CN103756317B - A kind of compliant conductive Kapton - Google Patents

A kind of compliant conductive Kapton Download PDF

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Publication number
CN103756317B
CN103756317B CN201410033581.9A CN201410033581A CN103756317B CN 103756317 B CN103756317 B CN 103756317B CN 201410033581 A CN201410033581 A CN 201410033581A CN 103756317 B CN103756317 B CN 103756317B
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kapton
compliant conductive
nutgrass flatsedge
extract
carbon dust
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CN103756317A (en
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徐伟伟
杨楚罗
李秋影
刘战合
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JIANGSU YABAO INSULATION MATERIAL CO Ltd
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JIANGSU YABAO INSULATION MATERIAL CO Ltd
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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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • 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
    • 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
    • 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
    • C08K3/04—Carbon
    • 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
    • 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
    • C08K5/00—Use of organic ingredients
    • 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
    • C08K9/04—Ingredients treated with organic substances
    • 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
    • C08K9/10—Encapsulated ingredients
    • 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
    • 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
    • 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
    • C08K2003/0856—Iron
    • 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
    • C08K2003/0862—Nickel
    • 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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    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets

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Abstract

The invention discloses a kind of compliant conductive Kapton belonging to technical field of polymer materials and preparation method thereof. This film is made up of the material of following parts by weight: 30-80 part polyimides, nutgrass flatsedge extract 1-10 part, coupling agent 2-10 part, 5-20 part metal powder and 5-20 part carbon dust. Kapton of the present invention conducts electricity very well, and softness meets the requirement of various compliant conductive electronic devices and components, introduces nutgrass flatsedge extract, has further increased electric conductivity and the suppleness of Kapton.

Description

A kind of compliant conductive Kapton
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of compliant conductive Kapton andIts preparation method.
Background technology
Opto-electronic information technology is current very active research field in the world, has become current three large sectionsOne of skill focus. Machine thin film transistor (TFT) (OTFT), organic photovoltaic devices (OPV) and biology sensorEtc. (Biosensor) opto-electronic device requires thin film flexible conduction.
One of key technology of preparation flexible substrate nesa coating is the selection of flexible substrate material, flexible linerEnd conducting film has three basic requirements to flexible substrate material: the one, and the light transmission rate of backing material is high; TwoThat between backing material and conductive film, thermal coefficient of expansion will mate; The 3rd, flexible substrate and transparent conductive film toolThe adhesiveness having had. Polyimides (PI) is a kind of fabulous exotic material, it possess good mechanics,The performances such as dielectric, radiation hardness and resistance to solvent, therefore polyimides becomes the first-selection of preparation flexible substrate conducting filmBacking material.
Utilize ito glass as electrode, inorganic transition metal oxide (as, yttrium oxide, rhodium oxide and oxygenChange tungsten etc.) as the inorganic electrochromic film of electrochromism active layer assembling, part commercialization. ButBe the inorganic electrochromic film based on ito glass, its manufacturing cost is higher, frangible, can not be bending, andAnd some inorganic transition metal oxide also has nondegradable toxicity.
Adopt polyimides as conductive film material, its difficult point is, metal component be difficult to sputter or pointBe dispersed in polyimides macromolecular material, be difficult to form conductive structure.
Summary of the invention
Technical problem to be solved by this invention is the present situation for prior art, provides a kind of compliant conductive poly-Imide membrane and preparation method thereof.
A kind of compliant conductive Kapton, comprises the material of following parts by weight: 30-80 part polyamides AsiaAmine, 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, titanate esters or isopropyl triisostearoyltitanate.
The molecular formula of described polyimides is:
The extracting method of described nutgrass flatsedge extract is: nutgrass flatsedge is dried, pulverize, then use 80% ethanol waterHeating and refluxing extraction three times, merges No. three times extract, is evaporated to without alcohol taste, and concentrate is diluted with water intoSuspension, more respectively with benzinum, ethyl acetate extraction, makes.
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 ether and 5,6,7,8-dicyclo[2.2.2]-2-heptene tetracarboxylic dianhydride joins reactor, under nitrogen protection, adds metacresol, after stirring,Add isoquinolin, be warming up to 190 DEG C, react 12 hours, pour reactant liquor into ethanol after cooling to separate out, systemBecome polyimide resin;
(2) metal powder and carbon dust are placed in organic solvent, add coupling agent, through high shear dispersion machine in additionAfter high-temperature process, disperse in advance, treatment temperature is 200-800 DEG C;
(3) by synthetic polyimide resin and the metal powder of handling well, carbon dust stirs through stirred autoclave,Mixing speed 1000rpm, mixing time 1-2h, adds nutgrass flatsedge extract, and rotating speed is transferred to 2000rpm, continuesStir 1-2h, make 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 machineProcess, make finished product.
Described organic solvent is dimethylacetylamide, methyl-sulfoxide, DMA, N, N-bis-NMF, dimethyl sulfoxide (DMSO) or 1-METHYLPYRROLIDONE.
Beneficial effect of the present invention: Kapton of the present invention conducts electricity very well, softness, meets variousThe requirement of compliant conductive electronic devices and components, introduce nutgrass flatsedge extract, further increased KaptonElectric conductivity and suppleness.
Detailed description of the invention
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 ether (TFODA) with992.8g5,6,7,8-dicyclo [2.2.2]-2-heptene tetracarboxylic dianhydride (BCDA) joins reactor, and nitrogen is protectedProtect down and add 15000g metacresol, after stirring, add 500g isoquinolin, be warming up to 190 DEG C, reaction12 hours, to pour reactant liquor into ethanol after cooling and separate out, thing is polyimide resin;
40g copper powder and 50g carbon dust are placed in 1000g dimethylacetylamide, add 18g silane, through high shearDispersion machine disperses after high-temperature process in advance in addition, and treatment temperature is 200-800 DEG C;
By synthetic polyimide resin and the copper powder of handling well, carbon dust stirs through stirred autoclave, stirs speedDegree 1000rpm, mixing time 1-2h, adds 12g nutgrass flatsedge extract, and rotating speed is transferred to 2000rpm, continues to stirMix 1-2h, make 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, undertaken by winder and cutting machineProcessing, makes finished product.
Kapton thickness prepared by the present embodiment is 40-45um, sheet resistance 7-8 ohm-sq liRice, hot 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 ether (TFODA) with992.8g5,6,7,8-dicyclo [2.2.2]-2-heptene tetracarboxylic dianhydride (BCDA) joins reactor, and nitrogen is protectedProtect down and add 15000g metacresol, after stirring, add 500g isoquinolin, be warming up to 190 DEG C, reaction12 hours, to pour reactant liquor into ethanol after cooling and separate out, thing is polyimide resin;
50g nickel powder and 60g carbon dust are placed in 1500g methyl-sulfoxide, add 17g titanate esters, divide through high shearLoose machine disperses after high-temperature process in advance in addition, and treatment temperature is 200-800 DEG C;
By synthetic polyimide resin and the copper powder of handling well, carbon dust stirs through stirred autoclave, stirs speedDegree 1000rpm, mixing time 1-2h, adds 13g nutgrass flatsedge extract, and rotating speed is transferred to 2000rpm, continues to stirMix 1-2h, make 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, undertaken by winder and cutting machineProcessing, makes finished product.
Kapton thickness prepared by the present embodiment is 42-44um, sheet resistance 10-12 ohm-sq liRice, hot 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 ether (TFODA) with992.8g5,6,7,8-dicyclo [2.2.2]-2-heptene tetracarboxylic dianhydride (BCDA) joins reactor, and nitrogen is protectedProtect down and add 15000g metacresol, after stirring, add 500g isoquinolin, be warming up to 190 DEG C, reaction12 hours, to pour reactant liquor into ethanol after cooling and separate out, thing is polyimide resin;
55g silver-coated copper powder and 60g carbon dust are placed on to 1500gN, and N-dimethylacetylamide, adds 17g tri-different hardFatty acyl group isopropyl titanate disperses after high-temperature process in advance through high shear dispersion machine in addition, and treatment temperature is200-800℃；
By synthetic polyimide resin and the copper powder of handling well, carbon dust stirs through stirred autoclave, stirs speedDegree 1000rpm, mixing time 1-2h, adds 13g nutgrass flatsedge extract, and rotating speed is transferred to 2000rpm, continues to stirMix 1-2h, make 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 carries out imidization processing, process by winder and cutting machine,Make finished product.
Kapton thickness prepared by the present embodiment is 40-45um, sheet resistance 9-10 ohm-sq liRice, hot strength is 560Mpa.

