CN111081470B - Polyimide capacitor - Google Patents
Polyimide capacitor Download PDFInfo
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- CN111081470B CN111081470B CN201911313362.5A CN201911313362A CN111081470B CN 111081470 B CN111081470 B CN 111081470B CN 201911313362 A CN201911313362 A CN 201911313362A CN 111081470 B CN111081470 B CN 111081470B
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- polyimide
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- 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
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- 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
- H01G4/005—Electrodes
Abstract
The invention provides a polyimide capacitor, which comprises a capacitor shell and a battery cell arranged in the capacitor shell, wherein the battery cell comprises a substrate, an adhesion layer, a lower electrode barrier layer, a polyimide film layer, an upper electrode barrier layer and an upper electrode layer which are sequentially connected. The polyimide capacitor provided by the invention has the advantages of good heat resistance, excellent cycle performance, wide application temperature range and wide application range.
Description
Technical Field
The invention relates to the field of materials, in particular to a polyimide capacitor.
Background
Capacitors are basic components of electronic devices and are widely used in circuits such as bypass circuits, filtering circuits, sample-and-hold circuits, oscillation circuits, timing delays, coupling circuits, and blocking circuits. Meanwhile, the accuracy and reliability of the electronic device depend on the quality of the film capacitor to a large extent. The film capacitor widely used in the current electronic equipment is a ceramic chip capacitor, but the film capacitor has the defects of large temperature coefficient, high loss and the like; meanwhile, with the further development of industrial electronics and aerospace industries, higher requirements are put forward on the temperature coefficient, the environmental adaptability, the use temperature, the process cost and the like of the chip type thin film capacitor.
Polyimide is a polymer having an imide ring (-CO-NH-CO-) in the main chain, and among them, a polymer having a phthalimide structure is most important. Polyimide is one of organic polymer materials with the best comprehensive performance, has the advantages of high temperature resistance, low dielectric constant, corrosion resistance and the like, has the high temperature resistance of over 400 ℃, has the long-term use temperature range of-200-300 ℃, and has very high insulating property.
Polyimide (PI) has excellent heat resistance, good mechanical property, stable chemical property, excellent dielectric property, non-toxicity, irradiation resistance and other properties, and has relatively simple preparation process and excellent comprehensive performance, and is receiving more and more attention.
Modifying polyimide to obtain a capacitor with excellent performance is one of the hot spots of the current research.
Disclosure of Invention
The technical problem is as follows: in order to solve the defects of the prior art, the invention provides a polyimide capacitor.
The technical scheme is as follows: the invention provides a polyimide capacitor, which comprises a capacitor shell, an electric core arranged in the capacitor shell and electrolyte filled in the capacitor shell, wherein the electric core comprises a substrate, an adhesion layer, a lower electrode barrier layer, a polyimide film layer, an upper electrode barrier layer and an upper electrode layer which are sequentially connected.
As an improvement, the polyimide film comprises low dielectric polyimide, fluorine-containing siloxane and porous chitosan; wherein, the mass of the fluorine-containing siloxane is 1 to 2 percent of the mass of the low dielectric polyimide, and the mass of the porous chitosan is 0.5 to 1 percent of the mass of the low dielectric polyimide.
As an improvement, the structural formula of the low dielectric polyimide is shown as a formula V:
the preparation method of the low dielectric polyimide film comprises the following steps:
(1) adding fluorine-containing siloxane and chitosan into an organic solvent respectively to obtain a fluorine-containing siloxane solution and a chitosan solution;
(2) heating low dielectric polyimide to 50-60 ℃, and stirring at constant temperature; then dropwise adding the fluorine-containing siloxane solution while stirring; stirring and naturally cooling to 30-40 ℃, and dripping chitosan solution while cooling;
(3) preparing the product of the step (2) into a film, namely the low dielectric polyimide film
The preparation method of the low dielectric polyimide comprises the following steps:
(2.1) reacting the compound shown in the formula VI with the compound shown in the formula VII to obtain an intermediate shown in the formula VIII;
(2.2) carrying out an intermediate reaction shown as VIII to obtain a compound shown as a formula V;
the reaction formula is as follows:
the preparation method of the low dielectric polyimide comprises the following steps:
(2.1) under the protection of nitrogen and at a certain temperature, stirring the compound shown in the formula VI and the compound shown in the formula VII in an organic solvent for reaction to obtain an intermediate shown in the formula VIII;
and (2.2) adding a dehydrating agent and a catalyst, continuously stirring the intermediate shown as VIII at a certain temperature for reaction, cleaning, filtering and drying to obtain the compound shown as the formula V.
In the step (2.1), the organic solvent is one of N-methylpyrrolidone, N-dimethylacetamide and N, N-dimethylformamide; the reaction temperature is 5-25 ℃.
In the step (2.2), the dehydrating agent is one or a mixture of more of trifluoroacetic anhydride, acetic anhydride, thionyl chloride or an organic silicon compound; the molar ratio of the dehydrating agent to the compound VII is 3: 1-5: 1; the catalyst is one or a mixture of triethylamine and pyridine, and the molar ratio of the catalyst to the compound VII is 2: 1-4: 1; the reaction temperature is 40-60 ℃.
