(=O)=O)C=C1.CC1=CC=C(S([O-])(=O)=O)C=C1 FYMCOOOLDFPFPN-UHFFFAOYSA-K 0.000 claims description 3
- 229940049964 oleate Drugs 0.000 claims description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 claims description 3
- 229940005642 polystyrene sulfonic acid Drugs 0.000 claims description 3
- 229910001487 potassium perchlorate Inorganic materials 0.000 claims description 3
- 229940048098 sodium sarcosinate Drugs 0.000 claims description 3
- ZUFONQSOSYEWCN-UHFFFAOYSA-M sodium;2-(methylamino)acetate Chemical compound [Na+].CNCC([O-])=O ZUFONQSOSYEWCN-UHFFFAOYSA-M 0.000 claims description 3
- 229940117013 triethanolamine oleate Drugs 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims 1
- 230000000996 additive effect Effects 0.000 claims 1
- 125000000687 hydroquinonyl group Chemical class C1(O)=C(C=C(O)C=C1)* 0.000 claims 1
- 229920001940 conductive polymer Polymers 0.000 abstract description 21
- 230000009286 beneficial effect Effects 0.000 abstract description 11
- 238000005516 engineering process Methods 0.000 abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 abstract description 6
- 238000004806 packaging method and process Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 239000004033 plastic Substances 0.000 abstract description 3
- 238000012797 qualification Methods 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 142
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 19
- 229910002804 graphite Inorganic materials 0.000 description 19
- 239000010439 graphite Substances 0.000 description 19
- 239000002002 slurry Substances 0.000 description 10
- 238000002791 soaking Methods 0.000 description 8
- 230000032683 aging Effects 0.000 description 7
- 238000010030 laminating Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 238000007654 immersion Methods 0.000 description 3
- 150000005208 1,4-dihydroxybenzenes Chemical class 0.000 description 2
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- 229920006243 acrylic copolymer Polymers 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- ONQDVAFWWYYXHM-UHFFFAOYSA-M potassium lauryl sulfate Chemical compound [K+].CCCCCCCCCCCCOS([O-])(=O)=O ONQDVAFWWYYXHM-UHFFFAOYSA-M 0.000 description 2
- LBLYYCQCTBFVLH-UHFFFAOYSA-N 2-Methylbenzenesulfonic acid Chemical compound CC1=CC=CC=C1S(O)(=O)=O LBLYYCQCTBFVLH-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010420 art technique Methods 0.000 description 1
- 238000013473 artificial intelligence Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000012864 cross contamination Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- WHRAZOIDGKIQEA-UHFFFAOYSA-L iron(2+);4-methylbenzenesulfonate Chemical compound [Fe+2].CC1=CC=C(S([O-])(=O)=O)C=C1.CC1=CC=C(S([O-])(=O)=O)C=C1 WHRAZOIDGKIQEA-UHFFFAOYSA-L 0.000 description 1
- LWLURCPMVVCCCR-UHFFFAOYSA-N iron;4-methylbenzenesulfonic acid Chemical compound [Fe].CC1=CC=C(S(O)(=O)=O)C=C1 LWLURCPMVVCCCR-UHFFFAOYSA-N 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
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
- H01G9/0029—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
- H01G9/04—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
- H01G9/15—Solid electrolytic capacitors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Laminated Bodies (AREA)
Abstract
The application relates to the technical field of capacitors, in particular to a method for reducing equivalent series resistance of a laminated capacitor, which comprises the following steps: impregnating a foil with monomer solution at a low temperature, then impregnating the foil with oxidation solution at a low temperature, removing the foil from the oxidation solution, and blowing off the excess oxidation solution on the side surface of the foil by using a high-pressure air curtain to form a cycle; and (4) after at least one cycle, impregnating the monomer solution again and drying. The invention adopts the technology of low-temperature impregnation monomer solution and oxidation solution, which is beneficial to forming conductive polymers with smaller particle size and higher bulk density, thereby preparing the conductive polymers with higher conductivity and better heat resistance; the technology of removing the redundant oxidizing solution by using high-pressure air is favorable for the oxidizing solution to be more easily permeated and firmly attached to the deep part of a hole of an anodized aluminum foil, and is favorable for forming a conductive polymer with higher compactness, high binding force, good plastic packaging impact resistance and higher conductivity; effectively reduces ESR of the laminated capacitor, and improves capacity and leakage current qualification rate.
