CN113257578B - Preparation method of 150 ℃ high-temperature-resistant solid polymer aluminum electrolytic capacitor - Google Patents
Preparation method of 150 ℃ high-temperature-resistant solid polymer aluminum electrolytic capacitor Download PDFInfo
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- CN113257578B CN113257578B CN202110621710.6A CN202110621710A CN113257578B CN 113257578 B CN113257578 B CN 113257578B CN 202110621710 A CN202110621710 A CN 202110621710A CN 113257578 B CN113257578 B CN 113257578B
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 119
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- 238000002360 preparation method Methods 0.000 title claims description 16
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 7
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- FLDCSPABIQBYKP-UHFFFAOYSA-N 5-chloro-1,2-dimethylbenzimidazole Chemical compound ClC1=CC=C2N(C)C(C)=NC2=C1 FLDCSPABIQBYKP-UHFFFAOYSA-N 0.000 claims description 6
- 239000001741 Ammonium adipate Substances 0.000 claims description 6
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- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 2
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- 238000004806 packaging method and process Methods 0.000 claims description 2
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims 2
- 239000005696 Diammonium phosphate Substances 0.000 claims 1
- -1 flavonoid compounds Chemical class 0.000 abstract description 6
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- LRBQNJMCXXYXIU-QWKBTXIPSA-N gallotannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@H]2[C@@H]([C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-QWKBTXIPSA-N 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 15
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 11
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- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 4
- 229920000144 PEDOT:PSS Polymers 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 4
- 235000011187 glycerol Nutrition 0.000 description 4
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- 229920006254 polymer film Polymers 0.000 description 2
- 125000004151 quinonyl group Chemical group 0.000 description 2
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-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
- QNVSXXGDAPORNA-UHFFFAOYSA-N Resveratrol Natural products OC1=CC=CC(C=CC=2C=C(O)C(O)=CC=2)=C1 QNVSXXGDAPORNA-UHFFFAOYSA-N 0.000 description 1
- LUKBXSAWLPMMSZ-OWOJBTEDSA-N Trans-resveratrol Chemical compound C1=CC(O)=CC=C1\C=C\C1=CC(O)=CC(O)=C1 LUKBXSAWLPMMSZ-OWOJBTEDSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000004636 anthocyanins Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
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- 235000005487 catechin Nutrition 0.000 description 1
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 1
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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
- H01G9/15—Solid 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
- H01G9/08—Housing; Encapsulation
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The invention relates to a method for preparing a solid polymer aluminum electrolytic capacitor resistant to high temperature of 150 ℃, which comprises the steps of immersing a capacitor element with aluminum and a dielectric layer formed by an aluminum oxide film in a conductive polymer aqueous dispersion, taking out, drying and operating at least once to obtain a capacitor element with a conductive polymer layer; then soaking the capacitor element in a plant polyphenol aqueous solution, wherein the plant polyphenol in the plant polyphenol aqueous solution comprises at least one of flavonoid compounds, tannin compounds, anthocyanin compounds and phenolic acid compounds, taking out the capacitor element after soaking for at least 20 minutes, drying the capacitor element at 155-165 ℃ for 1-3 hours, and performing at least one operation to obtain a plant polyphenol self-polymerization protective film outside the conductive polymer layer; after the assembly, the solid polymer aluminum electrolytic capacitor which can resist the high temperature of 150 ℃ is prepared; the method can improve the high temperature resistance of the solid polymer aluminum electrolytic capacitor and reduce the leakage current.
Description
Technical Field
The invention relates to the technical field of capacitors, in particular to a preparation method of a solid polymer aluminum electrolytic capacitor resistant to high temperature of 150 ℃.
Background
The traditional solid polymer aluminum electrolytic capacitor is generally manufactured by two production processes: in-situ polymerization of EDOT to form high molecular polymer; ② PEDOT/PSS is pre-polymerized, impregnated and dried to form high molecular polymer. In the two processes, the material polymerized in situ has strong corrosivity, which can cause the damage of the insulating oxide film on the surface of the positive foil, so that the leakage current of the final capacitor is larger and the voltage resistance is lower, therefore, the process is generally used for manufacturing the capacitor within 25V. And the PEDOT/PSS prepolymerization process has no corrosivity of in-situ polymerization, so that the problems of low voltage resistance and high leakage current of the capacitor are greatly improved, and the process is generally used for manufacturing 25-250V solid polymer aluminum capacitors.