Preferably, the fluorine-containing siloxane is one or more of heptafluoropentyltriethoxysilane, heptafluoropentyltrimethoxysilane, heptafluoropentyltrichlorosilane, perfluorooctylethyltrichlorosilane, perfluorooctylethyltrimethoxysilane, perfluorooctylethyltriethoxysilane, tridecafluorooctyltrimethoxysilane.
Preferably, the substrate material is alumina ceramic.
Preferably, the adhesion layer, the lower electrode barrier layer and the upper electrode barrier layer are made of titanium-tungsten alloy.
Preferably, the material of the upper electrode layer and the lower electrode layer is a platinum electrode.
Has the advantages that: the polyimide capacitor provided by the invention has the advantages of good heat resistance, excellent cycle performance, wide application temperature range and wide application range.
Detailed Description
Example 1
The preparation method of the low dielectric polyimide comprises the following steps:
(1) under the protection of nitrogen and at a certain temperature, stirring the compound shown in the formula VI and the compound shown in the formula VII in an organic solvent for reaction to obtain an intermediate shown in the formula VIII; the organic solvent is N-methyl pyrrolidone; the reaction temperature is 15 ℃;
(2) adding a dehydrating agent and a catalyst, continuously stirring the intermediate shown in the formula VIII at a certain temperature for reaction, cleaning, filtering and drying to obtain a compound shown in the formula V; the dehydrating agent is trifluoroacetic anhydride; the molar ratio of the dehydrating agent to the compound VII is 4: 1; the catalyst is triethylamine, and the molar ratio of the catalyst to the compound VII is 3: 1; the reaction temperature was 50 ℃.
Example 2
The preparation method of the low dielectric polyimide comprises the following steps:
(1) under the protection of nitrogen and at a certain temperature, stirring the compound shown in the formula VI and the compound shown in the formula VII in an organic solvent for reaction to obtain an intermediate shown in the formula VIII; the organic solvent is N, N-dimethylacetamide; the reaction temperature is 5 ℃;
(2) adding a dehydrating agent and a catalyst, continuously stirring the intermediate shown in the formula VIII at a certain temperature for reaction, cleaning, filtering and drying to obtain a compound shown in the formula V; the dehydrating agent is acetic anhydride; the molar ratio of the dehydrating agent to the compound VII is 5: 1; the catalyst is pyridine, and the molar ratio of the catalyst to the compound VII is 4: 1; the reaction temperature was 40 ℃.
Example 3
The preparation method of the low dielectric polyimide comprises the following steps:
(1) under the protection of nitrogen and at a certain temperature, stirring the compound shown in the formula VI and the compound shown in the formula VII in an organic solvent for reaction to obtain an intermediate shown in the formula VIII; the organic solvent is N, N-dimethyl formyl; the reaction temperature is 25 ℃;
(2) adding a dehydrating agent and a catalyst, continuously stirring the intermediate shown in the formula VIII at a certain temperature for reaction, cleaning, filtering and drying to obtain a compound shown in the formula V; the dehydrating agent is thionyl chloride; the molar ratio of the dehydrating agent to the compound VII is 3: 1; the catalyst is triethylamine, and the molar ratio of the catalyst to the compound VII is 2: 1; the reaction temperature was 60 ℃.
Example 4
The preparation method of the low dielectric polyimide film comprises the following steps:
(1) adding fluorine-containing siloxane and chitosan into an organic solvent respectively to obtain a fluorine-containing siloxane solution and a chitosan solution;
(2) heating the low dielectric polyimide of example 1 to 55 ℃, and stirring at constant temperature; then dropwise adding the fluorine-containing siloxane solution while stirring; stirring and naturally cooling to 305 ℃, and dripping chitosan solution while cooling;
(3) and (3) preparing the product of the step (2) into a film, namely the low dielectric polyimide film.
The prepared low dielectric polyimide film comprises the low dielectric polyimide of the embodiment 1, fluorine-containing siloxane and porous chitosan; wherein, the mass of the fluorine-containing siloxane is 1.5 percent of the mass of the low dielectric polyimide, and the mass of the porous chitosan is 0.75 percent of the mass of the low dielectric polyimide.
The fluorine-containing siloxane is heptafluoropentyl triethoxysilane and heptafluoropentyl trimethoxysilane in a mass ratio of 1: 2.
Example 5
The preparation method of the low dielectric polyimide film comprises the following steps:
(1) adding fluorine-containing siloxane and chitosan into an organic solvent respectively to obtain a fluorine-containing siloxane solution and a chitosan solution;
(2) heating the low dielectric polyimide of example 2 to 50 ℃, and stirring at constant temperature; then dropwise adding the fluorine-containing siloxane solution while stirring; stirring and naturally cooling to 30 ℃, and dripping chitosan solution while cooling;
(3) and (3) preparing the product of the step (2) into a film, namely the low dielectric polyimide film.
The prepared low dielectric polyimide film comprises the low dielectric polyimide of the embodiment 2, fluorine-containing siloxane and porous chitosan; wherein, the mass of the fluorine-containing siloxane is 1 percent of the mass of the low dielectric polyimide, and the mass of the porous chitosan is 1 percent of the mass of the low dielectric polyimide.
