CN110544587A - Low-cost solid-state aluminum electrolytic capacitor and preparation method thereof - Google Patents
Low-cost solid-state aluminum electrolytic capacitor and preparation method thereof Download PDFInfo
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- 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
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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
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- H01G9/151—Solid electrolytic capacitors with wound foil electrodes
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Abstract
The invention discloses a low-cost solid aluminum electrolytic capacitor and a preparation method thereof, belonging to the technical field of capacitors. The preparation method of the solid-state aluminum electrolytic capacitor comprises the following steps: firstly, carrying out chemical conversion repair treatment on the core cladding; then, sequentially carrying out treatment by using a pre-impregnation treatment agent and an impregnation oxidizing agent solution; then, injecting a monomer solution into the core package impregnated with the oxidant solution, carrying out temperature-section polymerization treatment, and applying direct-current voltage to the positive electrode and the negative electrode of the core package during the high-temperature-section polymerization treatment; and then, assembling and aging the core cladding subjected to polymerization treatment in the temperature sections to obtain the solid aluminum electrolytic capacitor. The preparation method provided by the invention can reduce the use amount of the monomer and avoid the waste of the monomer, thereby saving the production cost. In addition, the preparation method provided by the invention not only can greatly shorten the polymerization treatment time, but also can effectively improve the initial electrical property of the product.
Description
Technical Field
The invention relates to the technical field of capacitors, in particular to a low-cost solid aluminum electrolytic capacitor and a preparation method thereof.
Background
At present, the production process of the traditional solid aluminum electrolytic capacitor mainly comprises the procedures of nail coiling, welding, formation, drying, impregnation, polymerization or drying, assembly, aging, testing, forming and the like. Specifically, patent CN109192510A in the prior art discloses a method for manufacturing a solid aluminum electrolytic capacitor, which comprises immersing a core package subjected to formation repair treatment in a monomer solution for impregnation treatment; then, injecting an oxidant to carry out polymerization reaction; then, the solid aluminum electrolytic capacitor can be obtained after sealing, assembling and aging.
However, since the above-mentioned preparation method comprises the steps of impregnating the monomer and injecting the oxidant to perform the polymerization reaction, the monomer is easily excessive in the process, and the excessive monomer is volatilized under the dry condition, thereby causing a lot of waste. In addition, the preparation method has the advantages of longer polymerization time, lower production efficiency and higher preparation cost.
Disclosure of Invention
The present invention aims to provide a low-cost solid aluminum electrolytic capacitor and a method for manufacturing the same, so as to solve the problems in the background art.
In order to achieve the above purpose, the embodiments of the present invention provide the following technical solutions:
A preparation method of a low-cost solid-state aluminum electrolytic capacitor comprises the following steps:
(1) Stacking the positive foil, the electrolytic paper and the negative foil together, and winding into a core package;
(2) Applying direct-current voltage on the positive electrode and the negative electrode of the core bag, and immersing the core bag into formation liquid for formation repair treatment;
(3) Drying the core bag subjected to formation repair treatment, and then impregnating the dried core bag with a pretreatment agent; the pretreatment agent is an organic solution containing polydimethylsiloxane;
(4) Firstly, drying the core bag impregnated with the pretreatment agent, and then impregnating the dried core bag with an oxidant solution;
(5) firstly, drying the core bag impregnated with the oxidant solution, and then injecting a monomer solution into the dried core bag;
(6) Carrying out temperature-section-divided polymerization treatment on the core package injected with the monomer solution, and applying direct-current voltage to the positive electrode and the negative electrode of the core package during the high-temperature-section polymerization treatment;
(7) And (3) assembling and aging the core packet subjected to polymerization treatment in different temperature sections to obtain the solid aluminum electrolytic capacitor.
In a preferable embodiment of the present invention, in the step (2), the formation liquid is an aqueous solution of ammonium adipate or an aqueous solution of ammonium dihydrogen phosphate.
In another preferable embodiment adopted in the embodiment of the present invention, in the step (2), the value of the dc voltage applied to the positive electrode and the negative electrode of the core package is 0.8 to 1.2 times of the withstand voltage value of the positive electrode foil.
