CN113345717A - Capacitor cathode material, preparation method and application thereof - Google Patents
Capacitor cathode material, preparation method and application thereof Download PDFInfo
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- CN113345717A CN113345717A CN202110562033.5A CN202110562033A CN113345717A CN 113345717 A CN113345717 A CN 113345717A CN 202110562033 A CN202110562033 A CN 202110562033A CN 113345717 A CN113345717 A CN 113345717A
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- 239000003990 capacitor Substances 0.000 title claims abstract description 66
- 239000010406 cathode material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 307
- 229920001940 conductive polymer Polymers 0.000 claims abstract description 97
- 239000011888 foil Substances 0.000 claims abstract description 54
- 229920000642 polymer Polymers 0.000 claims abstract description 39
- 239000004094 surface-active agent Substances 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 19
- 235000011187 glycerol Nutrition 0.000 claims description 116
- 239000000178 monomer Substances 0.000 claims description 46
- 239000007800 oxidant agent Substances 0.000 claims description 39
- 230000001590 oxidative effect Effects 0.000 claims description 37
- 239000006185 dispersion Substances 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 18
- -1 pentaglycerol Chemical compound 0.000 claims description 12
- JYKSTGLAIMQDRA-UHFFFAOYSA-N tetraglycerol Chemical compound OCC(O)CO.OCC(O)CO.OCC(O)CO.OCC(O)CO JYKSTGLAIMQDRA-UHFFFAOYSA-N 0.000 claims description 10
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 9
- AGNTUZCMJBTHOG-UHFFFAOYSA-N 3-[3-(2,3-dihydroxypropoxy)-2-hydroxypropoxy]propane-1,2-diol Chemical compound OCC(O)COCC(O)COCC(O)CO AGNTUZCMJBTHOG-UHFFFAOYSA-N 0.000 claims description 9
- 229940077388 benzenesulfonate Drugs 0.000 claims description 9
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 9
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 239000002019 doping agent Substances 0.000 claims description 7
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- GPLRAVKSCUXZTP-UHFFFAOYSA-N diglycerol Chemical compound OCC(O)COCC(O)CO GPLRAVKSCUXZTP-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 claims description 3
- 229930192474 thiophene Natural products 0.000 claims description 3
- WOKDXPHSIQRTJF-UHFFFAOYSA-N 3-[3-[3-[3-[3-[3-[3-[3-[3-(2,3-dihydroxypropoxy)-2-hydroxypropoxy]-2-hydroxypropoxy]-2-hydroxypropoxy]-2-hydroxypropoxy]-2-hydroxypropoxy]-2-hydroxypropoxy]-2-hydroxypropoxy]-2-hydroxypropoxy]propane-1,2-diol Chemical compound OCC(O)COCC(O)COCC(O)COCC(O)COCC(O)COCC(O)COCC(O)COCC(O)COCC(O)COCC(O)CO WOKDXPHSIQRTJF-UHFFFAOYSA-N 0.000 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 2
- 150000008052 alkyl sulfonates Chemical class 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 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 2
- 229920000128 polypyrrole Polymers 0.000 claims description 2
- 229920000123 polythiophene Polymers 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 239000010410 layer Substances 0.000 description 162
- 238000007598 dipping method Methods 0.000 description 88
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 49
- 229910052782 aluminium Inorganic materials 0.000 description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 23
- 239000008367 deionised water Substances 0.000 description 22
- 229910021641 deionized water Inorganic materials 0.000 description 22
- 238000002156 mixing Methods 0.000 description 18
- 238000006116 polymerization reaction Methods 0.000 description 17
- 238000003756 stirring Methods 0.000 description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 15
- 238000007605 air drying Methods 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 9
- RFSKGCVUDQRZSD-UHFFFAOYSA-N 3-methoxythiophene Chemical compound COC=1C=CSC=1 RFSKGCVUDQRZSD-UHFFFAOYSA-N 0.000 description 8
- 229910052708 sodium Inorganic materials 0.000 description 7
- 239000011734 sodium Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- OXHNLMTVIGZXSG-UHFFFAOYSA-N 1-Methylpyrrole Chemical compound CN1C=CC=C1 OXHNLMTVIGZXSG-UHFFFAOYSA-N 0.000 description 1
- VPUAYOJTHRDUTK-UHFFFAOYSA-N 1-ethylpyrrole Chemical compound CCN1C=CC=C1 VPUAYOJTHRDUTK-UHFFFAOYSA-N 0.000 description 1
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 description 1
- NJAURUMTVMVSGR-UHFFFAOYSA-N 3-pentoxythiophene Chemical compound CCCCCOC=1C=CSC=1 NJAURUMTVMVSGR-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000004528 spin coating Methods 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
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
- H01G9/0425—Electrodes or formation of dielectric layers thereon characterised by the material specially adapted for cathode
-
- 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
- H01G9/004—Details
- H01G9/14—Structural combinations or circuits for modifying, or compensating for, electric characteristics of electrolytic capacitors
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
- Laminated Bodies (AREA)
Abstract
The application provides a capacitor cathode material, a preparation method and application thereof, and belongs to the technical field of capacitors. The capacitor cathode material comprises a surfactant layer, a first conductive polymer layer, a glycerol layer and a second conductive polymer layer which are sequentially attached to the surface of an electrode foil; the glycerol layer material comprises one or more of glycerol and glycerol polymers. In the application, the problems of large leakage current and low breakdown voltage of the capacitor can be effectively solved, and the preparation process of the cathode material of the capacitor is simple.