However, the PEDOT/PSS prepolymerized high molecular polymer material has poor chemical stability at high temperature, the rubber plug for sealing can be cracked at high temperature, air in the external environment can permeate into the capacitor through the surface of the rubber plug and generate chemical reaction with the high molecular polymer material in the capacitor, so that the capacitor fails, and the high molecular polymer material cannot be operated in the high temperature environment for a long time.
In order to improve the high temperature resistance of the solid polymer aluminum electrolytic capacitor, the high temperature heat resistance of the rubber plug can be increased; secondly, the structure of the capacitor is changed (the thickness of the rubber plug is increased, or the exposed area of the rubber material is reduced); and improving the chemical stability of the PEDOT/PSS prepolymerized high molecular polymer material at high temperature. The improvement method needs the research and development of a rubber plug manufacturer; secondly, the volume or the appearance structure of the capacitor can be increased by changing the structure of the capacitor, and the customer acceptance is low; and the mode for improving the chemical stability of the PEDOT/PSS prepolymerized high polymer material at high temperature is the development direction.
Disclosure of Invention
In order to solve the technical problem that the high temperature resistance of the solid polymer aluminum electrolytic capacitor is poor so that the capacitor cannot operate for a long time at high temperature, the preparation method of the solid polymer aluminum electrolytic capacitor resistant to the high temperature of 150 ℃ is provided. The invention can improve the high temperature resistance of the solid polymer aluminum electrolytic capacitor by covering a protective film on the polymer conductive polymer.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for preparing a solid polymer aluminum electrolytic capacitor resistant to high temperature of 150 ℃ comprises the steps of immersing a capacitor element with aluminum and a dielectric layer formed by an aluminum oxide film in a conductive polymer aqueous dispersion, taking out, drying and operating at least once to obtain a capacitor element with a conductive polymer layer;
then soaking the capacitor element with the conductive polymer layer into a plant polyphenol aqueous solution, taking out, drying, and performing at least one operation to obtain the capacitor element of the plant polyphenol self-polymerization protective film outside the conductive polymer layer;
after the assembly, the solid polymer aluminum electrolytic capacitor which can resist the high temperature of 150 ℃ is prepared.
Further, a preparation method of the solid polymer aluminum electrolytic capacitor resistant to the high temperature of 150 ℃, which comprises the following steps:
(1) cutting the anode aluminum foil, the electrolytic paper and the cathode aluminum foil into a specified sheet width, stacking the sheets in sequence, adding a metal lead, riveting and winding the sheets into a core package;
(2) immersing the core bag in a formation solution and electrifying the core bag to form a formation repair so as to repair the oxide film defect on the surface of the anode aluminum foil, and drying the core bag after the formation is finished to obtain a capacitor element;
(3) immersing the capacitor element after the formation and repair into the conductive high polymer aqueous dispersion, drying, and performing at least one operation to form the capacitor element with the conductive high polymer layer;
(4) then soaking the conductive polymer layer in plant polyphenol water solution, taking out, drying and performing at least one operation to obtain a capacitor element of the plant polyphenol self-polymerization protective film outside the conductive polymer layer;
(5) and finally, placing the aluminum shell into an aluminum shell, sealing the rubber plug, assembling and packaging the aluminum shell into a sealing structure, cleaning the surface, and performing aging treatment to obtain the solid polymer aluminum electrolytic capacitor resistant to the high temperature of 150 ℃.
Further, the plant polyphenol in the plant polyphenol water solution comprises at least one of flavonoid compounds, tannin compounds, anthocyanin compounds and phenolic acid compounds; the mass concentration of the plant polyphenol water solution is 0.01-25%; the time for soaking the plant polyphenol aqueous solution is at least 20 minutes, and the drying temperature after taking out is 155-165 ℃ for drying for 1-3 hours.
Still further, the plant polyphenol is at least one of catechin, resveratrol, anthocyanin, quinic acid, tannic acid and gallic acid.