Description
Technical Field
The present application relates to the field of capacitor technology, and more particularly, to a method for reducing equivalent series resistance of a stacked capacitor.
Background
When the laminated capacitor is applied to new application fields such as low-power-consumption servers, ultra-thin notebook computers, artificial intelligence, Beidou navigation, big data calculation processing and the like, the laminated capacitor is required to have lower ESR (equivalent series resistance).
For example, chinese invention patent CN201510886032.0 discloses a method for manufacturing a laminated sheet type polymer solid aluminum electrolytic capacitor, comprising the following steps: (1) pretreatment, (2) pretreatment, (3) chemical polymerization, (4) aluminum foil repair, (5) electrochemical polymerization, (6) conductive graphite layer formation, (7) conductive silver layer formation, (8) lamination and (9) packaging, moisture absorption, aging and other steps, wherein the chemical polymerization: carrying out chemical polymerization on the formed aluminum foil treated in the step (2) by adopting separate alternate immersion of reducing liquid and oxidizing liquid to form a first conductive polymer layer; the method specifically comprises the following steps: soaking in reducing solution for 0.5-3min, oven drying at 50-80 deg.C for 0.5-30min, soaking in oxidizing solution for 0.5-3min, and oven drying at 50-80 deg.C for 0.5-30 min; repeating the above operation, wherein the immersion time of the oxidizing solution is 2-10 times, and the immersion time of the reducing solution is 3-11 times. Although these prior art techniques can reduce ESR, the reduction is limited, the steps are cumbersome, the cost is increased, and extremely low ESR values cannot be overcome.
Disclosure of Invention
The technical problem to be solved by the embodiments of the present application is to provide a method for reducing equivalent series resistance of a stacked capacitor.
In order to solve the technical problem, the following technical scheme is adopted in the application:
a method of reducing equivalent series resistance of a stacked capacitor, said method comprising the steps of: impregnating a foil with monomer solution at a low temperature, then impregnating the foil with oxidation solution at a low temperature, removing the foil from the oxidation solution, and blowing off the excess oxidation solution on the side surface of the foil by using a high-pressure air curtain to form a cycle; and after at least one cycle, finally, impregnating the monomer solution again and drying.
Further, the temperature of the impregnation monomer solution is 1-6 ℃, and the time is 5-95 seconds.
Further, the monomer solution comprises the following components in percentage by weight: 1.5-9.5 wt% of monomer, 85-95 wt% of solvent, 0.5-5 wt% of dopant and 0.5-3 wt% of auxiliary agent.
Further, the monomer is at least one selected from pyrrole, thiophene, aniline and derivatives.
Further, the dopant is at least one selected from the group consisting of polyvinylsulfonic acid and salts thereof, polystyrenesulfonic acid and salts thereof, aliphatic sulfonic acid and salts thereof, aromatic sulfonic acid and salts thereof, m-sulfobenzamide, 3-sulfo-1, 8-naphthalic anhydride, 4-sulfo-1, 8-naphthalic anhydride, and sodium iodide.
Further, the auxiliary agent is selected from at least one of gamma-mercaptopropyltriethoxysilane and fluorinated acrylic acid copolymer, triethanolamine oleate, sodium sarcosinate oleate and hydroquinone derivative.
Further, the temperature of the low-temperature impregnation oxidizing solution is 1-4.5 ℃, and the time is 3-65 seconds.
Further, the oxidizing solution consists of the following components in percentage by weight: 1 wt% -19 wt% of oxidant and 81 wt% -99 wt% of solvent; the oxidant is selected from one of ferric p-toluenesulfonate, ammonium persulfate, potassium perchlorate, potassium permanganate, ammoniacal silver solution, sulfurous acid and hydrogen peroxide; the solvent is at least one of water, ethanol and n-butanol.
