CN103756317A - Flexible conductive polyimide film - Google Patents
Flexible conductive polyimide film Download PDFInfo
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- CN103756317A CN103756317A CN201410033581.9A CN201410033581A CN103756317A CN 103756317 A CN103756317 A CN 103756317A CN 201410033581 A CN201410033581 A CN 201410033581A CN 103756317 A CN103756317 A CN 103756317A
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- 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
- C08G73/12—Unsaturated polyimide precursors
- C08G73/124—Unsaturated polyimide precursors the unsaturated precursors containing oxygen in the form of ether bonds in the main chain
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K5/00—Use of organic ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/0856—Iron
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0862—Nickel
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2203/20—Applications use in electrical or conductive gadgets
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Abstract
The invention discloses a flexible conductive polyimide film and a preparation method thereof, and belongs to the technical field of high polymer materials. The film comprises the following substances in part by weight: 30-80 parts of polyimide, 1-10 parts of cyperus rotundus extractive, 2-10 parts of a coupling agent, 5-20 parts of metal powder and 5-20 parts of carbon powder. The flexible conductive polyimide film provided by the invention has the good conductive property; the flexible conductive polyimide film is soft, and the requirements of different conductive electron components are met; the cyperus rotundus extractive is imported, and the conductive property and the flexicity of the polyimide film are further increased.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of compliant conductive Kapton and preparation method thereof.
Background technology
Opto-electronic information technology is current very active research field in the world, has become one of current three large scientific and technological focuses.The opto-electronic devices such as machine thin film transistor (OTFT), organic photovoltaic devices (OPV) and biosensor (Biosensor) require thin film flexible conduction.
One of gordian technique of preparation flexible substrate nesa coating is the selection of flexible substrate material, and flexible substrate conducting film has three basic requirements to flexible substrate material: the one, and the light transmission rate of substrate material is high; The 2nd, between substrate material and conductive film, thermal expansivity will mate; The 3rd, the adhesivity that flexible substrate and transparent conductive film have had.Polyimide (PI) is a kind of fabulous high temperature material, and it possesses the performances such as good mechanics, dielectric, radiation hardness and resistance to solvent, and therefore polyimide becomes the first-selected substrate material of preparation flexible substrate conducting film.
Utilize ito glass as electrode, inorganic transition metal oxide (as, iridium oxide, rhodium oxide and Tungsten oxide 99.999 etc.) as the inorganic electrochromic film of electrochromism active coating assembling, part commercialization.But the inorganic electrochromic film based on ito glass, its manufacturing cost is higher, frangible, can not be bending, and also some inorganic transition metal oxide also has nondegradable toxicity.
Adopt polyimide as conductive film material, its difficult point is, metal component is difficult to sputter or is dispersed in polyimide macromolecular material, is difficult to form conductive structure.
Summary of the invention
Technical problem to be solved by this invention is the present situation for prior art, and a kind of compliant conductive Kapton and preparation method thereof is provided.
A kind of compliant conductive Kapton, comprises the material of following parts by weight: 30-80 part polyimide, nutgrass flatsedge extract 1-10 part, coupling agent 2-10 part, 5-20 part metal powder and 5-20 part carbon dust.
Described metal powder is copper, iron, nickel, silver-colored copper-clad, one or more in copper-clad nickel.
Described coupling agent is silane, titanic acid ester or isopropyl triisostearoyl titanate.
The molecular formula of described polyimide is:
The extracting method of described nutgrass flatsedge extract is: nutgrass flatsedge is dried, pulverize, then use 80% aqueous ethanolic solution heating and refluxing extraction three times, merge No. three times extracting solution, be evaporated to without alcohol taste, concentrated solution thin up becomes suspension, respectively with sherwood oil, ethyl acetate extraction, makes again.