Description
Technical Field
The application relates to the technical field of capacitors, in particular to a capacitor cathode material, and a preparation method and application thereof.
Background
The existing low-voltage (UR is less than or equal to 10V) conductive polymer solid chip type aluminum electrolytic capacitor product is prepared by adopting an electrolytic method or a chemical method polymerization process to form a layer of conductive polymer, and the product has large leakage current and low breakdown voltage, thus causing low qualification rate. In order to solve the problems of low-voltage products in the existing medium-voltage (UR is more than 10V and less than or equal to 35V) conductive polymer solid chip type aluminum electrolytic capacitor products, in the preparation process, after a layer of conductive polymer is formed by adopting an electrolytic method or a chemical method polymerization process, treatment liquids such as dispersion liquid and the like are generally required to be adopted to repeatedly form dozens of conductive polymer layers, so that the process is complex and the cost is high.
Disclosure of Invention
The application aims to provide a capacitor cathode material, a preparation method and application thereof, which can effectively solve the problems of large leakage current and low breakdown voltage of a capacitor and have a simple preparation process.
The embodiment of the application is realized as follows:
in a first aspect, embodiments of the present application provide a capacitor cathode material, including a surfactant layer, a first conductive polymer layer, a glycerin layer, and a second conductive polymer layer, which are sequentially attached to a surface of an electrode foil; the glycerol layer material comprises one or more of glycerol and glycerol polymers.
In a second aspect, embodiments of the present application provide a method for preparing a capacitor cathode material as provided in an embodiment of the first aspect, including: and sequentially forming a surfactant layer, a first conductive polymer layer, a glycerin layer and a second conductive polymer layer on the surface of the electrode foil.
In a third aspect, embodiments of the present application provide a use of the capacitor cathode material as provided in the embodiments of the first aspect or as prepared by the preparation method provided in the embodiments of the second aspect in a solid chip capacitor.
The capacitor cathode material, the preparation method and the application thereof have the advantages that:
the capacitor cathode material forms the glycerin layer on the surface of the first conductive polymer layer, and then forms the second conductive polymer layer on the surface of the glycerin layer, and the glycerin layer and the second conductive polymer layer can exert the effect equivalent to that of a composite conductive polymer layer formed by tens of layers of dispersion liquid, so that the preparation process of the material is simple and the cost is saved while the problems of large leakage current and low breakdown voltage of a capacitor are effectively improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
It should be noted that "and/or" in the present application, such as "feature 1 and/or feature 2" refers to "feature 1" alone, "feature 2" alone, and "feature 1" plus "feature 2" alone.
In addition, in the description of the present application, the meaning of "a plurality" of "one or more" means two or more unless otherwise specified; the range of "numerical value a to numerical value b" includes both values "a" and "b", and "unit of measure" in "numerical value a to numerical value b + unit of measure" represents both "unit of measure" of "numerical value a" and "numerical value b".
The capacitor cathode material, the preparation method and the application thereof according to the embodiments of the present application are specifically described below.
In a first aspect, embodiments of the present application provide a capacitor cathode material, including a surfactant layer, a first conductive polymer layer, a glycerin layer, and a second conductive polymer layer, which are sequentially attached to a surface of an electrode foil; the glycerol layer material comprises one or more of glycerol and glycerol polymers.
The capacitor cathode material is exemplarily suitable for a solid chip capacitor with a load voltage UR of 2-35V. The electrode foil is illustratively an aluminum foil, i.e., the capacitor cathode material is used for a solid-chip aluminum electrolytic capacitor.
The inventors have found that, by forming a single layer of the glycerin layer after forming a surfactant layer and a conductive polymer layer in this order on the surface of the electrode foil, and then forming a single layer of the glycerin layer, it is only necessary to form a single conductive polymer layer, and the glycerin layer and the second conductive polymer layer formed on the surface of the glycerin layer can exhibit effects equivalent to those of composite conductive polymer layers formed from tens of layers of the dispersion.
