WO2021027246A1 - Conductive carbon black coating liquid and conductive thin film - Google Patents

Conductive carbon black coating liquid and conductive thin film Download PDF

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WO2021027246A1
WO2021027246A1 PCT/CN2020/070611 CN2020070611W WO2021027246A1 WO 2021027246 A1 WO2021027246 A1 WO 2021027246A1 CN 2020070611 W CN2020070611 W CN 2020070611W WO 2021027246 A1 WO2021027246 A1 WO 2021027246A1
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carbon black
conductive
parts
black coating
conductive carbon
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PCT/CN2020/070611
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朴相玟
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苏州高泰电子技术股份有限公司
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/24—Electrically-conducting paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00—Adhesives based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04—Homopolymers or copolymers of esters
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    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/28—Metal sheet
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    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/40—Adhesives in the form of films or foils characterised by release liners
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    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02—Electrically-conducting adhesives
    • 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
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
    • C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
    • C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/314—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive layer and/or the carrier being conductive

Definitions

  • the present invention relates to the field of conductive films, in particular to a conductive carbon black coating solution and a conductive film.
  • Conductive films are currently widely used in electrical appliances.
  • conductive films mostly contain polymer resins such as polyurethane, polyethylene or polyester resin.
  • T g glass transition temperature
  • the purpose of the present invention is to provide a conductive carbon black coating liquid and a conductive film.
  • the conductive film of the present invention has low resistance and high conductivity.
  • the first object of the present invention is to provide a conductive carbon black coating solution, based on its total weight, including the following components in mass fractions:
  • the balance is thermoplastic resin.
  • the mass fraction of carbon black in the conductive filler is 20-25 parts.
  • the particle size of carbon black is 20-100 nm.
  • the solvent in the acidic polyester polyamide solution is xylene or butyl acetate, and the pH of the acidic polyester polyamide solution is 5-6.5.
  • the molecular weight of polydimethylsiloxane is 3000-10000 g/mol.
  • the one-component blocked isocyanate is methyl ethyl ketoxime blocked hexamethyl diisocyanate.
  • the molecular weight of the melamine resin is 5000-10000 g/mol.
  • thermoplastic resin is a polyester resin.
  • the conductive carbon black coating solution includes 25 parts of conductive fillers, 1.5 parts of acidic polyester polyamide solution; N-2-(aminoethanesulfonic acid)-3-aminopropyl three 1.0 part of ethoxysilane; 0.5 part of polydimethylsiloxane; 2.0 parts of one-component blocked isocyanate; 1.5 parts of 2-phenylimidazole; 1.5 parts of melamine resin; 67 parts of thermoplastic resin.
  • the conductive filler also includes one or more of carbon nanotubes, silver powder, copper powder and nickel powder.
  • the viscosity of the conductive carbon black coating liquid is 15,000 cps to 16,000 cps.
  • the conductive carbon black coating liquid of the present invention includes a thermoplastic polymer having a low glass transition temperature and a carbon black having thermally variable characteristics.
  • a thermoplastic polymer with a low glass transition temperature reaches a temperature above the glass transition temperature, due to thermal expansion, it separates the conductive powder particles dispersed in the polymer from the distance between the particles to hinder the flow of electrons, and at the same time, the electrical resistance will slow down. The phenomenon of rising. Using this phenomenon, a conductive film with low power consumption is manufactured in a specific temperature range.
  • the second object of the present invention is to provide a conductive film, including a first release film layer, a conductive carbon black coating, an electrodeposited copper foil layer, a conductive adhesive layer and a second release film layer arranged in sequence;
  • the conductive carbon black coating is prepared from the above conductive carbon black coating liquid of the present invention.
  • first release film layer and the second release film layer are transparent, and the materials of the first release film layer and the second release film layer are independently selected from PET.
  • the conductive adhesive layer is composed of acrylic adhesive and nickel powder. Among them, acrylic adhesive accounts for 88-92% of the mass fraction of the conductive adhesive layer; nickel powder accounts for 8-12% of the mass fraction of the conductive adhesive layer.