The preparation method of above-mentioned compliant conductive Kapton, carries out in accordance with the following steps:
(1) at room temperature, by 2,2 '-bis trifluoromethyl-4,4'-diaminodiphenyl oxide and 5,6,7,8-dicyclo [2.2.2]-2-heptene tetracarboxylic dianhydride joins reactor, under nitrogen protection, add meta-cresol, after stirring, add isoquinoline 99.9, be warming up to 190 ℃, react 12 hours, pour reaction solution into ethanol after cooling to separate out, make polyimide resin;
(2) metal powder and carbon dust are placed in organic solvent, add coupling agent, through high-shear dispersion machine, after pyroprocessing, disperse in advance in addition, treatment temp is 200-800 ℃;
(3) by synthetic polyimide resin and the metal powder of handling well, carbon dust stirs through stirred autoclave, stirring velocity 1000rpm, and churning time 1-2h, adds nutgrass flatsedge extract, and rotating speed is transferred to 2000rpm, continues to stir 1-2h, makes film liquid;
(4) film hydraulic pressure is entered to deaeration still, under vacuum condition, slough the bubble in film liquid;
(5) the film liquid after deaeration is put into casting machine in addition curtain coating form the Kapton of even thickness;
(6) Kapton is put into imidization stove and carried out imidization processing, by winder and cutting machine, process, make finished product.
Described organic solvent is N,N-DIMETHYLACETAMIDE, methyl-sulphoxide, N,N-dimethylacetamide, DMF, dimethyl sulfoxide (DMSO) or N-Methyl pyrrolidone.
Beneficial effect of the present invention: Kapton of the present invention conducts electricity very well, softness, meets the requirement of various compliant conductive electronic devices and components, introduces nutgrass flatsedge extract, has further increased conductivity and the suppleness of Kapton.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1
Compliant conductive Kapton, its preparation method is as follows:
At room temperature, take 1345g2,2 '-bis trifluoromethyl-4,4'-diaminodiphenyl oxide (TFODA) and 992.8g5,6,7,8-dicyclo [2.2.2]-2-heptene tetracarboxylic dianhydride (BCDA) joins reactor, under nitrogen protection, add 15000g meta-cresol, after stirring, add 500g isoquinoline 99.9, be warming up to 190 ℃, react 12 hours, pour reaction solution into ethanol after cooling to separate out, thing is polyimide resin;
40g copper powder and 50g carbon dust are placed in 1000g N,N-DIMETHYLACETAMIDE, add 18g silane, through high-shear dispersion machine, after pyroprocessing, disperse in advance in addition, treatment temp is 200-800 ℃;
By synthetic polyimide resin and the copper powder of handling well, carbon dust stirs through stirred autoclave, stirring velocity 1000rpm, and churning time 1-2h, adds 12g nutgrass flatsedge extract, and rotating speed is transferred to 2000rpm, continues to stir 1-2h, makes film liquid;
Film hydraulic pressure is entered to deaeration still, under vacuum condition, slough the bubble in film liquid;
By the film liquid after deaeration put into casting machine in addition curtain coating form the Kapton of even thickness;
Kapton is put into imidization stove and carry out imidization processing, by winder and cutting machine, process, make finished product.
Kapton thickness prepared by the present embodiment is 40-45um, surface resistivity 7-8 ohm-sq centimetre, and tensile strength is 500Mpa.