The capacitor cathode material disclosed by the application can effectively improve the problems of large leakage current and low breakdown voltage of a capacitor by exerting the effect equivalent to that of a composite conductive polymer layer formed by tens of layers of dispersion liquid through the glycerin layer and the second conductive polymer layer. Meanwhile, only one layer of the glycerin layer and one layer of the second conductive polymer layer need to be sequentially arranged on the surface of the first conductive polymer layer, so that the capacitor cathode material is simple in structure, and the operation of repeatedly forming dozens of conductive polymer layers on the surface of the first conductive polymer layer by adopting treatment liquids such as dispersion liquid and the like can be omitted in the preparation process, so that the preparation process is simple.
The inventors have also found that a glycerin layer mainly composed of glycerin and a glycerin polymer can well exert the breakdown resistance of a capacitor cathode material, and particularly that a glycerin layer mainly composed of a glycerin polymer can well exert the breakdown resistance of a capacitor cathode material while having good matching with a conductive polymer layer, so that the glycerin layer and the second conductive polymer layer can well exert effects of improving problems of large leakage current and low breakdown voltage of a capacitor.
In some alternative embodiments, the glycerol layer material is predominantly one or more of glycerol and glycerol polymers, for example the total content of glycerol and glycerol polymers in the glycerol layer material is above 60 wt%.
As one example, the material of the glycerin layer is one or more of glycerin and glycerin polymer.
Further, the material of the glycerin layer is mainly glycerin polymer, for example, the content of glycerin polymer in the material of the glycerin layer is more than 50 wt%.
As an example, the material of the glycerin layer is glycerin polymer.
In embodiments where a glycerol polymer is used to form the glycerol layer, it is contemplated that different degrees of polymerization may have an effect on the performance of the glycerol polymer. Further research shows that the glycerol polymer with a specific polymerization degree can better cooperate with the first conductive polymer layer and the second conductive polymer layer to play a role.
In some alternative embodiments, the glycerol polymer comprises one or more of diglycerol, triglycerol, tetraglycerol, pentaglycerol, and decaglycerol. Further, the glycerol polymer is mainly one or more of triglycerol, tetraglycerol and pentaglycerol. As an example, the total content of triglycerol, tetraglycerol and pentaglycerol in the glycerol polymer is above 50 wt%; for example, the glycerin polymer includes, in mass percent: 20-60% of triglycerol, 20-60% of tetraglycerol and 20-60% of pentaglycerol. Through selecting a specific glycerol polymer, the glycerol layer is better matched with the first conductive polymer layer and the second conductive polymer layer to play a role in improving the problems of large leakage current and low breakdown voltage of the capacitor.
In the research process, the glycerol layer can not exert the puncture resistance better when the thickness of the glycerol layer is smaller; when the thickness of the glycerin layer is large, the glycerin layer is not easy to dry, and the subsequent process for forming the second conductive polymer layer is easily affected. Therefore, the glycerin layer needs to be controlled to have a suitable thickness, so that the glycerin layer and the second conductive polymer layer can be conveniently formed while the use performance of the glycerin layer and the second conductive polymer layer can be well considered.
Illustratively, the glycerol layer has a thickness of 1 to 15 μm, such as but not limited to any one or a range between any two of 1 μm, 2 μm, 3 μm, 5 μm, 7 μm and 10 μm, such as 1 to 7 μm or 3 to 15 μm, further such as 2 to 5 μm.
It is to be understood that, in the embodiments of the present application, the materials of the surfactant layer, the first conductive polymer layer, and the second conductive polymer layer are not limited, and may be selected according to the kinds well known in the art.
As for the surfactant layer, as an example, the material of the surfactant layer is a silane coupling agent. In other embodiments, the material of the surfactant layer may also be a titanate coupling agent, or a combination of a silane coupling agent and a titanate coupling agent.
As for the first conductive polymer layer and the second conductive polymer layer, each of the conductive polymer layers is not limited to being produced by an electrolytic method or being produced by a chemical polymerization method.
In some alternative embodiments, the first conductive polymer layer and the second conductive polymer layer are formed from polymerization of a polymer monomer or from a dispersion, respectively, in both.
Optionally, the polymer monomer is one or more of pyrrole and its derivatives and thiophene and its derivatives, i.e., the conductive polymer contained in the conductive polymer layer is one or more of polypyrrole and its derivatives and polythiophene and its derivatives.
As an example, the polymer monomer is one or more of pyrrole, N-methylpyrrole, N-ethylpyrrole, 3-octanoyl pyrrole thiophene, 3, 4-ethylenedioxythiophene, 3-methoxythiophene and 3-pentyloxythiophene.
Optionally, the dispersion comprises one or more of LV, LVN, LVNs, KV2 and KV 2N. As an example, the dispersion liquid forming the first conductive polymer layer is one or more of LV, LVN and LVNs, and the dispersion liquid forming the second conductive polymer layer is one or more of LV, LVN, LVNs, KV2, KV 2N. In the present application, each dispersion is a dispersion produced by Heley or a dispersion having the same composition as that of the dispersion.