Preferably, the plant polyphenol is at least one of quinic acid, tannic acid and gallic acid.
Further, the step (4) is repeated for 1-3 times.
Furthermore, the conductive high molecular polymer aqueous dispersion is PEDOT/PSS aqueous dispersion.
Further, the formation liquid is one or more of diammonium hydrogen phosphate, ammonium adipate and boric acid; the mass concentration of the formed liquid is 0.01-10%.
Further, the formation repair in the step (2) adopts a step-by-step boosting mode: the first step is that the electrified formation repair time is 5-20 minutes after the anode aluminum foil is pressed under 0.3 times of the anode aluminum foil voltage; the second step is that the time of electrifying, forming and repairing is 5-20 minutes after pressing under the condition that the voltage of the anode aluminum foil is 0.7 times that of the anode aluminum foil; and thirdly, under the condition that the voltage of the anode aluminum foil is 1 time, the electrifying time is 5-20 minutes after the anode aluminum foil is pressed, so that the oxide film defect on the surface of the anode foil is repaired.
The beneficial technical effects are as follows:
in the invention, after the conductive polymer layer is formed, a polymer protective film is attached to the conductive polymer layer, and the polymer protective film is formed by self-polymerization of plant polyphenol at a high temperature of 155-165 ℃. This is because plant polyphenols such as tannic acid and quinic acid are very likely to generate free radicals in a high temperature environment and can react with oxygen to oxidize and self-polymerize into a polymer protective film. The polymer protective film protects the conductive polymer layer and is used as a barrier to prevent the conductive polymer layer from being deteriorated under the conditions of oxygen, moisture, heat and the like after the conductive polymer layer is contacted with oxygen, moisture, a heat environment and the like. The protective action of the plant polyphenol self-polymerization protective film is equivalent to that of an antioxidant, even though the density of the formed plant polyphenol self-polymerization protective film is not considered to be high, pores may exist, so that the conductive polymer layer of the inner layer is affected by conditions such as thermal oxygen and the like to generate degradation and decomposition into free radicals, then the exposed hydroxyl groups on the plant polyphenol self-polymerization protective film of the outer layer can be simultaneously dehydrogenated and combined with oxygen in the environment to prevent the oxidation of the conductive polymer layer of the inner layer by the oxygen, or the two adjacent exposed hydroxyls on the outer plant polyphenol self-polymerization protective film are condensed to form a quinone structure, the quinone structure is combined with degraded conductive polymer free radicals to break the chain initiation process, break the chain initiation of the free radicals, thereby preventing further oxidative degradation of the conductive polymer by oxygen heat and the like, and preventing the conductive polymer layer from thermal degradation aging and conductivity reduction caused by thermal oxidative degradation aging. The oxidation polymerization of the plant polyphenol substances forms a huge polymer film to cover the capacitor, so that the capacitor has better high-temperature resistance in a high-temperature environment, the problem of large high-temperature capacity attenuation of the capacitor is solved, and the leakage current of the capacitor can be reduced.
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. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. 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.
