CN111875828A - Polymer capacitor film with high breakdown field strength and preparation method thereof - Google Patents
Polymer capacitor film with high breakdown field strength and preparation method thereof Download PDFInfo
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- 230000015556 catabolic process Effects 0.000 title claims abstract description 34
- 239000003990 capacitor Substances 0.000 title claims abstract description 25
- 229920000642 polymer Polymers 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 18
- 239000004642 Polyimide Substances 0.000 claims abstract description 13
- 229920001721 polyimide Polymers 0.000 claims abstract description 13
- 229920000131 polyvinylidene Polymers 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims description 20
- 238000000576 coating method Methods 0.000 claims description 20
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 8
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 6
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 4
- 230000000171 quenching effect Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002356 single layer Substances 0.000 abstract description 9
- 230000004888 barrier function Effects 0.000 abstract description 2
- 238000013508 migration Methods 0.000 abstract description 2
- 230000005012 migration Effects 0.000 abstract description 2
- 229920006254 polymer film Polymers 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 50
- 238000004146 energy storage Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000007888 film coating Substances 0.000 description 3
- 238000009501 film coating Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000009194 climbing Effects 0.000 description 1
- 229920000891 common polymer Polymers 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 description 1
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1046—Polyimides containing oxygen in the form of ether bonds in the main chain
- C08G73/105—Polyimides containing oxygen in the form of ether bonds in the main chain with oxygen only in the diamino moiety
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
- C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/14—Organic dielectrics
- H01G4/18—Organic dielectrics of synthetic material, e.g. derivatives of cellulose
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/33—Thin- or thick-film capacitors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/16—Homopolymers or copolymers of vinylidene fluoride
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- Manufacturing & Machinery (AREA)
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Abstract
The invention belongs to the field of polymer films, and particularly relates to a polymer capacitor film with high breakdown field strength and a preparation method thereof. The polymer capacitor film with high breakdown field strength comprises a polyimide PI film and a polyvinylidene fluoride-trifluoroethylene-chlorodifluoroethylene PVTC film. The invention provides a polymer capacitor composite film with high breakdown field strength and a preparation method thereof. The result shows that the breakdown field intensity of the composite film is greatly improved relative to the field intensity of a single-layer film. Due to the existence of the interface barrier function, the charge migration and the growth of the electrical tree are prevented, and the breakdown field intensity of the composite film is larger than that of the single-layer film PI and P (VDF-TrFE-CFE). When the PI content is 83%, the breakdown field strength of the composite film is maximum and is 26% higher than that of the PI film with the same thickness.
Description
Technical Field
The invention belongs to the field of polymer films, and particularly relates to a polymer capacitor film with high breakdown field strength and a preparation method thereof.
Background
The thin film capacitor sometimes operates in an overvoltage, overcurrent, high temperature environment, and thus the breakdown field strength of the capacitor dielectric is highly required. Polyimide PI as a common polymer capacitor energy storage material has excellent insulating property (low dielectric constant and high breakdown field strength) and mechanical property, and the properties can still be kept at relatively high levels in wide temperature and frequency change processes, so the polyimide PI is the most concerned insulating material in the insulation field at present. When the polyimide is used as the energy storage medium of the capacitor, the breakdown field intensity of the polyimide is improved, so that the integral working voltage of the capacitor is improved. Polyvinylidene fluoride-trifluoroethylene-chlorodifluoroethylene P (VDF-TrFE-CFE) is also a common energy storage material, has excellent physical properties, better weather resistance, high temperature resistance, chemical corrosion resistance, ray radiation resistance, oxidation resistance, special properties such as thermoelectricity, dielectricity and piezoelectricity, is a key research object in the field of thin film capacitors, but is limited by lower breakdown field strength, so that the energy storage density is not high.
Disclosure of Invention
The invention aims to provide a polymer capacitor film with high breakdown field strength and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a polymer capacitor film with high breakdown field strength comprises a polyimide PI film and a polyvinylidene fluoride-trifluoroethylene-chlorodifluoroethylene PVTC film.
The thickness of the polyimide PI film is 2.5-15 mu m.
The volume ratio of the PI film to the PVTC film is 17-83: 83-17.
The volume ratio of the PI film to the PVTC film is 83: 17.