Further, blowing off the excess oxidizing solution on the side surface of the foil by using a high-pressure air curtain after the foil is removed from the oxidizing solution specifically comprises: after the foil is moved out of the liquid level of the oxidizing solution, the foil is in a vertical suspension state, and a high-pressure air curtain blown by an air knife moves along the width direction of the foil to blow off the excessive oxidizing solution on the side surface of the foil simultaneously; wherein the pressure of the high-pressure air curtain is 0.3 MPa-1 MPa.
Further, the moving speed of the air knife is 3 cm/s-7 cm/s; and an included angle of 0-20 degrees is formed between the high-pressure air curtain and the cross section of the foil in the length and height directions.
Further, heat treatment is not performed after impregnation in each cycle of the at least one cycle.
Compared with the prior art, the embodiment of the application mainly has the following beneficial effects:
the invention adopts the low-temperature monomer solution impregnation and oxidation solution technology, which is beneficial to forming conductive polymers with smaller particle size and higher bulk density, thereby preparing the conductive polymers with higher conductivity and better heat resistance; meanwhile, the technology of removing the redundant oxidizing solution by using the high-pressure air is beneficial to the oxidizing solution to be more easily permeated and firmly attached to the deep hole of the anodized aluminum foil, and is beneficial to forming a conductive polymer which is more compact, high in binding force, good in plastic packaging impact resistance and higher in conductivity, so that the ESR of the laminated capacitor can be effectively reduced, and the capacity and the leakage current qualification rate can be improved by using the low-temperature impregnation technology and the high-pressure air removal technology.
In the prior art, drying heat treatment (drying at 50-80 ℃ for 0.5-30min) is carried out in a circulating process in chemical polymerization, and mainly aims to heat excess solution on a foil to avoid influencing cross contamination of a monomer solution and an oxidizing solution, but the inventor finds that heat treatment after impregnation at each time can lead to uneven distribution of a conductive polymer, the ESR of the prepared conductive polymer is larger, and the ESR is obviously larger during over-reflow soldering. The invention does not carry out heating and drying in the circulating process, can avoid uneven coverage of the conductive polymer, and is beneficial to reducing ESR of the laminated capacitor and improving heat resistance of the laminated capacitor.
The monomer solution and the oxidizing solution adopted by the invention have specific formulas, and are beneficial to forming conductive macromolecules with high conductivity and good binding force.
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs; the terminology used in the description of the application herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application; the terms "comprising" and "having," and any variations thereof, in the description and claims of this application are intended to cover non-exclusive inclusions. The terms first, second and the like in the description and in the claims of the present application are used for distinguishing between different objects and not for describing a particular order.
Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the application. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. It is explicitly and implicitly understood by one skilled in the art that the embodiments described herein may be combined with other embodiments.
A method of reducing equivalent series resistance of a stacked capacitor, said method comprising the steps of: impregnating a foil with monomer solution at a low temperature, then impregnating the foil with oxidation solution at a low temperature, removing the foil from the oxidation solution, and blowing off the excess oxidation solution on the side surface of the foil by using a high-pressure air curtain to form a cycle; and after at least one cycle, finally, impregnating the monomer solution again and drying.
Wherein the temperature of the impregnation monomer solution is 1-6 ℃, and the time of the impregnation monomer solution is 5-95 seconds. The temperature of the low-temperature impregnation oxidizing solution is 1-4.5 ℃, and the time of the impregnation oxidizing solution is 3-65 seconds.
After the foil is removed from the oxidizing solution, blowing off the excessive oxidizing solution on the side surface of the foil by using a high-pressure air curtain specifically comprises the following steps: after the foil is moved out of the liquid level of the oxidizing solution, the foil is in a vertical suspension state, and a high-pressure air curtain blown by an air knife moves along the width direction of the foil to blow off the excessive oxidizing solution on the side surface of the foil simultaneously; wherein the pressure of the high-pressure air curtain is 0.3 MPa-1 MPa.
Further, the moving speed of the air knife is 3 cm/s-7 cm/s; and an included angle of 0-20 degrees is formed between the high-pressure air curtain and the section of the foil in the length and height directions. Preferably, the air blowing opening of the air knife is positioned about 2 cm-3 cm above the top of the foil.
The longitudinal section of the foil is a longitudinal section parallel to the side faces of the long and high components.
