CN114496577B - Conductive polymer mixed aluminum electrolytic capacitor and manufacturing method thereof - Google Patents

Conductive polymer mixed aluminum electrolytic capacitor and manufacturing method thereof Download PDF

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CN114496577B
CN114496577B CN202011152264.0A CN202011152264A CN114496577B CN 114496577 B CN114496577 B CN 114496577B CN 202011152264 A CN202011152264 A CN 202011152264A CN 114496577 B CN114496577 B CN 114496577B
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conductive polymer
capacitor element
capacitor
electrolyte
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CN114496577A (en
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熊军
林薏竹
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Fengbin Electronic Technology Co ltd
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Fengbin Electronic Technology Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/145—Liquid 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
    • H01G9/004—Details
    • H01G9/022—Electrolytes; Absorbents
    • H01G9/035—Liquid electrolytes, e.g. impregnating materials

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Fixed Capacitors And Capacitor Manufacturing Machines (AREA)

Abstract

The invention relates to a conductive polymer mixed aluminum electrolytic capacitor and a manufacturing method thereof, which is characterized in that: the method comprises the following steps: manufacturing a capacitor element, then placing the capacitor element in a formation liquid, applying voltage to repair the capacitor element; the purified capacitor element is washed by pure water and dried; impregnating the capacitor element after the formation and drying with a mixed conductive polymer dispersion liquid of insoluble conductive polymer particles and water-soluble self-circulation conductive polymer; drying the impregnated capacitor element; placing the impregnated and dried capacitor element in electrolyte for impregnation; the capacitor element group immersed in the electrolyte is assembled in an aluminum shell to be subjected to girdling and sealing processing; and performing aging treatment. The capacitor has the characteristics of miniaturization, high capacity, low equivalent series resistance and low impedance, and solves the problem that the capacity of the capacitor is attenuated, so that the equivalent series resistance and the capacitance change rate are increased.