The polyimide PI film is prepared by adopting the following method: the following components in parts by weight: 5 parts of 4, 4' -diaminodiphenyl ether ODA, 5.5 parts of pyromellitic dianhydride and 100 parts of N, N-dimethylacetamide are uniformly mixed to form PAA coating solution, the PAA coating solution is coated by a coating machine at room temperature, and the PAA coating solution is put into a vacuum drying oven for imidization and then quenched to obtain the PI film. (4, 4' -diaminodiphenyl ether ODA, pyromellitic anhydride, N-dimethylacetamide available from national drug group chemical Co., Ltd.)
The temperature of imidization treatment is 80-350 ℃.
The invention also comprises a preparation method of the polymer capacitor film with high breakdown field strength, which is characterized by comprising the following steps: dissolving 10 parts by weight of polyvinylidene fluoride-trifluoroethylene-chlorodifluoroethylene into 100 parts by weight of N, N-dimethylformyl, uniformly mixing to form PVTC coating liquid, coating the PVTC coating liquid on the prepared PI film by using a coating machine, putting the PI film into a vacuum drying oven for heat treatment, and then putting the PI film into ice water for quenching to obtain the composite film containing the polyimide PI film and the polyvinylidene fluoride-trifluoroethylene-chlorodifluoroethylene PVTC film. The vacuum oven was set at 50 ℃ for 10h, after which the temperature was raised to 205 ℃ for 5 min. (vinylidene fluoride-trifluoroethylene-chlorodifluoroethylene PVTC from DuPont, USA)
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a polymer capacitor composite film with high breakdown field strength and a preparation method thereof. The result shows that the breakdown field intensity of the composite film is greatly improved relative to the field intensity of a single-layer film. Due to the existence of the interface barrier function, the charge migration and the growth of the electrical tree are prevented, and the breakdown field intensity of the composite film is larger than that of the single-layer film PI and P (VDF-TrFE-CFE). When the PI content is 83%, the breakdown field strength of the composite film is maximum and is 26% higher than that of the PI film with the same thickness.
Drawings
FIG. 1 is a Weibull plot of single and composite films at room temperature.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and preferred embodiments.
The preparation method of the polymer capacitor film with high breakdown field strength comprises the following steps:
1) weighing 4, 4' -diaminodiphenyl ether (ODA), pyromellitic dianhydride (PMDA) and N, N-dimethylacetamide (DMAc) in a mass ratio of 5:5.5: 100. The dried three-hole flask was mounted on an electric stirrer stand. DMAc was added first, followed by ODA and the electric stirrer was turned on. After stirring uniformly and the ODA was completely dissolved, 1/2 PMDA was added first, half of the remaining PMDA was added after one hour, and this was repeated, PMDA was added in portions, and PMDA was added little by little when a large amount of bubbles appeared in the solution. And when the obvious pole climbing phenomenon occurs, stopping adding the PMDA to obtain the coating solution. And then putting the PAA solution into a vacuum drying oven for vacuum bubble removal treatment. And opening the film coating machine, regulating the thickness by a scraper, and coating the film with the thickness of 2.5, 5, 7.5, 10, 12.5 and 15 mu m on clean quenching glass by using the film coating machine. Putting the film into an air-blast drying oven for periodic temperature rise to realize imidization, wherein the temperature and the time are controlled as follows: 80 deg.C (1h), 160 deg.C (0.5h), 200 deg.C (0.5h), 240 deg.C (0.5h), 280 deg.C (0.5h), 320 deg.C (0.5h), 350 deg.C (1 h). And finally, taking out the prepared PI film.
2) Pouring N, N-dimethylformamide weighed in advance into a beaker, weighing P (VDF-TrFE-CFE) and adding the P into the beaker in a mass ratio of 10: 1. . The beaker is placed on a magnetic stirrer and stirred for 12 hours to prepare a P (VDF-TrFE-CFE) solution, and the solution is placed in a vacuum drying oven to remove air bubbles for 1 hour. And (3) coating the PI film prepared in the step (1) with a film coating machine to obtain a P (VDF-TrFE-CFE) film with the thickness of 12.5, 10, 7.5, 5, 2..5 mu m to obtain a composite film, and coating a group of single-layer P (VDF-TrFE-CFE) films with the thickness of 15 mu m.
3) And (3) putting the composite film obtained in the step (2) into a vacuum drying oven for heat treatment, vacuumizing, setting the temperature to be 50 ℃, keeping the temperature for 5min, taking out the film, putting the film into ice water, and quenching to obtain 5 groups of composite films, 2 groups of single-layer medium PI films and PVTC films, wherein the thickness of the composite films is a certain value, and the volume fractions of the PI films are respectively 17%, 33%, 50%, 67% and 83%.