The invention adopts the low-temperature monomer solution impregnation and oxidation solution technology, which is beneficial to forming conductive polymers with smaller particle size and higher bulk density, thereby preparing the conductive polymers with higher conductivity and better heat resistance; meanwhile, the technology of removing the redundant oxidizing solution by using the high-pressure air is beneficial to the oxidizing solution to be more easily permeated and firmly attached to the deep hole of the anodized aluminum foil, and is beneficial to forming a conductive polymer which is more compact, high in binding force, good in plastic packaging impact resistance and higher in conductivity, so that the ESR of the laminated capacitor can be effectively reduced, and the capacity and the leakage current qualification rate can be improved by using the low-temperature impregnation technology and the high-pressure air removal technology.
And in the process of each cycle of the at least one cycle, no heat treatment is carried out after impregnation. Therefore, the invention does not need heating and drying in the circulating process, can avoid uneven coverage of the conductive polymer, and is beneficial to reducing ESR of the laminated capacitor and improving heat resistance of the laminated capacitor.
The monomer solution is selected from a mixed solution of a monomer, a solvent, a doping agent and an auxiliary agent, and the monomer solution comprises the following components in percentage by weight: 1.5-9.5 wt% of monomer, 85-95 wt% of solvent, 0.5-5 wt% of dopant and 0.5-3 wt% of auxiliary agent. The monomer is at least one of pyrrole, thiophene, aniline and derivatives, and the solvent is at least one of water, ethanol and n-butanol. The dopant is at least one selected from the group consisting of polyvinyl sulfonic acid and salts thereof, polystyrene sulfonic acid and salts thereof, aliphatic sulfonic acid and salts thereof, aromatic sulfonic acid and salts thereof, m-sulfobenzamide, 3-sulfo-1, 8-naphthalic anhydride, 4-sulfo-1, 8-naphthalic anhydride and sodium iodide. The auxiliary agent is at least one selected from gamma-mercaptopropyl triethoxysilane and fluorinated acrylic acid copolymer, triethanolamine oleate, sodium sarcosinate oleate and hydroquinone derivatives.
The oxidizing solution is selected from a mixed solution of an oxidant and a solvent, and the oxidant solution comprises the following components in percentage by weight: 1 to 19 weight percent of oxidant and 81 to 99 weight percent of solvent. The oxidant is selected from one of ferric p-toluenesulfonate, ammonium persulfate, potassium perchlorate, potassium permanganate, ammoniacal silver solution, sulfurous acid and hydrogen peroxide. The solvent is at least one of water, ethanol and n-butanol.
The drying temperature is selected from 100 ℃ to 180 ℃, and the drying time is selected from 0.2h to 0.6 h.
The present invention will be described in detail with reference to examples, which are only preferred embodiments of the present invention and are not intended to limit the present invention.
Example one
A method of reducing equivalent series resistance of a stacked capacitor, comprising: impregnating monomer solution at low temperature, then impregnating oxidizing solution at low temperature, removing the foil from the oxidizing solution, and blowing off the excessive oxidizing solution on the side surface of the foil by using a high-pressure air curtain, wherein the steps are a cycle; and (5) after 1 cycle, finally, impregnating the monomer solution again and drying.
Wherein the monomer solution comprises the following components in percentage by weight: 9.5 wt% of monomer pyrrole, 85 wt% of solvent water, 5 wt% of doping agent polystyrene sodium sulfonate, 0.1 wt% of auxiliary agent gamma-mercaptopropyl triethoxysilane and 0.4 wt% of fluorinated acrylic copolymer.
The temperature of the impregnation monomer solution was 1 ℃ and the time for impregnation of the monomer solution was 95 seconds.
The weight percentage of each component of the oxidizing solution is as follows: 19 wt% of oxidant hydrogen peroxide and 81 wt% of solvent water.
The temperature for impregnating the oxidizing solution was 1 ℃ and the time for impregnating the oxidizing solution was 65 seconds.
After the foil is removed from the oxidizing solution, blowing off the excessive oxidizing solution on the side surface of the foil by using a high-pressure air curtain specifically comprises the following steps: after the foil is moved out of the liquid level of the oxidizing solution, the foil is in a vertical suspension state, and a high-pressure air curtain blown by an air knife moves along the width direction of the foil to blow off the excessive oxidizing solution on the side surface of the foil simultaneously; wherein the pressure of the high-pressure air curtain is 0.3MPa, and the moving speed of the air knife is 7 cm/s; and an included angle of 0 degree is formed between the high-pressure air curtain and the section of the foil in the length and height direction, and an air blowing opening of the air knife is positioned about 2cm above the top of the foil.