According to another preferable scheme adopted by the embodiment of the invention, in the step (2), the time of the formation repair treatment is 5-30 min.
In another preferred embodiment of the present invention, in the step (3), the organic solution containing polydimethylsiloxane further contains one or more of ethyl acetate, methyl formate and p-xylene.
According to another preferable scheme adopted by the embodiment of the invention, in the step (3), the mass percentage concentration of the polydimethylsiloxane is 30% -70%.
in another preferred embodiment adopted in the embodiment of the present invention, in the step (4), the solute in the oxidant solution is one or more of iron salt, hydrogen peroxide, peroxysulfate, persulfate, perborate, and copper salt; the solvent in the oxidant solution is one of ethanol, methanol and n-butanol.
According to another preferable scheme adopted by the embodiment of the invention, the mass percentage concentration of the solute in the oxidant solution is 40-60%
according to another preferable scheme adopted by the embodiment of the invention, in the step (5), the solute in the monomer solution is one of pyrrole monomers, thiophene monomers and aniline monomers; the solvent in the monomer solution is one of ethanol, methanol and n-butanol.
According to another preferable scheme adopted by the embodiment of the invention, the mass percentage concentration of the solute in the monomer solution is 15-25%.
In another preferred scheme adopted in the embodiment of the invention, the pyrrole monomer is one of N-methylpyrrole, N-ethylpyrrole and 3-octanoyl pyrrole; the thiophene monomer is one of 3, 4-ethylenedioxythiophene, 3-methoxythiophene and 3-pentoxythiophene; the aniline monomer is one of 4-tert-butyl aniline, N-butyl aniline and o-anisidine.
In another preferable embodiment adopted in the embodiment of the present invention, in the step (6), a value of the dc voltage applied to the positive electrode and the negative electrode of the core package during the high temperature section polymerization treatment is 0.9 to 1.15 times a withstand voltage value of the positive electrode foil.
The embodiment of the invention also provides the solid-state aluminum electrolytic capacitor prepared by the preparation method.
Compared with the prior art, the embodiment of the invention has the beneficial effects that:
(1) According to the embodiment of the invention, the oxidant solution is impregnated firstly, and then the monomer solution is injected into the core bag in a fixed amount, so that the use amount of the monomer can be reduced, the waste of the monomer is avoided, and the production cost can be saved.
(2) In the embodiment of the invention, the core package is electrified during the polymerization treatment in the temperature sections, so that the polymerization treatment time can be greatly shortened, the production efficiency is improved, and the initial electrical property of the solid aluminum electrolytic capacitor product can be effectively improved.
Detailed Description
the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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 invention.
Example 1
The embodiment provides a low-cost solid aluminum electrolytic capacitor and a preparation method thereof, and particularly the preparation method of the solid aluminum electrolytic capacitor comprises the following steps:
(1) The method comprises the steps of cutting the positive electrode foil, the electrolytic paper and the negative electrode foil into specified widths (according to actual requirements), then laminating the electrolytic paper, the positive electrode foil and the negative electrode foil, and winding the laminated electrolytic paper, the positive electrode foil and the negative electrode foil together into a core package.
(2) respectively and electrically connecting the anode lead and the cathode lead of the single core cladding with the anode and the cathode of a power supply, applying voltage to the anode and the cathode of the core cladding, immersing the core cladding in a formation solution, and performing formation repair treatment for 5 min; wherein, the voltage value applied to the positive electrode and the negative electrode of the core bag is 0.8 times of the voltage withstanding value of the positive electrode foil; the formation liquid can be aqueous solution of ammonium adipate in the prior art, specifically, the conductivity of the aqueous solution of ammonium adipate is less than or equal to 2.8 mu S/cm, the pH value is 2.6, and the mass percentage concentration of the ammonium adipate is 3%.
(3) Firstly, placing the core bag subjected to formation repair treatment in a drying oven at 50 ℃ for drying for 120min, and then impregnating the dried core bag with a pretreatment agent; wherein the pretreatment agent is an organic solution containing polydimethylsiloxane; specifically, the organic solution also contains ethyl acetate, wherein the mass percentage concentration of the polydimethylsiloxane is 30%.
