CN112735832B - Medium-high voltage solid-state aluminum electrolytic capacitor and preparation method thereof - Google Patents
Medium-high voltage solid-state aluminum electrolytic capacitor and preparation method thereof Download PDFInfo
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- CN112735832B CN112735832B CN202011552203.3A CN202011552203A CN112735832B CN 112735832 B CN112735832 B CN 112735832B CN 202011552203 A CN202011552203 A CN 202011552203A CN 112735832 B CN112735832 B CN 112735832B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
Abstract
A middle-high voltage solid aluminum electrolytic capacitor comprises a core package consisting of an anode foil, electrolytic paper and a cathode foil, wherein the electrolytic paper is arranged between the anode foil and the cathode foil; and a conductive high polymer is formed between the anode foil and the cathode foil, and the conductive high polymer comprises PEDOT: PSS film. In the present invention, PEDOT is reacted with concentrated sulfuric acid and dimethyl sulfoxide: and (3) etching the PSS polymer conductive film to remove PEDOT: the surplus PSS on the PSS high-molecular conductive film improves the yield of PEDOT: the PSS polymer conductive film has the conductivity, so that the internal resistance of the solid-state aluminum electrolytic capacitor is reduced, and the ripple current resistance of the solid-state aluminum electrolytic capacitor is improved.
Description
Technical Field
The invention relates to a solid-state aluminum electrolytic capacitor, in particular to a medium-high voltage solid-state aluminum electrolytic capacitor and a preparation method thereof.
Background
The solid aluminum electrolytic capacitor has small internal resistance, and compared with a liquid aluminum electrolytic capacitor, the solid aluminum electrolytic capacitor has no problems of liquid leakage and the like, so that the solid aluminum electrolytic capacitor is widely used in electronic products at present. The solid-state aluminum electrolytic capacitor is characterized in that a conductive high polymer is formed between an anode foil and a cathode foil, the common conductive high polymer is PEDOT, when the PEDOT is formed on a core package, the core package is provided with residual oxidant, and the oxidant can corrode an oxide film of the anode foil to a certain extent, so that the withstand voltage value of the solid-state capacitor is low, and the leakage current is high.
To solve the above problem, the core package is impregnated with PEDOT: PSS, and PEDOT: PSS is not corrosive towards anode foils, for example, a new solid state capacitor and a method for its preparation are disclosed in patent CN 2016103029087. But the PEDOT: the PSS contains a large amount of surplus PSS (poly-4-styrenesulfonic acid), which is insulating, and the conductivity of the conductive high polymer is seriously affected by the surplus PSS, so that the internal resistance of the solid aluminum electrolytic capacitor is increased, and the ripple current resistance is reduced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a medium-high voltage solid aluminum electrolytic capacitor with improved internal resistance and ripple current resistance and a preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a middle-high voltage solid aluminum electrolytic capacitor comprises a core package consisting of anode foil, electrolytic paper and cathode foil, wherein the electrolytic paper is arranged between the anode foil and the cathode foil; and a conductive high molecular polymer is formed between the anode foil and the cathode foil, and the conductive high molecular polymer comprises PEDOT: PSS film.
In the above medium-high voltage solid-state aluminum electrolytic capacitor, preferably, the ratio of PEDOT: the PSS film has multiple layers.
In the above medium-high voltage solid-state aluminum electrolytic capacitor, preferably, the ratio of PEDOT: the number of layers of the PSS film is two or three.
A preparation method of a medium-high voltage solid aluminum electrolytic capacitor comprises the following steps,
1) adding 3-8 parts by weight of dimethyl sulfoxide to 100 parts by weight of PEDOT: PSS dispersion liquid is added and stirred evenly; PEDOT: the weight ratio of PEDOT to PSS in the PSS dispersion is 1: 2.5; in the present example, PEDOT: the PSS dispersion contains a large amount of surplus PSS.
2) Impregnating the core bag into the dispersion solution obtained in the step 1), and drying after impregnation;
3) immersing the core wrap in the step 2) in a concentrated sulfuric acid solution at normal temperature or below, standing for 30 seconds to 10 minutes after the immersion is finished, and then cleaning in an organic solvent which can coexist with or dissolve the concentrated sulfuric acid; in this example, the concentration of concentrated sulfuric acid is 95% or more.
4) Annealing the core package of step 3) at a temperature of 120-150 ℃ for 2-10 minutes;
5) immersing the core bag treated in the step 4) in a dimethyl sulfoxide solution, and standing for 2-10 minutes;
6) cleaning the core bag obtained in the step 5) in an isopropanol solution;
7) and (5) drying.