The drying temperature is 100 ℃, and the drying time is 0.6 h.
And (3) impregnating the conductive polymer prepared by the method with conductive graphite slurry, and drying to form a conductive graphite layer. And then, continuously soaking conductive silver paste slurry on the conductive graphite layer, drying to form a conductive silver paste layer, and then laminating, encapsulating and aging.
The above method was applied to the fabrication of 2.5V/470 μ F stacked capacitors.
Example two
A method of reducing equivalent series resistance of a stacked capacitor, comprising: impregnating monomer solution at low temperature, then impregnating oxidizing solution at low temperature, removing the foil from the oxidizing solution, and blowing off the excessive oxidizing solution on the side surface of the foil by using a high-pressure air curtain, wherein the steps are a cycle; and 6 times of circulation, finally soaking the monomer solution again and drying.
Wherein the monomer solution comprises the following components in percentage by weight: 5.5 wt% of monomer 3, 4-ethylenedioxythiophene, 90 wt% of solvent ethanol, 2.75 wt% of dopant polyvinyl sulfonic acid, 1 wt% of auxiliary agent gamma-mercaptopropyltriethoxysilane and 0.75 wt% of fluorinated acrylic copolymer.
The temperature of the impregnated monomer solution was 4 ℃ and the time for impregnating the monomer solution was 50 seconds.
The weight percentage of each component of the oxidizing solution is as follows: 10 wt% of oxidant potassium permanganate and 90 wt% of solvent water.
The temperature of the impregnation with the oxidizing solution was 2.5 ℃ and the time of impregnation with the oxidizing solution was 34 seconds.
After the foil is removed from the oxidizing solution, blowing off the excessive oxidizing solution on the side surface of the foil by using a high-pressure air curtain specifically comprises the following steps: after the foil is moved out of the liquid level of the oxidizing solution, the foil is in a vertical suspension state, and a high-pressure air curtain blown by an air knife moves along the width direction of the foil to blow off the excessive oxidizing solution on the side surface of the foil simultaneously; wherein the pressure of the high-pressure air curtain is 0.7MPa, and the moving speed of the air knife is 5 cm/s; and an included angle of 10 degrees is formed between the high-pressure air curtain and the section of the foil in the length and height direction, and an air blowing opening of the air knife is positioned above the top of the foil by about 2.5 cm.
The drying temperature is 140 ℃, and the drying time is 0.4 h.
And (3) impregnating the conductive polymer prepared by the method with conductive graphite slurry, and drying to form a conductive graphite layer. And then, continuously impregnating conductive silver paste on the conductive graphite layer, drying to form a conductive silver paste layer, and then laminating, encapsulating and aging.
The method is applied to the manufacture of the 2V/470 muF laminated capacitor.
EXAMPLE III
A method of reducing equivalent series resistance of a stacked capacitor, comprising: impregnating monomer solution at low temperature, then impregnating oxidizing solution at low temperature, removing the foil from the oxidizing solution, and blowing off the excessive oxidizing solution on the side surface of the foil by using a high-pressure air curtain, wherein the steps are a cycle; after 11 cycles, the monomer solution was impregnated again and dried.
Wherein the monomer solution comprises the following components in percentage by weight: 1.5 wt% of monomer aniline, 70 wt% of solvent water and 25 wt% of ethanol, 0.5 wt% of doping agent m-sulfobenzamide, 1 wt% of auxiliary agent gamma-mercaptopropyltriethoxysilane and 2 wt% of potassium dodecyl sulfate.
The temperature of the impregnated monomer solution was 6 ℃ and the time for impregnating the monomer solution was 5 seconds.
The weight percentage of each component of the oxidizing solution is as follows: 1 wt% of oxidant p-toluenesulfonic acid iron, 90 wt% of solvent water and 9 wt% of n-butanol.
The temperature for impregnating the oxidation solution was 4.5 ℃ and the time for impregnating the oxidation solution was 3 seconds.