(4) Firstly, placing the core package impregnated with the pretreatment agent in a drying oven at 50 ℃ for drying for 90min, and then impregnating the dried core package with an oxidant solution; wherein the solute in the oxidant solution is iron salt; the solvent in the oxidant solution was ethanol, and the solute in the oxidant solution was impregnated for 30min at a mass percentage concentration of 40%.
(5) firstly, placing the core bag impregnated with the oxidant solution in an oven at 100 ℃ for drying for 10min, and then quantitatively injecting a monomer solution into the dried core bag (according to the specification and the size of the actual core bag); wherein, the solute in the monomer solution is pyrrole monomer; the solvent in the monomer solution is ethanol, specifically, the pyrrole monomer is N-methylpyrrole, or N-ethylpyrrole or 3-octanoylpyrrole, but not limited thereto; the solute concentration in the monomer solution was 15% by mass.
(6) Carrying out temperature-section-divided polymerization treatment on the core package injected with the monomer solution, and applying direct-current voltage to the positive electrode and the negative electrode of the core package during the high-temperature-section polymerization treatment; the specific temperature stages and times of the polymerization treatment in temperature stages are as follows: 50 ℃/10min, 75 ℃/20min, 90 ℃/10min, 115 ℃/10min, 135 ℃/5min, 150 ℃/5min, 175 ℃/5 min; wherein the temperature of the high-temperature section polymerization treatment is 175 ℃, and the direct-current voltage value applied to the positive electrode and the negative electrode of the core package during the high-temperature section polymerization treatment is 0.9 times of the voltage withstanding value of the positive electrode foil (rated voltage of a product).
(7) And (3) assembling, aging, testing and forming the core cladding subjected to polymerization treatment in the temperature sections to obtain the solid aluminum electrolytic capacitor.
example 2
The embodiment provides a low-cost solid aluminum electrolytic capacitor and a preparation method thereof, and particularly the preparation method of the solid aluminum electrolytic capacitor comprises the following steps:
(1) The method comprises the steps of cutting the positive electrode foil, the electrolytic paper and the negative electrode foil into specified widths (according to actual requirements), then laminating the electrolytic paper, the positive electrode foil and the negative electrode foil, and winding the laminated electrolytic paper, the positive electrode foil and the negative electrode foil together into a core package.
(2) Respectively and electrically connecting the obtained positive lead and negative lead of the single core cladding with the positive and negative electrodes of a power supply, applying voltage to the positive and negative electrodes of the core cladding, immersing the core cladding in a formation solution, and performing formation repair treatment for 30 min; wherein, the voltage value applied to the positive electrode and the negative electrode of the core bag is 1.2 times of the voltage withstanding value of the positive electrode foil; the formation liquid can be aqueous solution of ammonium dihydrogen phosphate in the prior art, specifically, the aqueous solution of ammonium dihydrogen phosphate has a conductivity of less than or equal to 2.8 μ S/cm, a pH value of 3.6, and a mass percent concentration of ammonium dihydrogen phosphate therein is 0.25%.
(3) firstly, placing the core bag subjected to formation repair treatment in an oven at 125 ℃ for drying for 60min, and then impregnating the dried core bag with a pretreatment agent; wherein the pretreatment agent is an organic solution containing polydimethylsiloxane; specifically, the organic solution also contains methyl formate, wherein the mass percentage concentration of polydimethylsiloxane is 70%.
(4) Firstly, placing the core package impregnated with the pretreatment agent in a drying oven at 125 ℃ for drying for 60min, and then impregnating the dried core package with an oxidant solution; wherein the solute in the oxidant solution is hydrogen peroxide; the solvent in the oxidant solution was methanol, the solute concentration in the oxidant solution was 60% by mass, and the impregnation time was 0.5 min.
(5) firstly, placing the core bag impregnated with the oxidant solution in an oven at 130 ℃ for drying for 3min, and then quantitatively injecting a monomer solution into the dried core bag (according to the specification and the size of the actual core bag); wherein, the solute in the monomer solution is thiophene monomer; the solvent in the monomer solution is methanol, specifically, the thiophene monomer is 3, 4-ethylenedioxythiophene, and 3-methoxythiophene or 3-pentoxythiophene, but is not limited thereto; the solute concentration in the monomer solution was 25% by mass.