  • the thickness of the first release film layer is 25-100 ⁇ m; the thickness of the conductive carbon black coating is 15-50 ⁇ m; the thickness of the electrodeposited copper foil layer is 9-50 ⁇ m; the conductive adhesive The thickness of the layer is 10-50 ⁇ m; the thickness of the second release film layer is 25-100 ⁇ m.
  • the present invention has at least the following advantages:
  • the conductive carbon black coating used in the present invention is prepared from a conductive carbon black coating solution, which has conductivity and thermal changeability, and can react at a low T g .
  • a conductive carbon black coating solution which has conductivity and thermal changeability, and can react at a low T g .
  • the conductive film of the present invention includes the above-mentioned conductive carbon black coating, which has thermal changeability, durability and low electrical resistance.
  • Figure 1 is a schematic cross-sectional structure diagram of a conductive film of the present invention
  • Figure 2 is the SEM characterization results of different conductive materials
  • first release film layer 2- conductive carbon black coating; 3- electrodeposited copper foil layer; 4- conductive adhesive layer; 5- second release film layer.
  • the preparation method of melamine resin is as follows:
  • the conductive carbon black coating liquid of the present invention has a viscosity of 16,000 cps, based on its total weight, and includes the following components in mass fractions:
  • the conductive filler contains 25% by mass of carbon black and 75% by mass of carbon nanotubes, and the average particle size of the carbon black is about 20 nm.
  • the conductive filler of the present invention is composed of carbon black and carbon nanotubes.
  • Figure 2 is the SEM characterization results of different conductive materials.
  • Figures 2a, b, and c are the morphology test results of carbon black, carbon nanotubes and graphite, respectively. The results show that, Because of its own structure, carbon black is not only difficult to achieve a low resistance value, but also the physical properties of the prepared coating liquid are poor, and peeling may occur. Therefore, in the present invention, multi-layer carbon nanotubes formed into a tube shape with flake graphite and have a network structure are mixed to ensure the structural stability of the conductive coating solution while achieving a low resistance value.
  • the conductive carbon black coating solution of the present invention has a viscosity of 15,000 cps, based on its total weight, and includes the following components in mass fractions:
  • the conductive filler contains 20% by mass of carbon black and 80% by mass of carbon nanotubes.
  • the average particle size of the carbon black is about 70 nm.
  • the conductive carbon black coating liquid of the present invention has a viscosity of 16,000 cps, based on its total weight, and includes the following components in mass fractions:
  • the conductive filler contains 22% by mass of carbon black and 78% by mass of carbon nanotubes.
  • the average particle size of the carbon black is about 100 nm.
  • the conductive coating solution of the present invention reacts at a low T g (35°C).
  • T g 35°C
  • the resistance of the conductive coating solution increases by more than 30% This indicates that the conductive coating liquid of the present invention can also suppress local heat generation under unstable voltage conditions, thereby avoiding fires.
  • This embodiment provides a conductive film, which includes a first release film layer 1, a conductive carbon black coating 2, an electrodeposited copper foil layer 3, a conductive adhesive layer 4, and a second release film layer 5 sequentially arranged ;
  • Conductive carbon black coating 2 is obtained by coating the conductive carbon black coating solution in Example 1 of the present invention.
  • the first release film layer 1 and the second release film layer 5 are transparent, and the material of the first release film layer 1 and the second release film layer 5 is preferably PET.
  • the first release film layer 1 can be colorless or blue.
  • the conductive adhesive layer is composed of acrylic adhesive and nickel powder. Among them, acrylic adhesive accounts for 88% of the mass fraction of the conductive adhesive layer; nickel powder accounts for 12% of the mass fraction of the conductive adhesive layer.
  • the thickness of the first release film layer 1 is 25 ⁇ m; the thickness of the conductive carbon black coating 2 is 15 ⁇ m; the thickness of the electrodeposited copper foil 3 layer is 9 ⁇ m; the thickness of the conductive adhesive layer 4 is 10 ⁇ m The thickness of the second release film layer 5 is 25 ⁇ m.
  • This embodiment provides a conductive film, which includes a first release film layer 1, a conductive carbon black coating 2, an electrodeposited copper foil layer 3, a conductive adhesive layer 4, and a second release film layer 5 sequentially arranged ;
  • Conductive carbon black coating 2 is obtained by coating the conductive carbon black coating solution in Example 1 of the present invention.