Claims (5)

1. a compliant conductive Kapton, is characterized in that, comprises the material of following parts by weight:30-80 part polyimides, nutgrass flatsedge extract 1-10 part, coupling agent 2-10 part, 5-20 part metal powder and 5-20Part carbon dust;
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 ether and 5,6,7,8-dicyclo[2.2.2]-2-heptene tetracarboxylic dianhydride joins reactor, under nitrogen protection, adds metacresol, after stirring,Add isoquinolin, be warming up to 190 DEG C, react 12 hours, pour reactant liquor into ethanol after cooling to separate out, systemBecome polyimide resin;
(2) metal powder and carbon dust are placed in organic solvent, add coupling agent, through high shear dispersion machine in additionAfter high-temperature process, disperse in advance, treatment temperature is 200-800 DEG C;
(3) by synthetic polyimide resin and the metal powder of handling well, carbon dust stirs through stirred autoclave,Mixing speed 1000rpm, mixing time 1-2h, adds nutgrass flatsedge extract, and rotating speed is transferred to 2000rpm, continuesStir 1-2h, make 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 machineProcess, make finished product;
The extracting method of described nutgrass flatsedge extract is: nutgrass flatsedge is dried, pulverize, then use 80% ethanol waterHeating and refluxing extraction three times, merges No. three times extract, is evaporated to without alcohol taste, and concentrate is diluted with water intoSuspension, more respectively with benzinum, ethyl acetate extraction, makes;
Described organic solvent be DMA, DMF, dimethyl sulfoxide (DMSO) or1-METHYLPYRROLIDONE.
2. a kind of compliant conductive Kapton according to claim 1, is characterized in that described goldGenus 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 idolConnection agent is silane or titanate esters.
4. a kind of compliant conductive Kapton according to claim 1, is characterized in that, described poly-Imido molecular formula is:
5. a kind of compliant conductive Kapton according to claim 3, is characterized in that, described inTitanate esters is isopropyl triisostearoyltitanate.
CN201410033581.9A 2014-01-24 2014-01-24 A kind of compliant conductive Kapton Active CN103756317B (en)

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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
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
KR102036227B1 (en) * 2018-01-31 2019-10-24 에스케이씨 주식회사 Polyamide-imide film and preparation method thereof
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
CN111402706B (en) * 2020-04-29 2022-07-22 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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CN101699920B (en) * 2009-11-20 2012-08-08 宁波今山电子材料有限公司 Method for preparing polyimide heating film
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