(6) Carrying out temperature-section-divided polymerization treatment on the core package injected with the monomer solution, and applying direct-current voltage to the positive electrode and the negative electrode of the core package during the high-temperature-section polymerization treatment; the specific temperature stages and times of the polymerization treatment in temperature stages are as follows: 50 ℃/20min, 75 ℃/30min, 90 ℃/30min, 115 ℃/30min, 135 ℃/15min, 150 ℃/15min, 175 ℃/10 min; wherein the temperature of the high-temperature section polymerization treatment is 175 ℃, and the direct-current voltage value applied to the positive electrode and the negative electrode of the core package during the high-temperature section polymerization treatment is 1.15 times of the voltage withstanding value of the positive electrode foil (rated voltage of a product).
(7) And (3) assembling, aging, testing and forming the core cladding subjected to polymerization treatment in the temperature sections to obtain the solid aluminum electrolytic capacitor.
Example 3
The embodiment provides a low-cost solid aluminum electrolytic capacitor and a preparation method thereof, and particularly the preparation method of the solid aluminum electrolytic capacitor comprises the following steps:
(1) the method comprises the steps of cutting the positive electrode foil, the electrolytic paper and the negative electrode foil into specified widths (according to actual requirements), then laminating the electrolytic paper, the positive electrode foil and the negative electrode foil, and winding the laminated electrolytic paper, the positive electrode foil and the negative electrode foil together into a core package.
(2) Respectively and electrically connecting the obtained positive lead and negative lead of the single core package with the positive and negative electrodes of a power supply, applying voltage to the positive and negative electrodes of the core package, immersing the core package in a formation solution, and performing formation repair treatment for 15 min; wherein, the voltage value applied to the positive electrode and the negative electrode of the core bag is 1 time of the voltage resistance value of the positive electrode foil; the formation liquid can be aqueous solution of ammonium adipate in the prior art, specifically, the conductivity of the aqueous solution of ammonium adipate is less than or equal to 2.8 mu S/cm, the pH value is 3, and the mass percentage concentration of the ammonium adipate is 4%.
(3) Firstly, placing the core bag subjected to formation repair treatment in a drying oven at 90 ℃ for drying for 90min, and then impregnating the dried core bag with a pretreatment agent; wherein the pretreatment agent is an organic solution containing polydimethylsiloxane; specifically, the organic solution also contains methyl formate and p-xylene, wherein the mass percentage concentration of polydimethylsiloxane is 50%.
(4) Firstly, placing the core package impregnated with the pretreatment agent in a drying oven at 90 ℃ for drying for 70min, and then impregnating the dried core package with an oxidant solution; wherein, the solute in the oxidant solution is peroxysulfate, persulfate and perborate; the solvent in the oxidant solution was n-butanol, and the solute in the oxidant solution was contained at a concentration of 50% by mass for 15 min.
(5) Firstly, placing the core bag impregnated with the oxidant solution in an oven at 120 ℃ for drying for 5min, and then quantitatively injecting a monomer solution into the dried core bag (according to the specification and the size of the actual core bag); wherein the solute in the monomer solution is aniline monomer; the solvent in the monomer solution is N-butyl alcohol, specifically, the aniline monomer is 4-tert-butyl aniline, and N-butyl aniline or o-anisidine can also be selected, but is not limited to the above; the solute concentration in the monomer solution was 20% by mass.
(6) carrying out temperature-section-divided polymerization treatment on the core package injected with the monomer solution, and applying direct-current voltage to the positive electrode and the negative electrode of the core package during the high-temperature-section polymerization treatment; the specific temperature stages and times of the polymerization treatment in temperature stages are as follows: 50 ℃/15min, 75 ℃/25min, 90 ℃/15min, 115 ℃/20min, 135 ℃/10min, 150 ℃/10min, 175 ℃/8 min; wherein the temperature of the high-temperature section polymerization treatment is 175 ℃, and the direct-current voltage value applied to the positive electrode and the negative electrode of the core package during the high-temperature section polymerization treatment is 1 time of the voltage withstanding value of the positive electrode foil (rated voltage of a product).