In the above method for preparing the medium-high voltage solid aluminum electrolytic capacitor, preferably, the steps 2) to 7) are repeated two to three times, so that PEDOT with two to three layers is obtained on the core package: PSS film.
In the above method for preparing a medium-high voltage solid aluminum electrolytic capacitor, preferably, the organic solvent capable of coexisting with or dissolving the concentrated sulfuric acid comprises n-amyl benzoate, n-amyl n-butyrate amyl biphenyl, n-amyl hexanoate, di-n-amyl ether DMI, DMF, DMPU or DMSO solution.
Compared with the prior art, the invention has the advantages that: in the present invention, PEDOT is reacted with concentrated sulfuric acid and dimethyl sulfoxide: and (3) etching the PSS polymer conductive film to remove PEDOT: the surplus PSS on the PSS high-molecular conductive film improves the yield of PEDOT: the PSS polymer conductive film has the conductivity, so that the internal resistance of the solid-state aluminum electrolytic capacitor is reduced, and the ripple current resistance of the solid-state aluminum electrolytic capacitor is improved.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.
It should be particularly noted that when an element is referred to as being "fixed to, connected to or communicated with" another element, it can be directly fixed to, connected to or communicated with the other element or indirectly fixed to, connected to or communicated with the other element through other intermediate connecting components.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Example 1
A middle-high voltage solid aluminum electrolytic capacitor comprises an anode foil, core packages formed by winding electrolytic paper and a cathode foil, wherein the electrolytic paper is arranged between the anode foil and the cathode foil; and a conductive high polymer is formed between the anode foil and the cathode foil, and the conductive high polymer comprises PEDOT: PSS film. In this example, the ratio of PEDOT between the anode foil and the cathode foil: the PSS film had two layers.
The embodiment also provides a preparation method of the medium-high voltage solid aluminum electrolytic capacitor, which comprises the following steps,
1) adding 3-8 parts by weight of dimethyl sulfoxide to 100 parts by weight of PEDOT: PSS dispersion liquid is added and stirred evenly; the PEDOT: the weight ratio of PEDOT to PSS in the PSS dispersion is 1: 2.5;
2) immersing the core wrap in the dispersion solution obtained in the step 1), and drying after immersing;
3) impregnating the core bag obtained in the step 2) in a concentrated sulfuric acid solution at normal temperature or below, standing for 30 seconds to 10 minutes after the impregnation is finished, and then cleaning in a DMSO solution; in this embodiment, stand 1 minute after soaking concentrated sulfuric acid, the time of soaking can not be longer, avoids concentrated sulfuric acid to the destruction of conducting polymer, also is in order to prevent concentrated sulfuric acid to enter into the core package depths simultaneously for it is difficult when wasing. Standing is to absorb the concentrated sulfuric acid by the core, and the concentrated sulfuric acid acts on PEDOT: the free PSS on the PSS film chain is removed. In this embodiment, the concentrated sulfuric acid does not affect the anode foil because the concentrated sulfuric acid passivates the aluminum foil and the aluminum oxide on the surface of the aluminum foil, but the concentrated sulfuric acid cannot be cleaned with water.
4) Annealing the core package of step 3) at a temperature of 120-150 ℃ for 5 minutes;
5) immersing the core bag treated in the step 4) in a dimethyl sulfoxide solution, and standing for 5 minutes;
6) cleaning the core packet obtained in the step 5) in an isopropanol solution;
7) drying;
8) repeating steps 2) -7) once, obtaining PEDOT on the core package containing two layers: PSS film.
In this example, PEDOT: PSS consists of hydrophobic PEDOT and hydrophilic PSS, which allows PEDOT to disperse in water. They are linked to each other by ionic interactions, PSS acting both as acid dopant and as stabilizer in aqueous dispersion. However, PSS is considered as an insulating impurity after the film forming process. In particular, free PSS, which is not complexed with PEDOT, has an amorphous region and disturbs the hopping mechanism between PEDOT grains. In this example, in step 1) PEDOT: the addition of dimethyl sulfoxide to the PSS dispersion allows phase separation between PEDOT and PSS, which, after separation, is separated as a result of the addition of PEDOT: the PSS dispersion liquid is baked at high temperature, so that a PEDOT-rich layer is formed towards the substrate, the PSS-rich layer is arranged between the PSS-rich layer and the conductive high molecular polymer in the core bag, after the PSS-rich layer is impregnated with concentrated sulfuric acid and dimethyl sulfoxide, the concentrated sulfuric acid can remove free PSS, even the PSS enriched in the middle of the conductive high molecular polymer can also remove a part of the PSS, and therefore the conductivity of the conductive high molecular polymer is improved.