Embodiment 2
Compliant conductive Kapton, its preparation method is as follows:
At room temperature, take 1345g2,2 '-bis trifluoromethyl-4,4 '-diaminodiphenyl oxide (TFODA) and 992.8g5,6,7,8-dicyclo [2.2.2]-2-heptene tetracarboxylic dianhydride (BCDA) joins reactor, under nitrogen protection, add 15000g meta-cresol, after stirring, add 500g isoquinoline 99.9, be warming up to 190 ℃, react 12 hours, pour reaction solution into ethanol after cooling to separate out, thing is polyimide resin;
50g nickel powder and 60g carbon dust are placed in 1500g methyl-sulphoxide, add 17g titanic acid ester, through high-shear dispersion machine, after pyroprocessing, disperse in advance in addition, treatment temp is 200-800 ℃;
By synthetic polyimide resin and the copper powder of handling well, carbon dust stirs through stirred autoclave, stirring velocity 1000rpm, and churning time 1-2h, adds 13g nutgrass flatsedge extract, and rotating speed is transferred to 2000rpm, continues to stir 1-2h, makes film liquid;
Film hydraulic pressure is entered to deaeration still, under vacuum condition, slough the bubble in film liquid;
By the film liquid after deaeration put into casting machine in addition curtain coating form the Kapton of even thickness;
Kapton is put into imidization stove and carry out imidization processing, by winder and cutting machine, process, make finished product.
Kapton thickness prepared by the present embodiment is 42-44um, surface resistivity 10-12 ohm-sq centimetre, and tensile strength is 550Mpa.
Embodiment 3
Compliant conductive Kapton, its preparation method is as follows:
At room temperature, take 1345g2,2 '-bis trifluoromethyl-4,4'-diaminodiphenyl oxide (TFODA) and 992.8g5,6,7,8-dicyclo [2.2.2]-2-heptene tetracarboxylic dianhydride (BCDA) joins reactor, under nitrogen protection, add 15000g meta-cresol, after stirring, add 500g isoquinoline 99.9, be warming up to 190 ℃, react 12 hours, pour reaction solution into ethanol after cooling to separate out, thing is polyimide resin;
55g silver-coated copper powder and 60g carbon dust are placed on to 1500g N,N-dimethylacetamide, add 17g isopropyl triisostearoyl titanate, through high-shear dispersion machine, after pyroprocessing, disperse in advance in addition, treatment temp is 200-800 ℃;
By synthetic polyimide resin and the copper powder of handling well, carbon dust stirs through stirred autoclave, stirring velocity 1000rpm, and churning time 1-2h, adds 13g nutgrass flatsedge extract, and rotating speed is transferred to 2000rpm, continues to stir 1-2h, makes film liquid;
Film hydraulic pressure is entered to deaeration still, under vacuum condition, slough the bubble in film liquid;
By the film liquid after deaeration put into casting machine in addition curtain coating form the Kapton of even thickness;
Kapton is put into imidization stove and carry out imidization processing, by winder and cutting machine, process, make finished product.
Kapton thickness prepared by the present embodiment is 40-45um, surface resistivity 9-10 ohm-sq centimetre, and tensile strength is 560Mpa.
Claims (7)
1. a compliant conductive Kapton, is characterized in that, comprises the material of following parts by weight: 30-80 part polyimide, nutgrass flatsedge extract 1-10 part, coupling agent 2-10 part, 5-20 part metal powder and 5-20 part carbon dust.
2. a kind of compliant conductive Kapton according to claim 1, is characterized in that, described metal powder is copper, iron, nickel, silver-colored copper-clad, one or more in copper-clad nickel.
3. a kind of compliant conductive Kapton according to claim 1, is characterized in that, described coupling agent is silane, titanic acid ester or isopropyl triisostearoyl titanate.
4. a kind of compliant conductive Kapton according to claim 1, is characterized in that, the molecular formula of described polyimide is:
5. a kind of compliant conductive Kapton according to claim 1, it is characterized in that, the extracting method of described nutgrass flatsedge extract is: nutgrass flatsedge is dried, pulverize, then use 80% aqueous ethanolic solution heating and refluxing extraction three times, merge No. three times extracting solution, be evaporated to without alcohol taste, concentrated solution thin up becomes suspension, more respectively with sherwood oil, ethyl acetate extraction, makes.