(7) and (3) assembling, aging, testing and forming the core cladding subjected to polymerization treatment in the temperature sections to obtain the solid aluminum electrolytic capacitor.
Example 4
The embodiment provides a low-cost solid aluminum electrolytic capacitor and a preparation method thereof, and particularly the preparation method of the solid aluminum electrolytic capacitor comprises the following steps:
(1) The method comprises the steps of cutting the positive electrode foil, the electrolytic paper and the negative electrode foil into specified widths (according to actual requirements), then laminating the electrolytic paper, the positive electrode foil and the negative electrode foil, and winding the laminated electrolytic paper, the positive electrode foil and the negative electrode foil together into a core package.
(2) Respectively and electrically connecting the obtained positive lead and negative lead of the single core cladding with the positive and negative electrodes of a power supply, applying voltage to the positive and negative electrodes of the core cladding, immersing the core cladding in a formation solution, and performing formation repair treatment for 20 min; wherein, the voltage value applied to the positive electrode and the negative electrode of the core bag is 1 time of the voltage resistance value of the positive electrode foil; the formation liquid can be aqueous solution of ammonium adipate in the prior art, specifically, the conductivity of the aqueous solution of ammonium adipate is less than or equal to 2.8 mu S/cm, the pH value is 3, and the mass percentage concentration of the ammonium adipate is 2%.
(3) Firstly, placing the core bag subjected to formation repair treatment in an oven at 80 ℃ for drying for 100min, and then impregnating the dried core bag with a pretreatment agent; wherein the pretreatment agent is an organic solution containing polydimethylsiloxane; specifically, the organic solution also contains ethyl acetate, methyl formate and p-xylene, wherein the mass percent concentration of polydimethylsiloxane is 40%.
(4) firstly, placing the core packet impregnated with the pretreatment agent in a drying oven at 70 ℃ for drying for 70min, and then impregnating the dried core packet with an oxidant solution; wherein, the solute in the oxidant solution is perborate and copper salt; the solvent in the oxidant solution was ethanol, and the solute in the oxidant solution was 45 mass% and the impregnation time was 25 min.
(5) Firstly, placing the core bag impregnated with the oxidant solution in an oven at 110 ℃ for drying for 8min, and then quantitatively injecting a monomer solution into the dried core bag (according to the specification and the size of the actual core bag); wherein, the solute in the monomer solution is pyrrole monomer; the solvent in the monomer solution is N-butanol, specifically, the pyrrole monomer is N-ethyl pyrrole, or N-methyl pyrrole or 3-octanoyl pyrrole, but not limited thereto; the solute concentration in the monomer solution was 20% by mass.
(6) carrying out temperature-section-divided polymerization treatment on the core package injected with the monomer solution, and applying direct-current voltage to the positive electrode and the negative electrode of the core package during the high-temperature-section polymerization treatment; the specific temperature stages and times of the polymerization treatment in temperature stages are as follows: 50 ℃/10min, 75 ℃/30min, 90 ℃/10min, 115 ℃/10min, 135 ℃/15min, 150 ℃/15min, 175 ℃/10 min; wherein the temperature of the high-temperature section polymerization treatment is 175 ℃, and the direct-current voltage value applied to the positive electrode and the negative electrode of the core package during the high-temperature section polymerization treatment is 1.1 times of the voltage withstanding value of the positive electrode foil (rated voltage of a product).
(7) And (3) assembling, aging, testing and forming the core cladding subjected to polymerization treatment in the temperature sections to obtain the solid aluminum electrolytic capacitor.
Example 5
The embodiment provides a low-cost solid aluminum electrolytic capacitor and a preparation method thereof, and particularly the preparation method of the solid aluminum electrolytic capacitor comprises the following steps:
(1) The method comprises the steps of cutting the positive electrode foil, the electrolytic paper and the negative electrode foil into specified widths (according to actual requirements), then laminating the electrolytic paper, the positive electrode foil and the negative electrode foil, and winding the laminated electrolytic paper, the positive electrode foil and the negative electrode foil together into a core package.