Unless specifically stated otherwise, the numerical values set forth in these examples do not limit the scope of the invention. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
Example 1
A preparation method of a solid polymer aluminum electrolytic capacitor resistant to high temperature of 150 ℃ comprises the following steps:
impregnating a capacitor element having aluminum and a dielectric layer formed of an aluminum oxide film in an aqueous dispersion of a conductive polymer, taking out the capacitor element, drying the capacitor element, and performing at least one operation to obtain a capacitor element having a conductive polymer layer; then soaking the capacitor element with the conductive polymer layer into a plant polyphenol aqueous solution, taking out, drying, and performing at least one operation to obtain the capacitor element of the plant polyphenol self-polymerization protective film outside the conductive polymer layer; assembling to obtain a solid polymer aluminum electrolytic capacitor;
the preparation method of the solid polymer aluminum electrolytic capacitor resistant to the high temperature of 150 ℃ in the embodiment comprises the following steps:
(1) cutting the anode aluminum foil, the electrolytic paper and the cathode aluminum foil into a specified sheet width, stacking the sheets in sequence, adding a metal lead, riveting and winding the sheets into a core package;
(2) immersing the core wrap in a formation solution (5% by mass of ammonium adipate aqueous solution) and electrifying to form repair, wherein the formation repair adopts a step-by-step pressure boosting mode: the first step is that the time of electrifying, forming and repairing is 10 minutes after pressing under the condition that the voltage of the anode aluminum foil is 0.3 times that of the anode aluminum foil; the second step is that the time of electrifying, forming and repairing is 10 minutes after pressing under the condition that the voltage of the anode aluminum foil is 0.7 times that of the anode aluminum foil; thirdly, under the voltage of 1 time of the positive aluminum foil, the electrifying time is 15 minutes after the positive aluminum foil is pressed, so that the oxide film defect on the surface of the positive aluminum foil is repaired, and the capacitor element is obtained after the formation and the drying are finished;
(3) immersing the capacitor element after formation repair in conductive high molecular polymer aqueous dispersion (PEDOT: PSS aqueous dispersion) for 10 minutes, drying at 160 ℃ for 2 hours, and performing operation twice to form a capacitor element with a conductive high molecular layer;
(4) then soaking the conductive polymer layer in a tannic acid aqueous solution (with the mass concentration of 5%) for 20 minutes, taking out the conductive polymer layer, and drying the conductive polymer layer at 160 ℃ for 2 hours, wherein the operations are performed twice to obtain a capacitor element of the tannic acid self-polymerization protective film outside the conductive polymer layer;
(5) finally, the solid polymer aluminum electrolytic capacitor is put into an aluminum shell, the rubber plug is sealed, the solid polymer aluminum electrolytic capacitor is assembled and packaged into a sealing structure, the surface is cleaned, and the solid polymer aluminum electrolytic capacitor of the embodiment is prepared through aging treatment.
Example 2
A preparation method of a solid polymer aluminum electrolytic capacitor resistant to high temperature of 150 ℃ comprises the following steps:
impregnating a capacitor element having aluminum and a dielectric layer formed of an aluminum oxide film in an aqueous dispersion of a conductive polymer, taking out the capacitor element, drying the capacitor element, and performing at least one operation to obtain a capacitor element having a conductive polymer layer; then soaking the capacitor element with the conductive polymer layer into a plant polyphenol aqueous solution, taking out, drying, and performing at least one operation to obtain the capacitor element of the plant polyphenol self-polymerization protective film outside the conductive polymer layer; assembling to obtain a solid polymer aluminum electrolytic capacitor;
the preparation method of the solid polymer aluminum electrolytic capacitor resistant to the high temperature of 150 ℃ in the embodiment comprises the following steps:
(1) cutting the anode aluminum foil, the electrolytic paper and the cathode aluminum foil into a specified sheet width, stacking the sheets in sequence, adding a metal lead, riveting and winding the sheets into a core package;
(2) immersing the core wrap in a formation solution (5% by mass of ammonium adipate aqueous solution) and electrifying to form repair, wherein the formation repair adopts a step-by-step pressure boosting mode: the first step is that the time of electrifying, forming and repairing is 10 minutes after pressing under the condition that the voltage of the anode aluminum foil is 0.3 times that of the anode aluminum foil; the second step is that the time of electrifying, forming and repairing is 10 minutes after pressing under the condition that the voltage of the anode aluminum foil is 0.7 times that of the anode aluminum foil; thirdly, under the voltage of 1 time of the positive aluminum foil, the electrifying time is 15 minutes after the positive aluminum foil is pressed, so that the oxide film defect on the surface of the positive aluminum foil is repaired, and the capacitor element is obtained after the formation and the drying are finished;
(3) immersing the capacitor element after formation repair in conductive high molecular polymer aqueous dispersion (PEDOT: PSS aqueous dispersion) for 10 minutes, drying at 160 ℃ for 2 hours, and performing operation twice to form a capacitor element with a conductive high molecular layer;
(4) then soaking the conductive polymer layer in a tannic acid aqueous solution (with the mass concentration of 10%) for 20 minutes, taking out the conductive polymer layer, and drying the conductive polymer layer at 160 ℃ for 2 hours, wherein the operations are performed twice to obtain a capacitor element of the tannic acid self-polymerization protective film outside the conductive polymer layer;
(5) finally, the solid polymer aluminum electrolytic capacitor is put into an aluminum shell, the rubber plug is sealed, the solid polymer aluminum electrolytic capacitor is assembled and packaged into a sealing structure, the surface is cleaned, and the solid polymer aluminum electrolytic capacitor of the embodiment is prepared through aging treatment.