In this example steps 2) -7) were repeated once, which resulted in PEDOT on the core package containing two layers: PSS film. Therefore, the conductive high molecular polymer can be obtained on the core cladding as much as possible, and the internal resistance of the solid aluminum electrolytic capacitor is further reduced.
In this example, 50 solid aluminum electrolytic capacitors were produced, which had an average ESR of 51.4m Ω; 50 solid-state aluminum electrolytic capacitors without being treated with concentrated sulfuric acid and dimethyl sulfoxide were prepared as a comparison, and the average ESR thereof was 75.5m Ω; therefore, the solid-state aluminum electrolytic capacitor treated by concentrated sulfuric acid and dimethyl sulfoxide can effectively reduce internal resistance, thereby improving the ripple current resistance.
Claims (3)
1. A preparation method of a medium-high voltage solid aluminum electrolytic capacitor is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
1) adding 3-8 parts by weight of dimethyl sulfoxide to 100 parts by weight of PEDOT: PSS dispersion liquid is added and stirred evenly;
2) immersing the core wrap in the dispersion solution obtained in the step 1), and drying after immersing;
3) immersing the core wrap in the step 2) in a concentrated sulfuric acid solution at normal temperature or below, standing for 30 seconds to 10 minutes after the immersion is finished, and then cleaning in an organic solvent which can coexist with or dissolve the concentrated sulfuric acid;
4) annealing the core package of step 3) at a temperature of 120-150 ℃ for 2-10 minutes;
5) immersing the core bag treated in the step 4) in a dimethyl sulfoxide solution, and standing for 2-10 minutes;
6) cleaning the core packet obtained in the step 5) in an isopropanol solution;
7) and (5) drying.
2. The method for preparing the medium-high voltage solid aluminum electrolytic capacitor according to claim 1, wherein the method comprises the following steps: repeating steps 2) -7) two to three times, obtaining PEDOT on the core package containing two to three layers: PSS film.
3. The method for preparing the medium-high voltage solid aluminum electrolytic capacitor according to claim 1, wherein the method comprises the following steps: the organic solvent which can coexist with or dissolve the concentrated sulfuric acid includes n-amyl benzoate, n-amyl n-butyrate amyl biphenyl, n-amyl hexanoate, di-n-amyl ether DMI, DMF, DMPU or DMSO solution.
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| CN114121492B (en) * | 2021-08-09 | 2023-09-01 | 湖南艾华集团股份有限公司 | Preparation method of solid aluminum electrolytic capacitor based on PEDOT (polymer electrolyte manufacturing) PSS (power system stabilizer) |
| CN114927348B (en) * | 2022-05-09 | 2023-09-01 | 湖南艾华集团股份有限公司 | Solid aluminum electrolytic capacitor with good stability and preparation method thereof |
| CN114813881A (en) * | 2022-05-09 | 2022-07-29 | 西安交通大学 | Biosensor based on organic electrochemical transistor and detection method |
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| CN105723472A (en) * | 2013-10-10 | 2016-06-29 | Lg化学株式会社 | Method of manufacturing surface-treated transparent conductive polymer thin film, and transparent electrode manufactured using same |
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| CN108893803A (en) * | 2018-05-30 | 2018-11-27 | 江西科技师范大学 | High-performance flexible PEDOT:The preparation method of PSS thermoelectric fiber |
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| CN111825880A (en) * | 2020-07-30 | 2020-10-27 | 河南农业大学 | High-frequency response porous PEDOT (PEDOT-PSS) film material as well as preparation method and application thereof |
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| CN105723472A (en) * | 2013-10-10 | 2016-06-29 | Lg化学株式会社 | Method of manufacturing surface-treated transparent conductive polymer thin film, and transparent electrode manufactured using same |
| CN105826076A (en) * | 2016-05-10 | 2016-08-03 | 湖南艾华集团股份有限公司 | Novel solid-state capacitor and production method of the same |
| CN108893803A (en) * | 2018-05-30 | 2018-11-27 | 江西科技师范大学 | High-performance flexible PEDOT:The preparation method of PSS thermoelectric fiber |
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