(2) Respectively and electrically connecting the obtained positive lead and negative lead of the single core package with the positive and negative electrodes of a power supply, applying voltage to the positive and negative electrodes of the core package, immersing the core package in a formation solution, and performing formation repair treatment for 15 min; wherein, the voltage value applied to the positive electrode and the negative electrode of the core bag is 1 time of the voltage resistance value of the positive electrode foil; the formation liquid can be aqueous solution of ammonium dihydrogen phosphate in the prior art, specifically, the aqueous solution of ammonium dihydrogen phosphate has a conductivity of not more than 2.8 μ S/cm, a pH value of 3, and a mass percentage concentration of 0.3%.
(3) Firstly, placing the core bag subjected to formation repair treatment in an oven at 125 ℃ for drying for 90min, and then impregnating the dried core bag with a pretreatment agent; wherein the pretreatment agent is an organic solution containing polydimethylsiloxane; specifically, the organic solution also contains p-xylene, wherein the mass percent concentration of polydimethylsiloxane is 60%.
(4) Firstly, placing the core package impregnated with the pretreatment agent in a drying oven at 125 ℃ for drying for 60min, and then impregnating the dried core package with an oxidant solution; wherein, the solute in the oxidant solution is ferric salt, and the solute can be ferric tosylate; the solvent in the oxidant solution was ethanol, and the solute in the oxidant solution was contained at a concentration of 60% by mass for 20 min.
(5) Firstly, placing the core bag impregnated with the oxidant solution in an oven at 125 ℃ for drying for 8min, and then quantitatively injecting a monomer solution into the dried core bag (according to the specification and the size of the actual core bag); wherein, the solute in the monomer solution is thiophene monomer; the solvent in the monomer solution is ethanol, specifically, the thiophene monomer is 3, 4-ethylenedioxythiophene, or 3-methoxythiophene or 3-pentoxythiophene, but is not limited thereto; the solute concentration in the monomer solution was 20% by mass.
(6) Carrying out temperature-section-divided polymerization treatment on the core package injected with the monomer solution, and applying direct-current voltage to the positive electrode and the negative electrode of the core package during the high-temperature-section polymerization treatment; the specific temperature stages and times of the polymerization treatment in temperature stages are as follows: 50 ℃/15min, 75 ℃/20min, 90 ℃/30min, 115 ℃/10min, 135 ℃/10min, 150 ℃/10min, 175 ℃/10 min; wherein the temperature of the high-temperature section polymerization treatment is 175 ℃, and the direct-current voltage value applied to the positive electrode and the negative electrode of the core package during the high-temperature section polymerization treatment is 1 time of the voltage withstanding value of the positive electrode foil (rated voltage of a product).
(7) And (3) assembling, aging, testing and forming the core cladding subjected to polymerization treatment in the temperature sections to obtain the solid aluminum electrolytic capacitor.
Comparative example 1
The comparative example provides a preparation method of a solid-state aluminum electrolytic capacitor, and specifically, the preparation method of the solid-state aluminum electrolytic capacitor comprises the following steps:
(1) The method comprises the steps of cutting the positive electrode foil, the electrolytic paper and the negative electrode foil into specified widths (according to actual requirements), then laminating the electrolytic paper, the positive electrode foil and the negative electrode foil, and winding the laminated electrolytic paper, the positive electrode foil and the negative electrode foil together into a core package.
(2) Respectively and electrically connecting the obtained positive lead and negative lead of the single core package with the positive and negative electrodes of a power supply, applying voltage to the positive and negative electrodes of the core package, immersing the core package in a formation solution, and performing formation repair treatment for 15 min; wherein, the voltage value applied to the positive electrode and the negative electrode of the core bag is 1 time of the voltage resistance value of the positive electrode foil; the formation liquid can be aqueous solution of ammonium dihydrogen phosphate in the prior art, specifically, the aqueous solution of ammonium dihydrogen phosphate has a conductivity of not more than 2.8 μ S/cm, a pH value of 3, and a mass percentage concentration of 0.3%.
(3) firstly, placing the core bag subjected to formation repair treatment in an oven at 125 ℃ for drying for 90min, and then impregnating the dried core bag with a pretreatment agent; wherein the pretreatment agent is an organic solution containing polydimethylsiloxane; specifically, the organic solution also contains p-xylene, wherein the mass percent concentration of polydimethylsiloxane is 60%.