4) And taking 9-10 samples of each single layer or composite film, cutting the samples into 5 multiplied by 5cm, placing each sample in silicon oil during testing, and gradually pressurizing and testing the samples by using an operation box of a YDK test transformer until breakdown occurs. And recording the test data.
5) The measurement results are plotted as a Weibull distribution diagram, and FIG. 1 shows the Weibull distribution diagram of the breakdown voltages of the single-layer film and the composite film at room temperature. Table 1 is a Weibull parameter table for films;
TABLE 1
The corresponding breakdown voltage value is the breakdown field strength of the material when the probability is 63.28%, and it can be seen in fig. 1 that the breakdown voltage of the composite film is much higher than that of the single-layer film.
The above description is only a preferred embodiment of the present invention, and for those skilled in the art, the present invention should not be limited by the description of the present invention, which should be interpreted as a limitation.
Claims (8)
1. A polymer capacitor film with high breakdown field strength is characterized by comprising a polyimide PI film and a polyvinylidene fluoride-trifluoroethylene-chlorodifluoroethylene PVTC film.
2. The polymer capacitor film with high breakdown field strength of claim 1, wherein the polyimide PI film has a thickness of 2.5 to 15 μm.
3. The polymer capacitor film with high breakdown field strength of claim 1, wherein the volume ratio of the PI film to the PVTC film is 17-83: 83-17.
4. The polymer capacitor film with high breakdown field strength of claim 1, wherein the volume ratio of the PI film to the PVTC film is 83: 17.
5. The polymer capacitor film with high breakdown field strength of claim 1, wherein the polyimide PI film is prepared by: the following components in parts by weight: 5 parts of 4, 4' -diaminodiphenyl ether ODA, 5.5 parts of pyromellitic dianhydride and 100 parts of N, N-dimethylacetamide are uniformly mixed to form PAA coating solution, the PAA coating solution is coated by a coating machine at room temperature, and the PAA coating solution is put into a vacuum drying oven for imidization and then quenched to obtain the PI film.
6. The polymer capacitor film with high breakdown field strength according to claim 5, wherein the imidization treatment temperature is 80 to 350 ℃.
7. A method for producing a polymer capacitor film having a high breakdown field strength as claimed in any one of claims 1 to 6, comprising the steps of: dissolving 10 parts by weight of polyvinylidene fluoride-trifluoroethylene-chlorodifluoroethylene into 100 parts by weight of N, N-dimethylformyl, uniformly mixing to form PVTC coating liquid, coating the PVTC coating liquid on the prepared PI film by using a coating machine, putting the PI film into a vacuum drying oven for heat treatment, and then putting the PI film into ice water for quenching to obtain the composite film containing the polyimide PI film and the polyvinylidene fluoride-trifluoroethylene-chlorodifluoroethylene PVTC film.
8. The method for preparing a polymer capacitor film with high breakdown field strength as claimed in claim 7, wherein the temperature of the vacuum drying oven is set to 50 ℃ for 10h, and then the temperature is raised to 205 ℃ and kept for 5 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113077986A (en) * | 2021-04-14 | 2021-07-06 | 无锡中汇汽车电子科技有限公司 | Metallized modified polyamide film capacitor and preparation method thereof |
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| CN110070991A (en) * | 2018-09-25 | 2019-07-30 | 南方科技大学 | All-polymer layer composite material and its preparation method and application |
| CN110303734A (en) * | 2019-05-23 | 2019-10-08 | 深圳先进技术研究院 | Capacitor flexible material, preparation method and printed wiring board |
| CN110628218A (en) * | 2019-10-28 | 2019-12-31 | 山东巨野盛鑫电器材料有限公司 | Fluorine-containing polyimide/fluorinated ethylene propylene lubricating composite membrane and preparation method thereof |
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2020
- 2020-06-01 CN CN202010483503.4A patent/CN111875828A/en active Pending
Patent Citations (6)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113077986A (en) * | 2021-04-14 | 2021-07-06 | 无锡中汇汽车电子科技有限公司 | Metallized modified polyamide film capacitor and preparation method thereof |
| CN113077986B (en) * | 2021-04-14 | 2022-04-29 | 无锡中汇汽车电子科技有限公司 | Metallized modified polyamide film capacitor and preparation method thereof |
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