Description

Conductive polymer mixed aluminum electrolytic capacitor and manufacturing method thereof
Technical Field
The invention belongs to the field of manufacturing of electrolyte aluminum electrolytic capacitors, and particularly relates to a conductive polymer mixed type aluminum electrolytic capacitor and a manufacturing method thereof.
Background
With the increase in the frequency of operation of electronic devices, there is a demand for an aluminum electrolytic capacitor in electronic parts having better impedance characteristics than before in the same high frequency range of operation. In order to meet this demand, electrolytic capacitors are widely used because they use valve metal such as tantalum or aluminum, and the valve metal is formed into a sintered body, a corrosion foil, or the like to form an extended dielectric, thereby achieving a small and large capacity. In particular, solid electrolytic capacitors, which are small in size, large in capacity, low in equivalent series resistance and low in impedance, have been widely used in recent years. Among these solid electrolytic capacitors, aluminum solid electrolytic capacitors having a sealed structure are generally used in which capacitor elements are formed by winding an electrolytic paper between an anode foil and a cathode foil made of aluminum, a solid electrolyte is formed in the capacitor, a conductive polymer layer is formed, and the capacitor elements are housed in a metal case made of aluminum or the like. The aluminum solid electrolytic capacitor using these solid electrolytes is a conductive polymer hybrid type aluminum electrolytic capacitor for a low equivalent in-line resistance high voltage which is small in size, large in capacity, and low in high frequency domain, and is difficult to manufacture. This is because the withstand voltage of the conductive polymer produced is low, and it is very difficult to raise the rated voltage of the capacitor. The solid electrolyte has the greatest disadvantage of repairing the oxide film of the aluminum anode foil. There is little recovery. This is for a non-solid aluminum electrolytic capacitor, and the failure mode of the non-solid aluminum electrolytic capacitor is the open mode of the capacitor, while the solid aluminum electrolytic capacitor is the short mode. In order to form a conductive polymer layer using a conductive polymer dispersion, a conductive polymer having a high withstand voltage can be used as a high voltage, but the capacity extraction rate of a capacitor is low due to the conductive polymer, so that the capacity extraction of the capacitor can be facilitated. The portion of which the capacity cannot be extracted is extracted by the electrolyte. Therefore, not only the equivalent series resistance becomes large, but also the reliability evaluation has a disadvantage of large capacity variation. This is considered to be because the capacitance of the capacitor drawn out with the electrolyte decays due to volatilization and evaporation of the electrolyte components at high temperature, resulting in a problem that the equivalent series resistance and the capacitance change rate become large.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a conductive polymer mixed aluminum electrolytic capacitor and a manufacturing method thereof, wherein after a mixed conductive polymer dispersion liquid of insoluble conductive polymer particles and water-soluble self-circulation conductive polymer is used in a capacitor element, the conductive polymer mixed aluminum electrolytic capacitor manufactured by a method of impregnating electrolyte has excellent capacity achievement rate, has the characteristics of miniaturization, high capacity, low equivalent series resistance and low impedance, and solves the problems that the capacity of a capacitor led out by electrolyte is attenuated due to volatilization and evaporation of electrolyte components at high temperature, and the equivalent series resistance and the capacitance change rate are increased.
The invention solves the technical problems by adopting the following technical scheme:
a conductive polymer mixed aluminum electrolytic capacitor and a manufacturing method thereof are characterized by comprising the following steps: manufacturing capacitor elements, and winding a dielectric film formed on the surface of an anode foil with pores and a cathode foil opposite to the dielectric film through electrolytic paper to form the capacitor elements; then placing the capacitor element in a formation liquid, and applying voltage to repair the capacitor element; the purified capacitor element is washed by pure water and dried; impregnating the capacitor element after the formation and drying with a mixed conductive polymer dispersion liquid of insoluble conductive polymer particles and water-soluble self-circulation conductive polymer; drying the impregnated capacitor element to form a conductive polymer layer on the surface of the dielectric film, in the electrolytic paper and on the surface of the opposite cathode foil; placing the impregnated and dried capacitor element in electrolyte for impregnation; the capacitor element group immersed in the electrolyte is assembled in an aluminum shell to be subjected to girdling and sealing processing; and performing aging treatment.
Further, the water-soluble self-circulating conductive polymer is composed of a conductive polymer having a sulfonic acid group.
Further, the chemical solution was an aqueous ammonium adipate solution, and the dielectric coating film on the cut surface of the anode foil and the electrode hammer terminal was repaired.
Furthermore, the formation drying adopts a high temperature of 125 ℃ to dry the capacitor element.
Further, the mixed conductive polymer dispersion is prepared by adding the poorly soluble conductive polymer particles and the water-soluble self-circulating conductive polymer to water.
Further, the capacitor element is immersed for 10 minutes under negative pressure under the condition of immersing the mixed conductive polymer dispersion liquid, and is heated for 60 minutes at a high temperature of 150 ℃ to dry the capacitor element, so that the capacitor element forms a conductive polymer layer.
Further, the capacitor element is placed in the electrolyte to be impregnated under the negative pressure of 50kPa under the condition of the electrolyte.
Further, the capacitor element is assembled in an aluminum shell under the environment of 25 ℃ and 35% of relative humidity.
Further, the direct current voltage of 35V is applied, and the aging treatment is performed at high temperature.
The invention has the advantages and positive effects that:
the invention provides a conductive polymer mixed type aluminum electrolytic capacitor and a manufacturing method thereof, wherein the conductive polymer mixed type aluminum electrolytic capacitor manufactured by a method of impregnating electrolyte after the mixed conductive polymer dispersion liquid of insoluble conductive polymer microparticles and water-soluble self-circulation conductive polymer is impregnated and dried in the capacitor element of the invention has excellent capacity achievement rate, equivalent series resistance and impedance characteristics in high frequency field are the same as those of the conductive polymer solid electrolytic capacitor, leakage current characteristics are the same as those of the non-solid aluminum electrolytic capacitor using electrolyte, the high reliability aluminum electrolytic capacitor which is not easy to be in a short mode can be provided, the capacity achievement rate of the conductive polymer mixed type aluminum electrolytic capacitor has excellent miniaturization, high capacity, low equivalent series resistance and low impedance characteristics, and the problems that the volatilization and evaporation of electrolyte components at high temperature lead to the capacitor with electrolyte can be attenuated, and the equivalent series resistance and the capacitance change rate of the capacitor are large are solved. Because of the dielectric repairing function, the capacitor with high reliability is adopted by vehicles, industrial 5G communication and the like, and has great popularization value and practicability.
Drawings
FIG. 1 is a schematic flow chart of a manufacturing method of the present invention.
Detailed Description
Embodiments of the present invention will be described in further detail with reference to the accompanying drawings:
as shown in fig. 1, the invention relates to a conductive polymer mixed aluminum electrolytic capacitor and a manufacturing method thereof, which is characterized by comprising the following steps: manufacturing capacitor elements, and winding a dielectric film formed on the surface of an anode foil with pores and a cathode foil opposite to the dielectric film through electrolytic paper to form the capacitor elements; then placing the capacitor element in a formation liquid, and applying voltage to repair the capacitor element; the purified capacitor element is washed by pure water and dried; impregnating the capacitor element after the formation and drying with a mixed conductive polymer dispersion liquid of insoluble conductive polymer particles and water-soluble self-circulation conductive polymer; drying the impregnated capacitor element to form a conductive polymer layer on the surface of the dielectric film, in the electrolytic paper and on the surface of the opposite cathode foil; placing the impregnated and dried capacitor element in electrolyte for impregnation; the capacitor element group immersed in the electrolyte is assembled in an aluminum shell to be subjected to girdling and sealing processing; and performing aging treatment.
A mixed conductive polymer dispersion of poorly-soluble conductive polymer particles and a water-soluble self-circulating conductive polymer is prepared by adding the poorly-soluble conductive polymer particles and the water-soluble self-circulating conductive polymer to water.
The water-soluble self-circulation conductive polymer is composed of a conductive polymer having a sulfonic acid group.
As the water-soluble self-circulating conductive polymer, a polyaniline sulfonic acid, a polypyrrolidine sulfonic acid, a polyisothianaphthene sulfonic acid, a polythiophene oxyalkane sulfonic acid can be used. As a method for producing such a mixed conductive polymer dispersion, a stable dispersion is produced by mixing conductive polymer fine particles which are hardly soluble with a polyanion and water and dispersing the mixture by a high shear force dispersing machine. The water-soluble self-circulating conductive polymer is preferably added before or after the high shear dispersing machine. The viscosity of the dispersion having a d50 of 100nm or less for the particle diameter of the hardly soluble conductive polymer particles after dispersion is preferable, but if the particle diameter is larger than this, the particle diameter is 1 μm or less.
Particles of a conductive polymer are dispersed in water, and the mixed conductive polymer dispersion is infiltrated into the surface of the dielectric film and the surface of the cathode foil in the electrolytic paper and facing each other to form a conductive polymer layer, whereby the capacitor element forms a conductive polymer layer. In the method for forming the conductive polymer layer, a pi-common double-bond polymer such as thiophene, pyrrole, aniline, etc. and a dopant, which are substituted or unsubstituted with conductive polymer microparticles that are hardly soluble in water, may be used as the polyanion polystyrene sulfonate, polyacetic acid sulfonate, polyester sulfonic acid, or polyacrylic acid alkylene sulfonic acid.
Impregnating the capacitor element with a mixed conductive polymer dispersion of poorly-soluble conductive polymer microparticles and a water-soluble self-circulating conductive polymer; the impregnated capacitor element is dried to form a conductive polymer layer on the surface of the dielectric film, in the electrolytic paper and on the surface of the cathode foil facing the electrolytic paper.
The capacitor element after the impregnation and drying is placed in an electrolyte solution to be impregnated, and as the electrolyte solution to be filled in the capacitor element, an electrolyte solution which is dissociated by ions in a normal state can be used. As the nonaqueous solvent which can be used for the electrolyte, a solvent having a boiling point of 150℃or higher is used. Examples of the solvent include γ -Ding Bingzhi, ethylene glycol, sulfolane, diethylene glycol-n-butyl ether, and the like. These may be used alone, but 2 or more may be used in combination.
The electrolyte may be at least one ammonium salt, quaternary aluminum salt, or amine salt of the above-mentioned solvent, organic acid, inorganic acid, or a complex of an organic acid and an inorganic acid.
The organic acids include: phthalic acid, isoflavone acid, terephthalic acid, maleic acid, adipic acid, benzoic acid, phenylacetic acid, heptanoic acid, malonic acid, 1, 6-dodecanoic acid, 1, 7-octabianoic acid, azelaic acid, and the like. In addition, the inorganic acid includes boric acid, phosphoric acid, phosphorous acid, hypophosphorous acid, phosphoric acid esters, carbonic acid, silicic acid, and the like. Examples of the compound of the organic acid and the inorganic acid include boron disalicylic acid, boron bisoxalic acid, and boron diglycolic acid.
Examples of the at least one salt of the organic acid, inorganic acid, or a complex compound of an organic acid and an inorganic acid include an ammonia salt, a quaternary ammonium salt, a quaternary amidine salt, and an amine salt. The 4-stage ammonium ion of the 4-stage ammonium salt includes tetraethylamine, triethylmethylamine, and tetramethylamine, and the amidinate salt includes dimethylethylimidazoline and tosylchloride.
The amine of the amine salt may be exemplified by a 1-stage amine, a 2-stage amine, and a 3-stage amine. The 1-stage amine includes ethylamine. The 2-stage amine is selected from dimethylamine, propylamine, ethylmethylamine, diethylamine, etc., and the 3-stage amine is selected from trimethylamine, triethylamine, tributylamine N.N-diisopropylethylamine.