Example 3
A preparation method of a solid polymer aluminum electrolytic capacitor resistant to high temperature of 150 ℃ comprises the following steps:
impregnating a capacitor element having aluminum and a dielectric layer formed of an aluminum oxide film in an aqueous dispersion of a conductive polymer, taking out the capacitor element, drying the capacitor element, and performing at least one operation to obtain a capacitor element having a conductive polymer layer; then soaking the capacitor element with the conductive polymer layer into a plant polyphenol aqueous solution, taking out, drying, and performing at least one operation to obtain the capacitor element of the plant polyphenol self-polymerization protective film outside the conductive polymer layer; assembling to obtain a solid polymer aluminum electrolytic capacitor;
the preparation method of the solid polymer aluminum electrolytic capacitor resistant to the high temperature of 150 ℃ in the embodiment comprises the following steps:
(1) cutting the anode aluminum foil, the electrolytic paper and the cathode aluminum foil into a specified sheet width, stacking the sheets in sequence, adding a metal lead, riveting and winding the sheets into a core package;
(2) immersing the core wrap in a formation solution (5% by mass of ammonium adipate aqueous solution) and electrifying to form repair, wherein the formation repair adopts a step-by-step pressure boosting mode: the first step is that the time of electrifying, forming and repairing is 10 minutes after pressing under the condition that the voltage of the anode aluminum foil is 0.3 times that of the anode aluminum foil; the second step is that the time of electrifying, forming and repairing is 10 minutes after pressing under the condition that the voltage of the anode aluminum foil is 0.7 times that of the anode aluminum foil; thirdly, under the voltage of 1 time of the positive aluminum foil, the electrifying time is 15 minutes after the positive aluminum foil is pressed, so that the oxide film defect on the surface of the positive aluminum foil is repaired, and the capacitor element is obtained after the formation and the drying are finished;
(3) immersing the capacitor element after formation repair in conductive high molecular polymer aqueous dispersion (PEDOT: PSS aqueous dispersion) for 10 minutes, drying at 160 ℃ for 2 hours, and performing operation twice to form a capacitor element with a conductive high molecular layer;
(4) then soaking the conductive polymer layer in quinic acid aqueous solution (mass concentration is 5%) for 20 minutes, taking out the conductive polymer layer, drying the conductive polymer layer at 160 ℃ for 2 hours, and performing operation twice to obtain a capacitor element of the quinic acid self-polymerization protective film outside the conductive polymer layer;
(5) finally, the solid polymer aluminum electrolytic capacitor is put into an aluminum shell, the rubber plug is sealed, the solid polymer aluminum electrolytic capacitor is assembled and packaged into a sealing structure, the surface is cleaned, and the solid polymer aluminum electrolytic capacitor of the embodiment is prepared through aging treatment.