It is understood that in embodiments of the present application, the materials of the first conductive polymer layer and the second conductive polymer layer may be the same or different.
As an example, the first conductive polymer layer is formed by polymerization of a polymer monomer; the first conductive polymer layer is formed by polymerization of a polymer monomer or formed from a dispersion liquid.
In a second aspect, embodiments of the present application provide a method for preparing a capacitor cathode material as provided in an embodiment of the first aspect, including: and sequentially forming a surfactant layer, a first conductive polymer layer, a glycerin layer and a second conductive polymer layer on the surface of the electrode foil.
It is to be understood that, in the embodiments of the present application, the structure of each of the surfactant layer, the first conductive polymer layer, the glycerin layer, and the second conductive polymer layer is not limited, and may be formed by, for example, dipping or spin coating.
In view of the simple operation of the impregnation method and the easy availability of a uniform layer structure, the surfactant layer, the first conductive polymer layer, the glycerin layer, and the second conductive polymer layer of the present application may be formed by impregnating them in respective solutions.
In the preparation method of the present application, the raw materials of each structural layer may be selected according to the materials of each structural layer in the capacitor cathode material, which are not explicitly described in the following embodiments, and all of the raw materials may refer to the example of the first aspect, and will not be described again.
With respect to the formation of the glycerol layer, in some exemplary embodiments, a glycerol layer is formed using a glycerol solution, the solute of the glycerol solution being one or more of glycerol and a glycerol polymer, such that the material of the resulting glycerol layer is one or more of glycerol and a glycerol polymer.
Considering that the concentration of the glycerol solution can generate great influence on the thickness of the glycerol layer in the formation process of the glycerol layer, particularly the formation process of the glycerol layer adopting a dipping mode, the glycerol solution is controlled to have certain solute concentration, and the glycerol layer with proper thickness can be ensured to be obtained.
Optionally, the weight percentage of the solute in the glycerol solution is 10-80 wt%, and the weight percentage of the solvent in the glycerol solution is 20-90 wt%; further optionally, the weight percentage of the solute in the glycerol solution is 30-60 wt%, and the weight percentage of the solvent in the glycerol solution is 40-70 wt%.
As an example, the weight percent of the solute of the glycerol solution is, for example and without limitation, a point value of any one of 30 wt%, 35 wt%, 40 wt%, 45 wt%, 50 wt%, 55 wt%, and 60 wt%, or a range value between any two.
With respect to the formation of the surfactant layer, in some exemplary embodiments, the surfactant layer is formed using a surfactant solution. In the surfactant solution, the solute is surfactant, and the solvent is ethanol and/or water.
With respect to the formation of the conductive polymer layer, in a first class of exemplary embodiments, the conductive polymer layer is formed using polymerization of a polymer monomer.
Illustratively, the method of forming the conductive polymer layer includes: and treating the surface to be treated by sequentially adopting a monomer solution and an oxidant solution. The solute of the monomer solution is a polymer monomer, and the polymer monomer is one or more of pyrrole and derivatives thereof, and thiophene and derivatives thereof. The oxidant solution comprises an oxidant, a doping agent and an oxidant solvent, wherein the oxidant is one or more of ferric chloride, ferric p-toluenesulfonate, ammonium persulfate, sodium persulfate and potassium permanganate. The doping agent is one or more of alkyl sulfonate, alkyl naphthalene sulfonate and alkyl benzene sulfonate.
As an example, in forming the first conductive polymer layer, the operation of treating the surface to be treated with the monomer solution and the oxidant solution in sequence is repeated for a plurality of times, optionally 3 to 28 times, further optionally 5 to 15 times, for example 8 times; when the second conductive polymer layer is formed, the operation of treating the surface to be treated with the monomer solution and the oxidant solution in this order is performed only once.
It should be noted that the surface to be treated refers to a surface to which the conductive polymer layer is formed. For example, when the first conductive polymer layer is formed, the surface to be treated refers to the surface of the surfactant layer; when the second conductive polymer layer is formed, the surface to be treated refers to the surface of the glycerin layer.
Optionally, the solute of the monomer solution is present in an amount of 5 to 40 wt%, such as but not limited to 5 wt%, 10 wt%, 15 wt%, 20 wt%, 25 wt%, 30 wt%, 35 wt%, and 40 wt%, or a range between any two.
Optionally, the weight percentage of the oxidizing agent in the oxidizing agent solution is 10 to 50 wt%, such as but not limited to a point value of any one of 10 wt%, 20 wt%, 30 wt%, 40 wt% and 50 wt%, or a range value therebetween. The weight percentage of the dopant is 0.5 to 5 wt%, such as but not limited to a point value of any one of 0.5 wt%, 1 wt%, 1.5 wt%, 2 wt%, 2.5 wt%, 3 wt%, 3.5 wt%, 4 wt%, 4.5 wt%, and 5 wt%, or a range value between any two. The oxidant solvent is 45 to 89.5 wt%, illustratively the balance of the oxidant solution after removal of the oxidant solution and the dopant.