  • the first release film layer 1 and the second release film layer 5 are transparent, and the material of the first release film layer 1 and the second release film layer 5 is preferably PET.
  • the first release film layer 1 can be colorless or blue.
  • the conductive adhesive layer is composed of acrylic adhesive and nickel powder. Among them, acrylic adhesive accounts for 90% of the mass fraction of the conductive adhesive layer; nickel powder accounts for 10% of the mass fraction of the conductive adhesive layer.
  • the thickness of the first release film layer 1 is 60 ⁇ m; the thickness of the conductive carbon black coating 2 is 30 ⁇ m; the thickness of the electrodeposited copper foil 3 layer is 30 ⁇ m; the thickness of the conductive adhesive layer 4 is 35 ⁇ m The thickness of the second release film layer 5 is 55 ⁇ m.
  • This embodiment provides a conductive film, which includes a first release film layer 1, a conductive carbon black coating 2, an electrodeposited copper foil layer 3, a conductive adhesive layer 4, and a second release film layer 5 sequentially arranged ;
  • Conductive carbon black coating 2 is obtained by coating the conductive carbon black coating solution in Example 1 of the present invention.
  • the first release film layer 1 and the second release film layer 5 are transparent, and the material of the first release film layer 1 and the second release film layer 5 is preferably PET.
  • the first release film layer 1 can be colorless or blue.
  • the conductive adhesive layer is composed of acrylic adhesive and nickel powder. Among them, acrylic adhesive accounts for 92% of the mass fraction of the conductive adhesive layer; nickel powder accounts for 8% of the mass fraction of the conductive adhesive layer.
  • the thickness of the first release film layer 1 is 100 ⁇ m; the thickness of the conductive carbon black coating 2 is 50 ⁇ m; the thickness of the electrodeposited copper foil 3 layer is 50 ⁇ m; the thickness of the conductive adhesive layer 4 is 50 ⁇ m The thickness of the second release film layer 5 is 100 ⁇ m.

Abstract

A conductive carbon black coating liquid, comprising the following components in parts by mass based on total weight: 23-25 parts of a conductive filler containing carbon black; 1-1.5 parts of an acid polyester polyamide solution; 0.8-1.0 part of N-2-(taurine)-3-aminopropyltriethoxysilane; 0.5 part of dimethylsiloxane; 1.8-2.0 parts of a liquid-type blocked isocyanate; 1.3-1.5 parts of 2-phenylimidazole; 1.5 parts of a melamine resin; and the balance of a thermoplastic resin. A conductive thin film comprises a first release layer (1), a conductive carbon black coating (2), an electrodeposition copper foil layer (3), a conductive adhesive layer (4), and a second release layer (5) which are successively arranged, and the conductive carbon black coating (2) is made from the conductive carbon black coating liquid.

Description

导电炭黑涂布液及导电薄膜Conductive carbon black coating liquid and conductive film 技术领域Technical field
本发明涉及导电薄膜领域，尤其涉及一种导电炭黑涂布液及导电薄膜。The present invention relates to the field of conductive films, in particular to a conductive carbon black coating solution and a conductive film.
背景技术Background technique
导电薄膜目前被广泛应用于电器领域，如导电薄膜大多含聚氨酯、聚乙烯或者聚酯树脂等高分子树脂，目前需要发展更多的在低的玻璃化转变温度(T g)下反应的导电薄膜，使其在电压不稳的条件下，也能抑制局部的发热，避免火灾的发生。 Conductive films are currently widely used in electrical appliances. For example, conductive films mostly contain polymer resins such as polyurethane, polyethylene or polyester resin. At present, it is necessary to develop more conductive films that react at a low glass transition temperature (T g ) , So that it can suppress local heating and avoid fire under the condition of unstable voltage.
发明内容Summary of the invention
为解决上述技术问题，本发明的目的是提供一种导电炭黑涂布液及导电薄膜，本发明的导电薄膜电阻低，具有高导电性。In order to solve the above technical problems, the purpose of the present invention is to provide a conductive carbon black coating liquid and a conductive film. The conductive film of the present invention has low resistance and high conductivity.