(4) Firstly, placing the core bag impregnated with the pretreatment agent in a drying oven at 125 ℃ for drying for 60min, and then impregnating the dried core bag with a monomer solution; wherein, the solute in the monomer solution is thiophene monomer; the solvent in the monomer solution is ethanol, and specifically, the thiophene monomer is 3, 4-ethylenedioxythiophene; the solute concentration in the monomer solution was 20% by mass, and the impregnation time was 10 min.
(5) Firstly, placing the core package impregnated with the oxidant solution in a drying oven at 50 ℃ for drying for 30min, and then impregnating the dried core package with the oxidant solution; wherein, the solute in the oxidant solution is ferric salt, and the solute can be ferric tosylate; the solvent in the oxidant solution was ethanol, and the solute in the oxidant solution was contained at a concentration of 60% by mass for 10 min.
(6) Carrying out temperature-divided section polymerization treatment on the core packet after being impregnated with the oxidant solution; the specific temperature stages and times of the polymerization treatment in temperature stages are as follows: 50 ℃/15min, 75 ℃/20min, 90 ℃/30min, 115 ℃/10min, 135 ℃/10min, 150 ℃/10min, 175 ℃/10 min;
(7) And (3) assembling, aging, testing and forming the core cladding subjected to polymerization treatment in the temperature sections to obtain the solid aluminum electrolytic capacitor.
10 sets of solid aluminum electrolytic capacitor products having a size of 6.3 x 8 and a specification of 1200uF/2.5V were prepared according to the preparation methods provided in example 5 and comparative example 1, and the 20 sets were subjected to the measurement of Capacitance (CAP), loss Factor (DF), (Equivalent Series Resistance, ESR) values at a frequency of 120Hz, and the measurement of Leakage Current (LC) by applying a voltage of 2.5V to the 20 sets of products, and the measurement results are shown in tables 1-2 (wherein Table 1 is the performance test result of the 10 sets of products prepared in example 5, and Table 2 is the performance test result of the 10 sets of products prepared in comparative example 1).
Table 1 results of performance testing of 10 groups of products obtained in example 5
| serial number | CAP(uF/120Hz) | DF(%) | ESR(mΩ) | LC(uA) |
| 1 | 1109.99 | 2.36 | 6.05 | 46.59 |
| 2 | 1104.01 | 2.34 | 5.98 | 11.96 |
| 3 | 1129.69 | 2.46 | 6.06 | 16.34 |
| 4 | 1131.21 | 2.37 | 6.16 | 16.55 |
| 5 | 1111.81 | 2.29 | 6.13 | 19.78 |
| 6 | 1132.55 | 2.23 | 6.21 | 74.62 |
| 7 | 1129.89 | 2.17 | 5.68 | 48.15 |
| 8 | 1123.04 | 2.56 | 5.83 | 67.45 |
| 9 | 1124.19 | 2.22 | 5.95 | 10.99 |
| 10 | 1135.29 | 2.16 | 6.02 | 15.11 |
table 2 results of performance test of 10 groups of products prepared in comparative example 1
| Serial number | CAP(uF/120Hz) | DF(%) | ESR(mΩ) | LC(uA) |
| 1 | 1135.88 | 2.28 | 5.96 | 116.38 |
| 2 | 1144.29 | 2.28 | 6.23 | 142.01 |
| 3 | 1118.34 | 2.45 | 6.12 | 40.81 |
| 4 | 1125.81 | 2.35 | 6.42 | 86.97 |
| 5 | 1115.10 | 2.50 | 5.84 | 99.70 |
| 6 | 1141.04 | 2.68 | 6.32 | 101.68 |
| 7 | 1146.14 | 2.43 | 6.09 | 95.59 |
| 8 | 1142.65 | 2.32 | 6.01 | 73.22 |
| 9 | 1137.01 | 2.05 | 5.96 | 187.76 |
| 10 | 1147.23 | 2.05 | 6.33 | 70.28 |
As can be seen from tables 1-2 above, the LC of the solid aluminum electrolytic capacitor product prepared in example 5 of the present invention is smaller than that of the solid aluminum electrolytic capacitor product prepared in comparative example 1, which can effectively improve the initial electrical properties of the solid aluminum electrolytic capacitor product.