Example 4
A preparation method of a solid polymer aluminum electrolytic capacitor resistant to high temperature of 150 ℃ comprises the following steps:
impregnating a capacitor element having aluminum and a dielectric layer formed of an aluminum oxide film in an aqueous dispersion of a conductive polymer, taking out the capacitor element, drying the capacitor element, and performing at least one operation to obtain a capacitor element having a conductive polymer layer; then soaking the capacitor element with the conductive polymer layer into a plant polyphenol aqueous solution, taking out, drying, and performing at least one operation to obtain the capacitor element of the plant polyphenol self-polymerization protective film outside the conductive polymer layer; assembling to obtain a solid polymer aluminum electrolytic capacitor;
the preparation method of the solid polymer aluminum electrolytic capacitor resistant to the high temperature of 150 ℃ in the embodiment comprises the following steps:
(1) cutting the anode aluminum foil, the electrolytic paper and the cathode aluminum foil into a specified sheet width, stacking the sheets in sequence, adding a metal lead, riveting and winding the sheets into a core package;
(2) immersing the core wrap in a formation solution (5% by mass of ammonium adipate aqueous solution) and electrifying to form repair, wherein the formation repair adopts a step-by-step pressure boosting mode: the first step is that the time of electrifying, forming and repairing is 10 minutes after pressing under the condition that the voltage of the anode aluminum foil is 0.3 times that of the anode aluminum foil; the second step is that the time of electrifying, forming and repairing is 10 minutes after pressing under the condition that the voltage of the anode aluminum foil is 0.7 times that of the anode aluminum foil; thirdly, under the voltage of 1 time of the positive aluminum foil, the electrifying time is 15 minutes after the positive aluminum foil is pressed, so that the oxide film defect on the surface of the positive aluminum foil is repaired, and the capacitor element is obtained after the formation and the drying are finished;
(3) immersing the capacitor element after formation repair in conductive high molecular polymer aqueous dispersion (PEDOT: PSS aqueous dispersion) for 10 minutes, drying at 160 ℃ for 2 hours, and performing operation twice to form a capacitor element with a conductive high molecular layer;
(4) then soaking the conductive polymer layer in quinic acid aqueous solution (with the mass concentration of 10%) for 20 minutes, taking out the conductive polymer layer, drying the conductive polymer layer at 160 ℃ for 2 hours, and performing operation twice to obtain a capacitor element of the quinic acid self-polymerization protective film outside the conductive polymer layer;
(5) finally, the solid polymer aluminum electrolytic capacitor is put into an aluminum shell, the rubber plug is sealed, the solid polymer aluminum electrolytic capacitor is assembled and packaged into a sealing structure, the surface is cleaned, and the solid polymer aluminum electrolytic capacitor of the embodiment is prepared through aging treatment.
Example 5
The solid polymer aluminum electrolytic capacitor of this example was produced in the same manner as in example 1, except that in step (4), the capacitor element having a conductive polymer layer was immersed in a mixed aqueous solution of tannic acid and quinic acid (10% by mass, 1:1 by mass of tannic acid to quinic acid) for 20 minutes, and then dried at 160 ℃ for 2 hours after taking out.
Comparative example 1
The solid polymer aluminum electrolytic capacitor of this comparative example was produced in the same manner as in example 5 except that step (4) was not present.
Comparative example 2
The solid polymer aluminum electrolytic capacitor of this comparative example was produced in the same manner as in example 5, except that in step (4), the capacitor element having the conductive polymer layer was immersed in a mixed solution of glycerin and sorbitol (mass ratio of 1: 1).
The durability test was performed by applying a rated dc voltage at a high temperature of 150 c to the above examples and comparative capacitors, and 5 capacitors were manufactured for each of the examples and comparative examples to perform the electrical parameter measurement test of the capacitors. In the measurement of electrical parameters of the capacitor, capacitance (Cap, 25 ℃ C. 120 Hz), loss tangent (Df, 25 ℃ C. 120 Hz), and equivalent series resistance (ESR, 25 ℃ C. 100 KHz) were measured using an LCR tester, model 4284A, manufactured by Agilent, and leakage current (Lc, 25 ℃ C. applied with a rated voltage of 35V for 1 minute) was measured using a leakage current tester, model TH2689A, manufactured by Tongh. mu.i. The measured data are shown in Table 1.
TABLE 1 examples and 150 ℃ high temperature durability test data for comparative capacitors
（35V270μF, D10*12.5）
As can be seen from Table 1, comparative example 1, which is not impregnated with polyhydroxy-based material, has capacity fading already at 150 degrees 1000H, reaching a maximum of about-14% capacity fading, and at 3000H, the capacity can only reach about 74% of the initial value; the ESR changes more obviously, the ESR reaches 3-4 times of the initial value at 1000H, and the ESR reaches 15 times of the initial value at 3000H. In examples 1-5, the problem of high temperature capacitance attenuation of the capacitor can be effectively improved by impregnating plant polyphenols outside the conductive polymer layer and self-polymerizing the plant polyphenols on the surface of the conductive polymer layer to obtain the polymer protective film, and the ESR rise rate after 3000H is not more than 1.5 times. Among them, the parameters of example 1 and example 5 are stable, and are preferred examples.