The fluorine-containing siloxane is heptafluoropentyl trichlorosilane and perfluorooctyl ethyl trichlorosilane in a mass ratio of 1: 1.
Example 6
The preparation method of the low dielectric polyimide film comprises the following steps:
(1) adding fluorine-containing siloxane and chitosan into an organic solvent respectively to obtain a fluorine-containing siloxane solution and a chitosan solution;
(2) heating the low dielectric polyimide of example 3 to 60 ℃, and stirring at constant temperature; then dropwise adding the fluorine-containing siloxane solution while stirring; stirring and naturally cooling to 40 ℃, and dripping chitosan solution while cooling;
(3) and (3) preparing the product of the step (2) into a film, namely the low dielectric polyimide film.
The prepared low dielectric polyimide film comprises the low dielectric polyimide of the embodiment 3, fluorine-containing siloxane and porous chitosan; wherein, the mass of the fluorine-containing siloxane is 2 percent of the mass of the low dielectric polyimide, and the mass of the porous chitosan is 0.5 percent of the mass of the low dielectric polyimide.
The fluorine-containing siloxane is perfluorooctyl ethyl trimethoxy silane, perfluorooctyl ethyl triethoxy silane and tridecafluorooctyl triethoxy silane in a mass ratio of 1:2: 1.
Example 7
Polyimide capacitors were prepared from the low dielectric polyimide films of examples 4 to 6.
The polyimide capacitor comprises a capacitor shell, a battery cell arranged in the capacitor shell and electrolyte filled in the capacitor shell, wherein the battery cell comprises a substrate, an adhesion layer, a lower electrode barrier layer, a polyimide film layer, an upper electrode barrier layer and an upper electrode layer which are sequentially connected.
The substrate material is alumina ceramic.
The adhesion layer, the lower electrode barrier layer and the upper electrode barrier layer are made of titanium-tungsten alloy.
The material of the upper electrode layer and the lower electrode layer is a platinum electrode.
And (3) testing the performance of the prepared capacitor, wherein the test method comprises the following steps: charging to 2.7V at 60A, discharging to 0.1V at a constant current of 60A, circulating for 10 times, and testing the discharge capacity, specific energy and specific power after 10 times; the capacitor is placed in a high-temperature impact box, the temperature is raised to 185 ℃ at the speed of 5 ℃/min, the temperature is kept for 2 hours, the appearance change of the product is observed, and the discharge capacity change is measured; the charge and discharge cycles were 10000 times at 60A, and the change in discharge capacity was measured. The results are as follows:
Claims (5)
1. a polyimide capacitor, characterized by: the capacitor comprises a capacitor shell, a battery cell arranged in the capacitor shell and electrolyte filled in the capacitor shell, wherein the battery cell comprises a substrate, an adhesion layer, a lower electrode barrier layer, a polyimide film layer, an upper electrode barrier layer and an upper electrode layer which are sequentially connected; the polyimide film comprises low-dielectric polyimide, fluorine-containing siloxane and porous chitosan; wherein, the mass of the fluorine-containing siloxane is 1 to 2 percent of the mass of the low dielectric polyimide, and the mass of the porous chitosan is 0.5 to 1 percent of the mass of the low dielectric polyimide; the structural formula of the low dielectric polyimide is shown as the formula V:
2. the polyimide capacitor according to claim 1, wherein: the fluorine-containing siloxane is one or more of heptafluoropentyl triethoxysilane, heptafluoropentyl trimethoxysilane, heptafluoropentyl trichlorosilane, perfluorooctyl ethyl trimethoxysilane, perfluorooctyl ethyl triethoxysilane, tridecafluorooctyl trimethoxysilane and tridecafluorooctyl trichlorosilane.
3. The polyimide capacitor according to claim 1, wherein: the substrate material is alumina ceramic.
4. The polyimide capacitor according to claim 1, wherein: the adhesion layer, the lower electrode barrier layer and the upper electrode barrier layer are made of titanium-tungsten alloy.
5. The polyimide capacitor according to claim 1, wherein: the upper electrode layer and the lower electrode layer are made of platinum electrodes.
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CN104220487A (en) * | 2012-03-28 | 2014-12-17 | 巴斯夫欧洲公司 | Polyimides as dielectrics |
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US6974620B1 (en) * | 2000-02-28 | 2005-12-13 | Toray Industries, Inc. | Polyester film for heat-resistant capacitor, metallized film thereof, and heat-resistant film capacitor containing the same |
CN206584827U (en) * | 2017-02-24 | 2017-10-24 | 中国振华集团云科电子有限公司 | A kind of high-temperature high-frequency polyimides chip thin film capacitor |
CN109096758A (en) * | 2018-08-21 | 2018-12-28 | 无锡创彩光学材料有限公司 | A kind of low dielectric coefficient polyimide film and preparation method thereof |
CN109627764A (en) * | 2018-12-17 | 2019-04-16 | 无锡创彩光学材料有限公司 | Low dielectric Kapton of a kind of high bonding and preparation method thereof |
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