With respect to the formation of the conductive polymer layer, in a second exemplary embodiment, the conductive polymer layer is formed using a dispersion. Illustratively, the dispersion comprises one or more of, for example any of LV, LVN, LVNs, KV2, KV 2N; in the preparation process, the dispersion liquid is adopted to dip the surface to be treated, and then drying treatment is carried out to remove the solvent in the dispersion liquid.
As an example, the formation of the first conductive polymer layer refers to the first type of exemplary embodiment described above, and the formation of the second conductive polymer layer refers to the first type of exemplary embodiment or the second type of exemplary embodiment described above.
In a third aspect, embodiments of the present application provide a use of the capacitor cathode material as provided in the embodiments of the first aspect or as prepared by the preparation method provided in the embodiments of the second aspect in a solid sheet type aluminum capacitor.
As an example, the solid chip capacitor is a solid chip aluminum electrolytic capacitor, and the load voltage UR is 2-35V.
The features and properties of the present application are described in further detail below with reference to examples.
In each of examples and comparative examples, the electrode foils used were aluminum foils. The aluminum foil is Y100LN03-67.0VF in specific volume of 19.0 muF/cm2。
Example 1
A method for preparing a capacitor cathode material, comprising:
s1, forming a surfactant layer
Mixing 1000g of deionized water and 500g of absolute ethyl alcohol uniformly, adding 63g of silane coupling agent, magnetically stirring for 10min, pouring into a dipping tank, putting an aluminum foil to be pretreated, dipping for 5min, air-drying for 15min, and then putting into an oven to be dried for 60min at 120 ℃.
S2, forming a first conductive polymer layer
(1) Mixing 2500g of absolute ethyl alcohol and 80g of 3-methoxythiophene uniformly, then stirring for 10min by magnetic force to prepare a monomer solution, then pouring the monomer solution into a dipping tank, putting the pretreated aluminum foil into the dipping tank, dipping for 3min, and then putting the monomer solution into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
(2) 2500g of deionized water, 1000g of sodium persulfate and 5g of sodium alkyl benzene sulfonate are uniformly mixed, then stirred for 60min to prepare an oxidant solution, then the oxidant solution is poured into a dipping tank, an aluminum foil dipped with a monomer solution is placed into the dipping tank, the dipping tank is dipped for 3min, and then the dipping tank is placed into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
(3) And (3) putting the aluminum foil soaked with the oxidant solution into deionized water for cleaning for 4min, and then putting the aluminum foil into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
Repeating the steps (1), (2) and (3)8 times.
S3, forming a glycerin layer
And (2) uniformly mixing 1000g of deionized water and a mixture of 300g of diglycerol and 700g of triglycerol, stirring for 60min, pouring into a dipping tank, putting the aluminum foil subjected to polymerization into the dipping tank, dipping for 10min, and then putting into a 120 ℃ oven to dry for 60 min.
S4, forming a second conductive polymer layer
Pouring the dispersion KV2N into a dipping tank, adding the aluminum foil, dipping for 4min, air-drying for 40min, and then putting into an oven to dry for 30min at 145 ℃.
Example 2
A method for preparing a capacitor cathode material, comprising:
s1, forming a surfactant layer
Mixing 1000g of deionized water and 500g of absolute ethyl alcohol uniformly, adding 63g of silane coupling agent, magnetically stirring for 10min, pouring into a dipping tank, putting an aluminum foil to be pretreated, dipping for 5min, air-drying for 15min, and then putting into an oven to be dried for 60min at 120 ℃.
S2, forming a first conductive polymer layer
(1) Mixing 2500g of absolute ethyl alcohol and 80g of 3-methoxythiophene uniformly, then stirring for 10min by magnetic force to prepare a monomer solution, then pouring the monomer solution into a dipping tank, putting the pretreated aluminum foil into the dipping tank, dipping for 3min, and then putting the monomer solution into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
(2) 2500g of deionized water, 1000g of sodium persulfate and 5g of sodium alkyl benzene sulfonate are uniformly mixed, then stirred for 60min to prepare an oxidant solution, then the oxidant solution is poured into a dipping tank, an aluminum foil dipped with a monomer solution is placed into the dipping tank, the dipping tank is dipped for 3min, and then the dipping tank is placed into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
(3) And (3) putting the aluminum foil soaked with the oxidant solution into deionized water for cleaning for 4min, and then putting the aluminum foil into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
Repeating the steps (1), (2) and (3)8 times.