本发明的第一个目的是提供一种导电炭黑涂布液，以其总重为基准，包括以下质量分数的各组分：The first object of the present invention is to provide a conductive carbon black coating solution, based on its total weight, including the following components in mass fractions:
导电填料23-25份，所述导电填料中含有炭黑；23-25 parts of conductive filler, said conductive filler containing carbon black;
酸性聚酯聚酰胺溶液1-1.5份；1-1.5 parts of acidic polyester polyamide solution;
N-2-(氨基乙磺酸)-3-氨丙基三乙氧基硅烷0.8-1.0份；其结构式如下：0.8-1.0 parts of N-2-(aminoethanesulfonic acid)-3-aminopropyltriethoxysilane; its structural formula is as follows:
Figure PCTCN2020070611-appb-000001
Figure PCTCN2020070611-appb-000001
聚二甲基硅氧烷0.5份；0.5 part of polydimethylsiloxane;
一液型封端异氰酸酯1.8-2.0份；1.8-2.0 parts of one-component blocked isocyanate;
2-苯基咪唑1.3-1.5份；1.3-1.5 parts of 2-phenylimidazole;
密氨树脂1.5份；所述密氨树脂的结构式如下：1.5 parts of melamine resin; the structural formula of the melamine resin is as follows:
Figure PCTCN2020070611-appb-000002
Figure PCTCN2020070611-appb-000002
余量为热塑性树脂。The balance is thermoplastic resin.
进一步地，以导电填料的总重为基准，导电填料中炭黑的质量分数为20-25份。Further, based on the total weight of the conductive filler, the mass fraction of carbon black in the conductive filler is 20-25 parts.
进一步地，炭黑的粒径为20-100nm。Further, the particle size of carbon black is 20-100 nm.
进一步地，酸性聚酯聚酰胺溶液中的溶剂为二甲苯或乙酸丁酯，所述酸性聚酯聚酰胺溶液的pH值为5-6.5。Further, the solvent in the acidic polyester polyamide solution is xylene or butyl acetate, and the pH of the acidic polyester polyamide solution is 5-6.5.
进一步地，聚二甲基硅氧烷的分子量为3000-10000g/mol。Further, the molecular weight of polydimethylsiloxane is 3000-10000 g/mol.
进一步地，一液型封端异氰酸酯为甲乙酮肟封闭六甲基二异氰酸酯。Further, the one-component blocked isocyanate is methyl ethyl ketoxime blocked hexamethyl diisocyanate.
进一步地，密氨树脂的分子量为5000-10000g/mol。Further, the molecular weight of the melamine resin is 5000-10000 g/mol.
进一步地，热塑性树脂为涤纶树脂。Further, the thermoplastic resin is a polyester resin.
优选的，导电炭黑涂布液中，以其总重为基准，包括导电填料25份，酸性聚酯聚酰胺溶液1.5份；N-2-(氨基乙磺酸)-3-氨丙基三乙氧基硅烷1.0份；聚二甲基硅氧烷0.5份；一液型封端异氰酸酯2.0份；2-苯基咪唑1.5份；密氨树脂1.5份；热塑性树脂67份。Preferably, the conductive carbon black coating solution, based on its total weight, includes 25 parts of conductive fillers, 1.5 parts of acidic polyester polyamide solution; N-2-(aminoethanesulfonic acid)-3-aminopropyl three 1.0 part of ethoxysilane; 0.5 part of polydimethylsiloxane; 2.0 parts of one-component blocked isocyanate; 1.5 parts of 2-phenylimidazole; 1.5 parts of melamine resin; 67 parts of thermoplastic resin.
进一步地，导电填料还包括碳纳米管、银粉、铜粉和镍粉中的一种或几种。Further, the conductive filler also includes one or more of carbon nanotubes, silver powder, copper powder and nickel powder.
进一步地，导电炭黑涂布液的粘度为15,000cps-16,000cps。Further, the viscosity of the conductive carbon black coating liquid is 15,000 cps to 16,000 cps.