Examples of additives for the electrolyte include polyethylene glycol, a complex compound of boric acid and polysaccharides (mannitol, sorbitol, etc.), a complex compound of boric acid and polyvalent alcohol, a nitro compound of o-nitrobenzoic acid, m-nitrobenzoic acid, p-nitrobenzoic acid, o-nitrophenols of m-nitrophenols, p-nitrophenols, etc., phosphate esters, and antioxidants.
The above-described electrolytic solution is filled in the capacitor element, and the filling amount thereof can be filled in the void inside the capacitor element. The amount of moisture in these electrolytes is preferably 1wt% or less, and more preferably 0.5wt% or less.
This is because the dissolution of the water-soluble self-circulating conductive polymer occurs slowly when the water content in the assembled capacitor element is 2wt% or more, resulting in the occurrence of characteristic degradation. As a countermeasure, it is necessary to impregnate an electrolyte solution after drying the electrolyte solution by immersing the capacitor element in the mixed conductive polymer dispersion solution, and to perform a corset and sealing process in an aluminum case, the capacitor element being assembled in the aluminum case in an environment having a temperature of 25 ℃ and a relative humidity of 35%.
Embodiment 1
A capacitor element is produced by winding a dielectric film formed on the surface of an anode body having fine holes and a cathode foil facing each other through an electrolytic paper. That is, the aluminum foil having the surface subjected to the etching treatment and the dielectric coating film formed by the anodic oxidation treatment is cut into a predetermined width as the anode foil, and the hammer terminals of the external lead electrodes are connected to the respective foils. Anode foil and cathode foil were passed through a separator having a density of 0.35g/cm ３ Aramid fiber having a thickness of 50 a ㎛ aThe non-woven fabric electrolytic paper composed of polyester fiber and cellulose fiber is wound to complete the capacitor element with the diameter of the final product of 10mm and the height of the product of 10 mm.
Then, the capacitor element is subjected to repair formation by placing the capacitor element in a formation liquid, and applying a voltage, wherein the formation liquid is an ammonium adipate aqueous solution, and the repair of the dielectric coating on the cut surface of the anode foil and the electrode hammer terminal is performed, so that the repair formation of the capacitor element is performed. The formed capacitor element was washed with pure water and dried at 125 ℃.
Next, as the conductive polymer 3wt% of PEDOT/polystyrene sulfonic acid conductive polymer fine particles and water-soluble self-circulation type conductive polymer, a mixed dispersion (remainder: water) containing 0.5wt% of polyaniline sulfonic acid was impregnated with capacitor elements under a negative pressure of 50kpa for 10 minutes, and heated at 150 ℃ for 60 minutes to dry them. Thereafter, the impregnation and drying of the mixed conductive polymer dispersion are repeated twice. The surface of the dielectric film and the surface of the cathode foil in the electrolytic paper and opposite to each other are formed with conductive polymer layers.
In the capacitor element for forming the conductive polymer layer, the capacitor element after impregnation and drying is placed in an electrolyte for impregnation, wherein 35wt% of gamma-butyrolactone and 35wt% of sulfolane mixed solvent used in the electrolyte are dissolved, 30wt% of benzoic acid amidine salt (benzoic acid) electrolyte (moisture content: 0.4 wt%) is impregnated under a negative pressure of 50kPa, and the capacitor element is assembled in an aluminum shell at a temperature of 25 ℃ and a relative humidity of 35%, and is packaged by a rubber pad for packaging made of butyl rubber, and then subjected to waistline processing and sealing processing. A direct current voltage of 35V was applied while performing an aging treatment at a high temperature.
Embodiment 2
The same capacitor was fabricated under the same conditions as in example 1 except that the moisture content in the element was adjusted to 2.0 wt%.
Comparative example 1
The same capacitor was fabricated under the same conditions as in example 1 except that the moisture content in the element was adjusted to 3.0 wt%.
Comparative example 2
In example 1, a capacitor was fabricated without an electrolyte.
Comparative example 3
The mixed dispersion of example 1 was used for a capacitor prepared from a dispersion of conductive polymer microparticles of 3wt% PEDOT/PSS/PSS.
Table 1 shows the initial characteristics (capacity: cap, equivalent series resistance: ESR, impedance: Z, leakage current: LC) of the capacitor and the characteristics after 2000 hours of no-load placement at 150 ℃. The capacitance was 120Hz, the equivalent serial resistance and impedance were 100kHz, and the current value of the 35V leakage current after 2 minutes was applied was displayed. Each of 20 averages is shown.
TABLE 1
In example 1, the capacity was decreased and the equivalent series resistance was increased after 2000 hours at 150℃as compared with example 2 and comparative example 1 having a large amount of water. It is assumed that this is caused by dissolution of the water-soluble conductive polymer. In comparative example 2, in which the electrolyte was not impregnated, had a slightly lower initial characteristic capacity and a high leakage current. The leakage current became large after 2000 hours of standing at 150 ℃, and the defect of the conductive polymer solid electrolytic capacitor was revealed. The conductive polymer hybrid aluminum electrolytic capacitor of example 1 and example 2 can maintain the initial characteristics and the high-temperature degradation characteristics at the same level as those of the conductive polymer solid electrolytic capacitor of comparative example 2. The conventional conductive polymer hybrid aluminum electrolytic capacitor of comparative example 3 has initial characteristics equivalent to those of example 1 and example 2, but has a large capacity change rate after being left at 150 ℃ for 2000 hours, and has deteriorated equivalent series resistance and impedance characteristics. It is assumed that the capacity component part extracted by volatilization and evaporation of the electrolyte has disappeared.
In order to solve these problems, a mixed conductive polymer dispersion liquid in which a poorly soluble conductive polymer fine particle and a water-soluble self-conductive polymer are added to water is used, whereby the equivalent series resistance is further reduced, and the high capacity and the small capacity change are achieved, thereby providing a highly reliable conductive polymer mixed aluminum electrolytic capacitor.
It should be emphasized that the examples described herein are illustrative rather than limiting, and therefore the invention is not limited to the examples described in the detailed description, but rather falls within the scope of the invention as defined by other embodiments derived from the technical solutions of the invention by those skilled in the art.