in summary, in the embodiment of the present invention, the core package is impregnated with the oxidant solution first, and then the monomer solution is injected into the core package at a predetermined amount, so that the usage amount of the monomer can be reduced, the waste of the monomer can be avoided, and the production cost can be saved. In addition, the core package is electrified during the polymerization treatment in the temperature sections, so that the polymerization treatment time can be greatly shortened, the production efficiency is improved, and the initial electrical property of the solid aluminum electrolytic capacitor product can be effectively improved.
In addition, the core package is impregnated with the post-treatment agent, so that the conductive polymer film formed by the conductive polymer dispersion liquid in the core package can be protected, the stability and the conductivity of the conductive polymer film are improved, and the electrical property and the service life of the solid aluminum electrolytic capacitor product can be improved.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. A preparation method of a low-cost solid-state aluminum electrolytic capacitor is characterized by comprising the following steps:
(1) Stacking the positive foil, the electrolytic paper and the negative foil together, and winding into a core package;
(2) Applying direct-current voltage on the positive electrode and the negative electrode of the core bag, and immersing the core bag into formation liquid for formation repair treatment;
(3) Drying the core bag subjected to formation repair treatment, and then impregnating the dried core bag with a pretreatment agent; the pretreatment agent is an organic solution containing polydimethylsiloxane;
(4) Firstly, drying the core bag impregnated with the pretreatment agent, and then impregnating the dried core bag with an oxidant solution;
(5) Firstly, drying the core bag impregnated with the oxidant solution, and then injecting a monomer solution into the dried core bag;
(6) carrying out temperature-section-divided polymerization treatment on the core package injected with the monomer solution, and applying direct-current voltage to the positive electrode and the negative electrode of the core package during the high-temperature-section polymerization treatment;
(7) And (3) assembling and aging the core packet subjected to polymerization treatment in different temperature sections to obtain the solid aluminum electrolytic capacitor.
2. The method for manufacturing a low-cost solid aluminum electrolytic capacitor as claimed in claim 1, wherein in the step (2), the formation liquid is an aqueous solution of ammonium adipate or an aqueous solution of ammonium dihydrogen phosphate.
3. The method for preparing a low-cost solid aluminum electrolytic capacitor as claimed in claim 2, wherein in the step (2), the dc voltage value applied to the positive and negative electrodes of the core pack is 0.8-1.2 times of the withstand voltage value of the positive foil.
4. The method for preparing a low-cost solid aluminum electrolytic capacitor as claimed in claim 3, wherein in the step (2), the time for the formation repair treatment is 5-30 min.
5. The method for preparing a low-cost solid aluminum electrolytic capacitor as claimed in claim 1, wherein in the step (3), the organic solution containing polydimethylsiloxane further contains one or more of ethyl acetate, methyl formate and p-xylene.
6. The method for preparing a low-cost solid aluminum electrolytic capacitor as claimed in claim 5, wherein the concentration of polydimethylsiloxane in step (3) is 30-70% by weight.
7. The method for preparing a low-cost solid aluminum electrolytic capacitor as claimed in claim 1, wherein in the step (4), the solute in the oxidant solution is one or more of iron salt, hydrogen peroxide, peroxysulfate, persulfate, perborate and copper salt; the solvent in the oxidant solution is one of ethanol, methanol and n-butanol.
8. The method for preparing a low-cost solid-state aluminum electrolytic capacitor according to claim 1, wherein in the step (5), the solute in the monomer solution is one of pyrrole monomers, thiophene monomers and aniline monomers; the solvent in the monomer solution is one of ethanol, methanol and n-butanol.
9. The method for preparing a low-cost solid-state aluminum electrolytic capacitor as claimed in claim 1, wherein in the step (6), the dc voltage value applied to the positive and negative electrodes of the core package during the high temperature section polymerization process is 0.9-1.15 times of the withstand voltage value of the positive foil.
10. a solid-state aluminum electrolytic capacitor produced by the production method according to any one of claims 1 to 9.
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Application publication date: 20191206 |