Compared with the ESR of the embodiment 2, the ESR of the embodiment 1 is lower, and the capacity attenuation is stable, which shows that in a certain range, the increase of the concentration of the tannic acid aqueous solution is more beneficial to the absorption of the core package of the capacitor, and is more beneficial to the wrapping and protection of the tannic acid self-polymerization protective film on the conductive polymer layer of the capacitor;
compared with the embodiment 4, the embodiment 4 has lower capacitance attenuation in the embodiment 3, which shows that in a certain range, the increase of the concentration of the quinic acid aqueous solution is more beneficial to the wrapping and protection of the quinic acid group polymeric protective film on the conductive polymer layer of the capacitor;
compared with the embodiments 3 and 4, the embodiment 1 has smaller capacity attenuation, and it is preliminarily considered that the tannic acid has a larger molecular weight than quinic acid, and after the tannic acid is soaked in the core package of the capacitor under the condition of the same concentration, an effective self-polymerization protective film layer can be formed on the surface of the conductive polymer layer, and the contact between the conductive polymer layer and air is reduced, so that the deterioration of the conductive polymer layer is avoided, the structural stability of the conductive polymer layer is improved, and the service life of the capacitor is prolonged;
example 5 compared to example 1, the capacitance attenuation of example 5 is close to, the ESR is slightly larger, but the leakage current of the capacitor is smaller, and it can be found that: under the mutual soluble condition of tannic acid and quinic acid, due to the addition of quinic acid, the protection effect of the formed self-polymerization protective film layer on the conductive polymer layer is not obviously reduced, the leakage current (Lc) of the capacitor can also be reduced to a certain degree, and the consistency of the leakage current of the capacitor is improved.
The comparative example 2 adopts the glycerol and sorbitol solution with the mass ratio of 1:1, and the oxidative polymerization polymer film layer cannot be obtained on the surface of the conductive polymer layer, because the glycerol and sorbitol are difficult to obtain free radicals under the high-temperature drying condition, and can be subjected to oxidative polymerization with oxygen only under the condition of the noble metal catalyst, so that the comparative example 2 adopting the glycerol and sorbitol with the mass ratio of 1:1 as the protective film still has larger capacity attenuation and more obvious ESR increase, but the ESR is less changed than that of the comparative example 1, and has a certain effect of reducing the ESR. Likewise, under the condition of no catalyst, such as hydroxybenzoic acid compounds, phenol compounds and the like, the self-polymerization can not occur, and these substances are all oil-soluble compounds, and organic solvent is needed for dissolving or converting the compounds into water-soluble substances, so that the cost is increased after the operation, and the ESR rise is still higher after high temperature compared with the method of the present invention.
The high-temperature resistance of the solid polymer aluminum electrolytic capacitor can be effectively improved by the aqueous solution containing plant polyphenols, wherein the 5% tannic acid aqueous solution has obvious effect and meets the design requirement under the high-temperature condition of 150 ℃. According to requirements, the 10% (tannic acid: quinic acid =1:1) mixed aqueous solution can reduce the leakage current of the capacitor under the condition that other electrical properties are not changed greatly, and the consistency of the leakage current is good.
For the capacitors produced by the above examples and comparative examples, 5 additional capacitors were produced and tested for the insulation breakdown voltage BDV using a tester model TH2689A with a test current of 1mA and a delay time of 180s, as shown in table 2.
TABLE 2 BDV insulation breakdown Voltage test data for the examples and comparative examples capacitors
（35v270 D10*12.5）
Note: the unit of data in the table is V.
As is clear from Table 2, it is understood from the average value that the BVD of comparative example 1 in which no self-polymerizable protective film of plant polyphenol is attached to the surface of the conductive polymer layer is 51.8V, whereas the BVD of the capacitor is increased to 54-60V after the self-polymerizable protective film of plant polyphenol is attached to the surface of the conductive polymer layer in examples 1-5 of the present invention, which indicates that the withstand voltage of the capacitor is increased and that the leakage current is reduced as well from the reverse side. While comparative example 2 using the conventional hydroxy compound did not significantly improve the withstand voltage.