6. the preparation method of compliant conductive Kapton described in claim 1, is characterized in that, carries out in accordance with the following steps:
(1) at room temperature, by 2,2 '-bis trifluoromethyl-4,4'-diaminodiphenyl oxide and 5,6,7,8-dicyclo [2.2.2]-2-heptene tetracarboxylic dianhydride joins reactor, under nitrogen protection, add meta-cresol, after stirring, add isoquinoline 99.9, be warming up to 190 ℃, react 12 hours, pour reaction solution into ethanol after cooling to separate out, make polyimide resin;
(2) metal powder and carbon dust are placed in organic solvent, add coupling agent, through high-shear dispersion machine, after pyroprocessing, disperse in advance in addition, treatment temp is 200-800 ℃;
(3) by synthetic polyimide resin and the metal powder of handling well, carbon dust stirs through stirred autoclave, stirring velocity 1000rpm, and churning time 1-2h, adds nutgrass flatsedge extract, and rotating speed is transferred to 2000rpm, continues to stir 1-2h, makes film liquid;
(4) film hydraulic pressure is entered to deaeration still, under vacuum condition, slough the bubble in film liquid;
(5) the film liquid after deaeration is put into casting machine in addition curtain coating form the Kapton of even thickness;
(6) Kapton is put into imidization stove and carried out imidization processing, by winder and cutting machine, process, make finished product.
7. the preparation method of compliant conductive Kapton according to claim 6, it is characterized in that, described organic solvent is N,N-DIMETHYLACETAMIDE, methyl-sulphoxide, N, N-N,N-DIMETHYLACETAMIDE, DMF, dimethyl sulfoxide (DMSO) or N-Methyl pyrrolidone.
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| CN201410033581.9A CN103756317B (en) | 2014-01-24 | 2014-01-24 | A kind of compliant conductive Kapton |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104774461A (en) * | 2015-04-29 | 2015-07-15 | 江苏亚宝绝缘材料股份有限公司 | Polyimide film prepared through carbonyl dianhydride and diamine |
| CN104774460A (en) * | 2015-04-29 | 2015-07-15 | 江苏亚宝绝缘材料股份有限公司 | Thermoplastic polyimide film and preparation method thereof |
| CN111402706A (en) * | 2020-04-29 | 2020-07-10 | 广东聚航新材料研究院有限公司 | Film with rasterization encryption pattern on surface and preparation method thereof |
| JPWO2020138360A1 (en) * | 2018-12-28 | 2021-11-04 | 三菱瓦斯化学株式会社 | Imid-amidic acid copolymer and its production method, varnish, and polyimide film |
| US20220162388A1 (en) * | 2018-01-31 | 2022-05-26 | Skc Co., Ltd. | Polyamide-imide film and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104774461A (en) * | 2015-04-29 | 2015-07-15 | 江苏亚宝绝缘材料股份有限公司 | Polyimide film prepared through carbonyl dianhydride and diamine |
| CN104774460A (en) * | 2015-04-29 | 2015-07-15 | 江苏亚宝绝缘材料股份有限公司 | Thermoplastic polyimide film and preparation method thereof |
| US20220162388A1 (en) * | 2018-01-31 | 2022-05-26 | Skc Co., Ltd. | Polyamide-imide film and preparation method thereof |
| US11780965B2 (en) * | 2018-01-31 | 2023-10-10 | Sk Microworks Co., Ltd. | Polyamide-imide film and preparation method thereof |
| JPWO2020138360A1 (en) * | 2018-12-28 | 2021-11-04 | 三菱瓦斯化学株式会社 | Imid-amidic acid copolymer and its production method, varnish, and polyimide film |
| JP7392660B2 (en) | 2018-12-28 | 2023-12-06 | 三菱瓦斯化学株式会社 | Imide-amic acid copolymer and its manufacturing method, varnish, and polyimide film |
| CN111402706A (en) * | 2020-04-29 | 2020-07-10 | 广东聚航新材料研究院有限公司 | Film with rasterization encryption pattern on surface and preparation method thereof |
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| CN103756317B (en) | 2016-05-11 |
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