Claims (6)

1. A method for manufacturing a conductive polymer hybrid aluminum electrolytic capacitor is characterized by comprising the following steps: manufacturing capacitor elements, and winding a dielectric film formed on the surface of an anode foil with pores and a cathode foil opposite to the dielectric film through electrolytic paper to form the capacitor elements; then placing the capacitor element in a formation liquid, and applying voltage to repair the capacitor element; repairing the dielectric coating film on the cut surface of the anode foil and the electrode hammer terminal; the purified capacitor element is washed by pure water and dried; impregnating the capacitor element after the formation and drying with a mixed conductive polymer dispersion liquid of insoluble conductive polymer particles and water-soluble self-circulation conductive polymer; drying the impregnated capacitor element to form a conductive polymer layer on the surface of the dielectric film, in the electrolytic paper and on the surface of the cathode foil opposite to the surface of the dielectric film; placing the impregnated and dried capacitor element into electrolyte for impregnation; the capacitor element sub-group immersed in the electrolyte is assembled in an aluminum shell to be subjected to girdling and sealing processing; and performing aging treatment;
the mixed conductive polymer dispersion is prepared by mixing poorly soluble conductive polymer microparticles with a polyanion, water and a water-soluble self-circulating conductive polymer;
the water-soluble self-circulation conductive polymer is polypyrrolidine sulfonic acid, polyisothianaphthene sulfonic acid, polythiophene alkane sulfonic acid and polythiophene oxyalkane sulfonic acid;
the particle diameter d50 of the insoluble conductive polymer particles is less than 100 nm;
the amount of moisture in the electrolyte is below 1 wt%;
a nonaqueous solvent of the electrolyte having a boiling point of 150 ℃ or higher;
the solvent of the electrolyte is one or more of sulfolane and diethylene glycol-n-butyl ether.
2. The method for manufacturing a conductive polymer hybrid aluminum electrolytic capacitor according to claim 1, wherein: the formation drying adopts a high temperature of 125 ℃ to dry the capacitor element.
3. The method for manufacturing a conductive polymer hybrid aluminum electrolytic capacitor according to claim 1, wherein: the capacitor element is impregnated for 10 minutes under negative pressure under the condition of mixing conductive polymer dispersion liquid, and is heated for 60 minutes at a high temperature of 150 ℃ to dry the capacitor element, so that the capacitor element forms a conductive polymer layer.
4. The method for manufacturing a conductive polymer hybrid aluminum electrolytic capacitor according to claim 1, wherein: the capacitor element is placed in the electrolyte to be impregnated under the negative pressure of 50 kPa.
5. The method for manufacturing a conductive polymer hybrid aluminum electrolytic capacitor according to claim 1, wherein: the capacitor element sub-assembly is assembled in an aluminum shell under the environment of 25 ℃ and 35% of relative humidity.
6. The method for manufacturing a conductive polymer hybrid aluminum electrolytic capacitor according to claim 1, wherein: the direct current voltage of 35V is applied, and the aging treatment is carried out at high temperature.
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