The protective film is obtained by utilizing the fact that plant polyphenols are oxidized and self-polymerized at high temperature to obtain the high-molecular protective film, and the high-molecular protective film obtained by self-polymerization has hydrophobicity and solvent resistance. In addition, the invention does not need to use organic solvent, and has lower cost.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. A method for preparing a solid polymer aluminum electrolytic capacitor resistant to high temperature of 150 ℃ is characterized in that a capacitor element with a dielectric layer formed by aluminum and an aluminum oxide film is soaked in a conductive polymer aqueous dispersion, and then taken out, dried and operated at least once to obtain a capacitor element with a conductive polymer layer;
then soaking the capacitor element with the conductive polymer layer into a plant polyphenol aqueous solution, taking out, drying, and performing at least one operation to obtain the capacitor element of the plant polyphenol self-polymerization protective film outside the conductive polymer layer;
after the assembly, the solid polymer aluminum electrolytic capacitor which can resist the high temperature of 150 ℃ is prepared;
the plant polyphenol in the plant polyphenol water solution is quinic acid and tannic acid, and the mass ratio of the tannic acid to the quinic acid is 1: 1; the mass concentration of the plant polyphenol water solution is 10 percent; the plant polyphenol aqueous solution was impregnated for 20 minutes, and the drying temperature after taking out was 160 ℃ for 2 hours.
2. The preparation method of the 150 ℃ high-temperature-resistant solid polymer aluminum electrolytic capacitor according to claim 1 is characterized by comprising the following specific steps:
(1) cutting the anode aluminum foil, the electrolytic paper and the cathode aluminum foil into a specified sheet width, stacking the sheets in sequence, adding a metal lead, riveting and winding the sheets into a core package;
(2) immersing the core bag in a formation solution and electrifying the core bag to form a formation repair so as to repair the oxide film defect on the surface of the anode aluminum foil, and drying the core bag after the formation is finished to obtain a capacitor element;
(3) immersing the capacitor element after the formation and repair into the conductive high polymer aqueous dispersion, drying, and performing at least one operation to form the capacitor element with the conductive high polymer layer;
(4) then soaking the conductive polymer layer in plant polyphenol water solution, taking out, drying and performing at least one operation to obtain a capacitor element of the plant polyphenol self-polymerization protective film outside the conductive polymer layer;
(5) and finally, placing the aluminum shell into an aluminum shell, sealing the rubber plug, assembling and packaging the aluminum shell into a sealing structure, cleaning the surface, and performing aging treatment to obtain the solid polymer aluminum electrolytic capacitor resistant to the high temperature of 150 ℃.
3. The method according to claim 2, wherein the step (4) is repeated 1 to 3 times.
4. The method according to claim 1 or 2, wherein the aqueous dispersion of the conductive polymer is an aqueous dispersion of PEDOT PSS.
5. The preparation method according to claim 2, wherein the formation solution is one or more of diammonium phosphate, ammonium adipate and boric acid; the mass concentration of the formed liquid is 0.01-10%.
6. The preparation method according to claim 2, wherein the formation repair in the step (2) adopts a step-by-step boosting mode: the first step is that the electrified formation repair time is 5-20 minutes after the anode aluminum foil is pressed under 0.3 times of the anode aluminum foil voltage; the second step is that the time of electrifying, forming and repairing is 5-20 minutes after pressing under the condition that the voltage of the anode aluminum foil is 0.7 times that of the anode aluminum foil; and thirdly, under the condition that the voltage of the anode aluminum foil is 1 time, the electrifying time is 5-20 minutes after the anode aluminum foil is pressed, so that the oxide film defect on the surface of the anode foil is repaired.
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| CN105632768A (en) * | 2016-01-13 | 2016-06-01 | 湖南艾华集团股份有限公司 | Square solid-state capacitor and fabrication method thereof |
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| TW200741780A (en) * | 2005-12-27 | 2007-11-01 | Showa Denko Kk | Solid electrolyte capacitor and production method thereof |
| CN103518244A (en) * | 2011-05-12 | 2014-01-15 | 帝化株式会社 | Method for manufacturing solid electrolyte capacitor |
| CN105632768A (en) * | 2016-01-13 | 2016-06-01 | 湖南艾华集团股份有限公司 | Square solid-state capacitor and fabrication method thereof |
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