After the foil is removed from the oxidizing solution, blowing off the excessive oxidizing solution on the side surface of the foil by using a high-pressure air curtain specifically comprises the following steps: after the foil is moved out of the liquid level of the oxidizing solution, the foil is in a vertical suspension state, and a high-pressure air curtain blown by an air knife moves along the width direction of the foil to blow off the excessive oxidizing solution on the side surface of the foil simultaneously; wherein the pressure of the high-pressure air curtain is 0.5MPa, and the moving speed of the air knife is 3 cm/s; and an included angle of 20 degrees is formed between the high-pressure air curtain and the section of the foil in the length and height direction, and an air blowing opening of the air knife is positioned above the top of the foil by about 3 cm.
The drying temperature is 180 ℃, and the drying time is 0.2 h.
And (3) impregnating the conductive polymer prepared by the method with conductive graphite slurry, and drying to form a conductive graphite layer. And then, continuously soaking conductive silver paste slurry on the conductive graphite layer, drying to form a conductive silver paste layer, and then laminating, encapsulating and aging.
The method is applied to the manufacture of the 2V/560 muF laminated capacitor.
Example four
A method of reducing equivalent series resistance of a stacked capacitor, comprising: impregnating monomer solution at low temperature, then impregnating oxidizing solution at low temperature, removing the foil from the oxidizing solution, and blowing off the excessive oxidizing solution on the side surface of the foil by using a high-pressure air curtain, wherein the steps are a cycle; and 3 times of circulation, finally soaking the monomer solution again and drying.
Wherein the monomer solution comprises the following components in percentage by weight: 3.5 wt% of monomer thiophene, 87 wt% of solvent water and 5.5 wt% of n-butyl alcohol, 1.25 wt% of doping agent sodium iodide, 2 wt% of auxiliary agent gamma-mercaptopropyltriethoxysilane and 0.75 wt% of hydroquinone.
The temperature of the impregnated monomer solution was 2 ℃ and the time for impregnating the monomer solution was 80 seconds.
The oxidizing solution comprises the following components in percentage by weight: 5 wt% of oxidant ammonium persulfate, 85 wt% of solvent water and 10 wt% of ethanol.
The temperature for impregnating the oxidizing solution was 3 ℃ and the time for impregnating the oxidizing solution was 48 seconds.
After the foil is removed from the oxidizing solution, blowing off the excessive oxidizing solution on the side surface of the foil by using a high-pressure air curtain specifically comprises the following steps: after the foil is moved out of the liquid level of the oxidizing solution, the foil is in a vertical suspension state, and a high-pressure air curtain blown out by an air knife moves along the width direction of the foil so as to blow off the excessive oxidizing solution on the side surface of the foil; wherein the pressure intensity of the high-pressure air curtain is 0.8MPa, and the moving speed of the air knife is 6 cm/s; and an included angle of 5 degrees is formed between the high-pressure air curtain and the section of the foil in the length and height direction, and an air blowing opening of the air knife is positioned above the top of the foil by about 2.25 cm.
The drying temperature is 120 ℃, and the drying time is 0.3 h.
And (3) impregnating the conductive polymer prepared by the method with conductive graphite slurry, and drying to form a conductive graphite layer. And then, continuously impregnating conductive silver paste on the conductive graphite layer, drying to form a conductive silver paste layer, and then laminating, encapsulating and aging.
The above method was applied to the fabrication of 2.5V/470 μ F stacked capacitors.
EXAMPLE five
A method of reducing equivalent series resistance of a stacked capacitor, comprising: impregnating monomer solution at low temperature, then impregnating oxidizing solution at low temperature, removing the foil from the oxidizing solution, and blowing off the excessive oxidizing solution on the side surface of the foil by using a high-pressure air curtain, wherein the steps are a cycle; after 9 times of circulation, the mixture is finally impregnated with the monomer solution again and dried.
Wherein the monomer solution comprises the following components in percentage by weight: 7.5 wt% of monomer 3, 4-ethylenedioxythiophene, 60 wt% of solvent water and 27.5 wt% of n-butyl alcohol, 3.75 wt% of dopant 4-sulfo-1, 8-naphthalic anhydride, 1 wt% of auxiliary agent gamma-mercaptopropyltriethoxysilane and 0.25 wt% of potassium dodecyl sulfate.