S3, forming a glycerin layer
And (3) uniformly mixing 1500g of deionized water and a mixture of 150g of diglycerol and 450g of pentaglycerol, stirring for 60min, pouring into a dipping tank, putting the aluminum foil subjected to polymerization into the dipping tank, dipping for 10min, and then putting into a 120 ℃ oven to dry for 60 min.
S4, forming a second conductive polymer layer
Pouring the LVN dispersion liquid into a dipping tank, adding the aluminum foil subjected to chemical polymerization, dipping for 7min, air-drying for 15min, and then putting into an oven to dry for 30min at 120 ℃.
Example 3
A method for preparing a capacitor cathode material, comprising:
s1, forming a surfactant layer
Mixing 1000g of deionized water and 500g of absolute ethyl alcohol uniformly, adding 63g of silane coupling agent, magnetically stirring for 10min, pouring into a dipping tank, putting an aluminum foil to be pretreated, dipping for 5min, air-drying for 15min, and then putting into an oven to be dried for 60min at 120 ℃.
S2, forming a first conductive polymer layer
(1) Mixing 2500g of absolute ethyl alcohol and 80g of 3-methoxythiophene uniformly, then stirring for 10min by magnetic force to prepare a monomer solution, then pouring the monomer solution into a dipping tank, putting the pretreated aluminum foil into the dipping tank, dipping for 3min, and then putting the monomer solution into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
(2) 2500g of deionized water, 1000g of sodium persulfate and 5g of sodium alkyl benzene sulfonate are uniformly mixed, then stirred for 60min to prepare an oxidant solution, then the oxidant solution is poured into a dipping tank, an aluminum foil dipped with a monomer solution is placed into the dipping tank, the dipping tank is dipped for 3min, and then the dipping tank is placed into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
(3) And (3) putting the aluminum foil soaked with the oxidant solution into deionized water for cleaning for 4min, and then putting the aluminum foil into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
Repeating the steps (1), (2) and (3) for 8 times by taking the steps as a cycle period.
S3, forming a glycerin layer
And (2) uniformly mixing 700g of deionized water and a mixture of 300g of triglycerin, 300g of tetraglycerol and 300g of pentaglycerol, stirring for 60min, pouring into a dipping tank, putting the aluminum foil subjected to polymerization into the dipping tank, dipping for 10min, and then putting into a 120 ℃ oven for drying for 60 min.
S4, forming a second conductive polymer layer
(1) Mixing 2500g of absolute ethyl alcohol and 80g of 3-methoxythiophene uniformly, then stirring for 10min by magnetic force to prepare a monomer solution, then pouring the monomer solution into a dipping tank, putting the pretreated aluminum foil into the dipping tank, dipping for 3min, and then putting the monomer solution into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
(2) 2500g of deionized water, 1000g of sodium persulfate and 5g of sodium alkyl benzene sulfonate are uniformly mixed, then stirred for 60min to prepare an oxidant solution, then the oxidant solution is poured into a dipping tank, an aluminum foil dipped with a monomer solution is placed into the dipping tank, the dipping tank is dipped for 3min, and then the dipping tank is placed into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
Example 4
A method for preparing a capacitor cathode material, comprising:
s1, forming a surfactant layer
Mixing 1000g of deionized water and 500g of absolute ethyl alcohol uniformly, adding 63g of silane coupling agent, magnetically stirring for 10min, pouring into a dipping tank, putting an aluminum foil to be pretreated, dipping for 5min, air-drying for 15min, and then putting into an oven to be dried for 60min at 120 ℃.
S2, forming a first conductive polymer layer
(1) Mixing 2500g of absolute ethyl alcohol and 80g of 3-methoxythiophene uniformly, then stirring for 10min by magnetic force to prepare a monomer solution, then pouring the monomer solution into a dipping tank, putting the pretreated aluminum foil into the dipping tank, dipping for 3min, and then putting the monomer solution into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
(2) 2500g of deionized water, 1000g of sodium persulfate and 5g of sodium alkyl benzene sulfonate are uniformly mixed, then stirred for 60min to prepare an oxidant solution, then the oxidant solution is poured into a dipping tank, an aluminum foil dipped with a monomer solution is placed into the dipping tank, the dipping tank is dipped for 3min, and then the dipping tank is placed into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
(3) And (3) putting the aluminum foil soaked with the oxidant solution into deionized water for cleaning for 4min, and then putting the aluminum foil into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
Repeating the steps (1), (2) and (3)8 times.
S3, forming a glycerin layer
And (2) uniformly mixing a mixture of 1000g of deionized water and 1500g of glycerol, stirring for 60min, pouring into a dipping tank, putting the aluminum foil subjected to polymerization into the dipping tank, dipping for 10min, and then putting into a 120 ℃ oven to dry for 60 min.
S4, forming a second conductive polymer layer
Pouring the dispersion liquid LVNS into a dipping tank, adding the aluminum foil, dipping for 4min, air-drying for 40min, and then putting into an oven to dry for 30min at 145 ℃.
Example 5
A method for preparing a capacitor cathode material, comprising:
s1, forming a surfactant layer
Mixing 1000g of deionized water and 500g of absolute ethyl alcohol uniformly, adding 63g of silane coupling agent, magnetically stirring for 10min, pouring into a dipping tank, putting an aluminum foil to be pretreated, dipping for 5min, air-drying for 15min, and then putting into an oven to be dried for 60min at 120 ℃.
S2, forming a first conductive polymer layer
(1) Mixing 2500g of absolute ethyl alcohol and 80g of 3-methoxythiophene uniformly, then stirring for 10min by magnetic force to prepare a monomer solution, then pouring the monomer solution into a dipping tank, putting the pretreated aluminum foil into the dipping tank, dipping for 3min, and then putting the monomer solution into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
(2) 2500g of deionized water, 1000g of sodium persulfate and 5g of sodium alkyl benzene sulfonate are uniformly mixed, then stirred for 60min to prepare an oxidant solution, then the oxidant solution is poured into a dipping tank, an aluminum foil dipped with a monomer solution is placed into the dipping tank, the dipping tank is dipped for 3min, and then the dipping tank is placed into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
(3) And (3) putting the aluminum foil soaked with the oxidant solution into deionized water for cleaning for 4min, and then putting the aluminum foil into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
Repeating the steps (1), (2) and (3) for 8 times by taking the steps as a cycle period.
S3, forming a glycerin layer
And (3) uniformly mixing 700g of deionized water and a mixture of 600g of triglycerin and 150g of tetraglycerol and 150g of pentaglycerol, stirring for 60min, pouring into a dipping tank, putting the aluminum foil subjected to polymerization into the dipping tank, dipping for 10min, and then putting into a 120 ℃ oven for drying for 60 min.
S4, forming a second conductive polymer layer
(1) Mixing 2500g of absolute ethyl alcohol and 80g of 3-methoxythiophene uniformly, then stirring for 10min by magnetic force to prepare a monomer solution, then pouring the monomer solution into a dipping tank, putting the pretreated aluminum foil into the dipping tank, dipping for 3min, and then putting the monomer solution into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
(2) 2500g of deionized water, 1000g of sodium persulfate and 5g of sodium alkyl benzene sulfonate are uniformly mixed, then stirred for 60min to prepare an oxidant solution, then the oxidant solution is poured into a dipping tank, an aluminum foil dipped with a monomer solution is placed into the dipping tank, the dipping tank is dipped for 3min, and then the dipping tank is placed into a constant temperature and humidity box with the temperature of 30 ℃ and the humidity of 60% RH for 10 min.
Comparative example 1
A method for preparing a capacitor cathode material, which is different from example 1 in that: the S3 step and the S4 step are replaced with the following S3' step.
S3' forming a conductive polymer composite layer from a plurality of dispersions
(1) Pouring the dispersion liquid LVN into a dipping tank, adding the aluminum foil subjected to chemical polymerization, dipping for 7min, air-drying for 15min, and then putting into an oven to dry for 30min at 120 ℃.
Repeating the step (1)7 times.
(2) Pouring the dispersion KV2N into a dipping tank, adding the aluminum foil, dipping for 10min, air-drying for 40min, and then putting into an oven to dry for 30min at 145 ℃.
(3) Pouring the dispersion liquid W8N into a dipping tank, adding the aluminum foil, dipping for 10min, air-drying for 20min, and then putting into an oven to dry for 40min at 120 ℃.
Repeating the steps (2) and (3) for 6 times by taking the steps as a cycle period.
Test examples
The capacitor cathode materials provided in each example and comparative example were formed into capacitors; then, 5 capacitors are selected from each group, the number of the capacitors is 1-5 in sequence, and the electrical performance of each capacitor is tested.
The preparation method of the capacitor comprises the following steps:
the method comprises the following steps of aluminum foil cutting, arraying, formation, gluing, polymerization, graphite, silver paste, lamination, packaging, aging and the like.
The method for testing the electrical property of the capacitor comprises the following steps:
capacity test conditions: normal temperature, frequency 100Hz, DC bias should be 2V;
loss tangent test conditions: normal temperature, frequency 100Hz, DC bias should be 2V;
equivalent Series Resistance (ESR) test conditions: normal temperature, frequency 100KHz, direct current bias voltage should be 2V;
and (3) leakage current test conditions: nominal voltage, charge 30 seconds reading.
The results of the electrical performance tests of the capacitors are shown in table 1.