The temperature of the impregnated monomer solution was 5 ℃ and the time for impregnating the monomer solution was 30 seconds.
The weight percentage of each component of the oxidizing solution is as follows: 15 wt% of oxidizing agent sulfurous acid, 70 wt% of solvent water and 15 wt% of ethanol.
The temperature of the impregnation with the oxidizing solution was 4 ℃ and the time for impregnation with the oxidizing solution was 16 seconds.
After the foil is removed from the oxidizing solution, blowing off the excessive oxidizing solution on the side surface of the foil by using a high-pressure air curtain specifically comprises the following steps: after the foil is moved out of the liquid level of the oxidizing solution, the foil is in a vertical suspension state, and a high-pressure air curtain blown by an air knife moves along the width direction of the foil to blow off the excessive oxidizing solution on the side surface of the foil simultaneously; the pressure of the high-pressure air curtain is 1MPa, and the moving speed of the air knife is 4 cm/s; and an included angle of 15 degrees is formed between the high-pressure air curtain and the section of the foil in the length and height direction, and an air blowing opening of the air knife is positioned above the top of the foil by about 2.75 cm.
The drying temperature is 160 ℃, and the drying time is 0.5 h.
And (3) impregnating the conductive polymer prepared by the method with conductive graphite slurry, and drying to form a conductive graphite layer. And then, continuously soaking conductive silver paste slurry on the conductive graphite layer, drying to form a conductive silver paste layer, and then laminating, encapsulating and aging.
The above method was applied to the fabrication of 2.5V/470 μ F stacked capacitors.
Comparative example 1
A prior art method is used for preparing a 2.5V/470 muF laminated capacitor, which comprises the following steps:
by impregnating the substrate with a monomer solution and then with an oxidizing solution. The monomer solution comprises the following components in percentage by weight: 5.3 wt% of monomer pyrrole, 86 wt% of solvent water and 8.7 wt% of dopant toluenesulfonic acid. The temperature of the impregnated monomer solution was normal temperature, the time for impregnating the monomer solution was 25 seconds, and the impregnation was performed at 50 ℃/10 minutes after the impregnation. The oxidant solution comprises the following components in percentage by weight: 6.8 wt% of iron p-toluenesulfonate and 93.2 wt% of solvent water. The temperature of the impregnation with the oxidizing solution was normal temperature, the time for impregnation with the oxidizing solution was 20 seconds, and the impregnation was performed at 50 ℃/10 minutes after the impregnation. The steps are a cycle, and the preparation is repeated for 15 times to obtain the polypyrrole conductive polymer layer.
And (3) impregnating the conductive polymer prepared by the method with conductive graphite slurry, and drying to form a conductive graphite layer. And then, continuously soaking conductive silver paste slurry on the conductive graphite layer, drying to form a conductive silver paste layer, and then laminating, encapsulating and aging.
Comparative example No. two
This comparative example is based on example three, with the only difference that: the temperature of the impregnated monomer solution was 10 ℃.
Comparative example No. three
This comparative example is based on example three, with the only difference that: the temperature for impregnating the oxidizing solution was 5 ℃.
Comparative example No. four
This comparative example is based on example three, with the only difference that: excess oxidizing solution was not blown off using a high-pressure air curtain.
Comparative example five
This comparative example is based on example three, with the only difference that: after the circulation is finished, the monomer solution is not impregnated again.
Comparative example six
This comparative example is based on example three, with the only differences being: the pressure of the high-pressure air curtain is 2MPa, and the moving speed of the air knife is 15 cm/s.
Comparative example seven
This comparative example is based on example three, with the only difference that: not only the excess solution is removed by adopting a high-pressure air curtain after the oxidizing solution is impregnated, but also the excess solution is removed by adopting a high-pressure air curtain after the monomer solution is impregnated.
Comparative example eight
This comparative example is based on example three, with the only differences being: each cycle process comprises a heat treatment step, namely drying at 50 ℃ for 10min after the monomer solution is impregnated, and drying at 50 ℃ for 10min after the oxidizing solution is impregnated.