TABLE 1 Electrical Performance test results for capacitors
In examples 1 to 5 of the present application, after a glycerin layer was formed on the surface of the first conductive polymer layer, a second conductive polymer layer was formed only on the surface of the glycerin layer by a single treatment; in comparative example 1, a conductive polymer composite layer was formed on the surface of the first conductive polymer layer by repeating ten times the treatment using the plurality of dispersions. Compared with the comparative example 1, the preparation method of the capacitor cathode material is simpler, and the cost can be saved in the embodiments 1-5.
As can be seen from table 1, in examples 1 to 5 of the present application, by forming a glycerin layer on the surface of the first conductive polymer layer, only one second conductive polymer layer needs to be formed on the surface of the glycerin layer by one treatment, and the obtained capacitor cathode material shows comparable electrical properties to the capacitor cathode material formed by the complicated process in comparative example 1 when applied to a capacitor under the same conditions.
According to the comparison between the embodiments 1 to 5, the glycerol polymer in the embodiment 3 is prepared by mixing the triglycerol, the tetraglycerol and the pentaglycerol, and the content of the triglycerol, the tetraglycerol and the pentaglycerol in the glycerol polymer is within the range of 20 to 60 percent, so that the breakdown voltage of the product is obviously higher compared with the embodiment composed of other glycerol layers.
The embodiments described above are some, but not all embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Claims (10)
1. A capacitor cathode material is characterized by comprising a surfactant layer, a first conductive polymer layer, a glycerol layer and a second conductive polymer layer which are sequentially attached to the surface of an electrode foil;
the material of the glycerol layer comprises one or more of glycerol and glycerol polymers.
2. The capacitor cathode material according to claim 1, wherein the material of the glycerol layer is one or more of glycerol and glycerol polymer;
optionally, the material of the glycerol layer is the glycerol polymer.
3. The capacitor cathode material of claim 1, wherein the glycerol polymer comprises one or more of diglycerol, triglycerol, tetraglycerol, pentaglycerol, and decaglycerol;
optionally, the glycerol polymer comprises, in mass percent: 20-60% of the triglycerol, 20-60% of the tetraglycerol and 20-60% of the pentaglycerol.
4. The capacitor cathode material according to any one of claims 1 to 3, wherein the glycerol layer has a thickness of 1 to 7 μm, optionally 2 to 5 μm.
5. The capacitor cathode material according to any one of claims 1 to 3, wherein the surfactant layer is made of one or both of a silane coupling agent and a titanate coupling agent;
and/or, in both the first conductive polymer layer and the second conductive polymer layer, the conductive polymer contained is one or more of polypyrrole and derivatives thereof, and polythiophene and derivatives thereof, or is formed from a dispersion liquid; the dispersion comprises one or more of LV, LVN, LVNS, KV2 and KV 2N;
optionally, the dispersion forming the first conductive polymer layer is one or more of LV, LVN and LVNs, and the dispersion forming the second conductive polymer layer is one or more of LV, LVN, LVNs, KV2, KV 2N.
6. A method for preparing the capacitor cathode material according to any one of claims 1 to 5, comprising: the surfactant layer, the first conductive polymer layer, the glycerin layer, and the second conductive polymer layer are formed on the surface of the electrode foil in this order.
7. The method according to claim 6, wherein the glycerin layer is formed by using a glycerin solution, the glycerin solution having a solute of one or more of the glycerin and the glycerin polymer, the glycerin solution having a solute weight percentage of 10 to 80 wt%;
optionally, the glycerol solution has a solute weight percentage of 30-60 wt%.
8. The production method according to claim 6 or 7, characterized in that the method of forming the second conductive polymer layer comprises: sequentially adopting a monomer solution and an oxidant solution to treat the surface of the glycerol layer;
the solute of the monomer solution is a polymer monomer, and the polymer monomer is one or more of pyrrole and derivatives thereof and thiophene and derivatives thereof;
the oxidant solution comprises an oxidant, a doping agent and an oxidant solvent, wherein the oxidant is one or more of ferric chloride, ferric p-toluenesulfonate, ammonium persulfate, sodium persulfate and potassium permanganate; the dopant is one or more of alkyl sulfonate, alkyl naphthalene sulfonate and alkyl benzene sulfonate;
optionally, the weight percentage of the solute of the monomer solution is 5-40 wt%;
optionally, in the oxidant solution, the weight percentage of the oxidant is 10 to 50 wt%, the weight percentage of the dopant is 0.5 to 5 wt%, and the weight percentage of the oxidant solvent is 45 to 89.5 wt%.
9. The production method according to claim 6 or 7, characterized in that the method of forming the second conductive polymer layer comprises: and treating the surface of the glycerol layer by using a dispersion liquid, wherein the dispersion liquid comprises one or more of LV, LVN, LVNS, KV2 and KV 2N.
10. Use of a capacitor cathode material as provided in any one of claims 1 to 5 or prepared by the preparation method of any one of claims 6 to 9 in a solid chip capacitor.
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