Comparative data of electrical properties of the above examples one to five and comparative examples one to eight are shown in the following table: (in the table, the costs of the first, second, fourth and fifth examples are based on the comparison of comparative example 1, and the costs of the third, third and eighth examples are based on the comparison of comparative example two.)
It should be understood that the above-described embodiments are only a part of the embodiments of the present application, and not all of the embodiments, and do not limit the scope of the present application. This application is capable of embodiments in many different forms and is provided for the purpose of enabling a thorough understanding of the disclosure of the application. Although the present application has been described in detail with reference to the foregoing embodiments, it will be apparent to one skilled in the art that the present application may be practiced without modification or with equivalents of some of the features described in the foregoing embodiments. All equivalent structures made by using the content of the specification of the present application are directly or indirectly applied to other related technical fields, and the same is within the protection scope of the present application.
Claims (10)
1. A method of reducing equivalent series resistance of a stacked capacitor, said method comprising the steps of: impregnating a foil with monomer solution at a low temperature, then impregnating the foil with oxidation solution at a low temperature, removing the foil from the oxidation solution, and blowing off the excess oxidation solution on the side surface of the foil by using a high-pressure air curtain to form a cycle; and after at least one cycle, finally, impregnating the monomer solution again and drying.
2. The method for reducing the equivalent series resistance of a multilayer capacitor according to claim 1, wherein the temperature of the monomer-impregnating solution is 1 to 6 ℃ for 5 to 95 seconds.
3. A method for reducing equivalent series resistance of a stacked capacitor as defined in claim 2 wherein said monomer solution is comprised of the following components in weight percent: 1.5-9.5 wt% of monomer, 85-95 wt% of solvent, 0.5-5 wt% of dopant and 0.5-3 wt% of auxiliary agent.
4. The method for reducing equivalent series resistance of a stacked capacitor as claimed in claim 3, wherein said monomer is selected from at least one of pyrrole, thiophene, aniline and derivatives; the dopant is at least one selected from the group consisting of polyvinyl sulfonic acid and salts thereof, polystyrene sulfonic acid and salts thereof, aliphatic sulfonic acid and salts thereof, aromatic sulfonic acid and salts thereof, m-sulfobenzamide, 3-sulfo-1, 8-naphthalic anhydride, 4-sulfo-1, 8-naphthalic anhydride and sodium iodide.
5. A method for reducing equivalent series resistance of a stacked capacitor as defined in claim 3 wherein said additive is selected from at least one of gamma-mercaptopropyltriethoxysilane and fluorinated acrylic acid copolymer, triethanolamine oleate, sodium sarcosinate oleate, hydroquinone derivatives.
6. The method for reducing the equivalent series resistance of a multilayer capacitor according to claim 2, wherein the temperature of the low-temperature impregnation oxidizing solution is 1 ℃ to 4.5 ℃ for 3 seconds to 65 seconds.
7. The method of reducing equivalent series resistance of a stacked capacitor as recited in claim 7, wherein said oxidizing solution is comprised of the following components in weight percent: 1 wt% -19 wt% of oxidant and 81 wt% -99 wt% of solvent; the oxidant is selected from one of ferric p-toluenesulfonate, ammonium persulfate, potassium perchlorate, potassium permanganate, ammoniacal silver solution, sulfurous acid and hydrogen peroxide; the solvent is at least one of water, ethanol and n-butanol.
8. The method of claim 1, wherein blowing off the excess oxidizing solution from the side of the foil after removing the oxidizing solution by using a high pressure air curtain comprises: after the foil is moved out of the liquid level of the oxidizing solution, the foil is in a vertical suspension state, and a high-pressure air curtain blown out by an air knife moves along the width direction of the foil so as to blow off the excessive oxidizing solution on the side surface of the foil; wherein the pressure of the high-pressure air curtain is 0.3 MPa-1 MPa.
9. The method for reducing equivalent series resistance of a stacked capacitor according to claim 1, wherein the moving speed of the air knife is 3cm/s to 7 cm/s; and an included angle of 0-20 degrees is formed between the high-pressure air curtain and the section of the foil in the length and height directions.
10. The method of claim 1, wherein the at least one cycle is not followed by a heat treatment.
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