进一步地，密氨树脂的制备方法如下：Further, the preparation method of melamine resin is as follows:
将三聚氰胺与甲醛混合，二者摩尔比为1:3，在85℃及pH＝8的条件下反应。具体反应路线如下：Mix melamine and formaldehyde with a molar ratio of 1:3, and react at 85°C and pH=8. The specific reaction route is as follows:
在装有搅拌器、温度计、回流装置的反应釜中，加入甲醛水溶液(37％)和乌洛托品，搅拌溶解。在搅拌下加入三聚氰胺，慢慢升温至80℃，待完全溶解后，测试沉淀比，沉淀比达到2：2时，加入三乙醇胺调节PH值为8。In a reactor equipped with a stirrer, a thermometer and a reflux device, add the aqueous formaldehyde solution (37%) and urotropine and stir to dissolve. Add melamine under stirring and slowly raise the temperature to 80°C. After it is completely dissolved, test the precipitation ratio. When the precipitation ratio reaches 2:2, add triethanolamine to adjust the pH to 8.
本发明的导电炭黑涂布液包括具有低的玻璃化转变温度的热塑性聚合物以及有热可变特性的的炭黑。玻璃化转变温度低的热塑性聚合物达到玻璃化转变温度以上的温度时，因热膨胀性，其将分散在高分子内的导电粉粒子间距离隔开来妨碍电子流动的同时，会出现电阻缓缓上升的现象。利用此现象，在特定的温度领域制造低耗电量的导电薄膜。The conductive carbon black coating liquid of the present invention includes a thermoplastic polymer having a low glass transition temperature and a carbon black having thermally variable characteristics. When a thermoplastic polymer with a low glass transition temperature reaches a temperature above the glass transition temperature, due to thermal expansion, it separates the conductive powder particles dispersed in the polymer from the distance between the particles to hinder the flow of electrons, and at the same time, the electrical resistance will slow down. The phenomenon of rising. Using this phenomenon, a conductive film with low power consumption is manufactured in a specific temperature range.
本发明的第二个目的是提供一种导电薄膜，包括依次设置的第一离型膜层、导电炭黑涂层、电沉积铜箔层、导电胶黏剂层和第二离型膜层；所述导电炭黑涂层由本发明的上述导电炭黑涂布液制得。The second object of the present invention is to provide a conductive film, including a first release film layer, a conductive carbon black coating, an electrodeposited copper foil layer, a conductive adhesive layer and a second release film layer arranged in sequence; The conductive carbon black coating is prepared from the above conductive carbon black coating liquid of the present invention.
进一步地，第一离型膜层和第二离型膜层呈透明状，所述第一离型膜层和第二离型膜层的材质独立的选自PET。Further, the first release film layer and the second release film layer are transparent, and the materials of the first release film layer and the second release film layer are independently selected from PET.
进一步地，导电胶黏剂层的由丙烯酸胶粘剂和镍粉组成。其中，丙烯酸胶粘剂占导电胶黏剂层质量分数的88-92％；镍粉占导电胶黏剂层质量分数的8-12％。Further, the conductive adhesive layer is composed of acrylic adhesive and nickel powder. Among them, acrylic adhesive accounts for 88-92% of the mass fraction of the conductive adhesive layer; nickel powder accounts for 8-12% of the mass fraction of the conductive adhesive layer.
进一步地，第一离型膜层的厚度为25-100μm；所述导电炭黑涂层的厚度为15-50μm；所述电沉积铜箔层的厚度为9-50μm；所述导电胶黏剂层的厚度为10-50μm；所述第二离型膜层的厚度为25-100μm。Further, the thickness of the first release film layer is 25-100 μm; the thickness of the conductive carbon black coating is 15-50 μm; the thickness of the electrodeposited copper foil layer is 9-50 μm; the conductive adhesive The thickness of the layer is 10-50 μm; the thickness of the second release film layer is 25-100 μm.
借由上述方案，本发明至少具有以下优点：With the above solution, the present invention has at least the following advantages:
本发明作为的导电炭黑涂层由导电炭黑涂布液制得，该涂布液具有导电性及热可变型性，其可在低的T g下反应，外界温度变化时，其热膨胀性能导致其发生变形，即使在电压不稳条件下也能抑制局部的发热，从而避免火灾发生。 The conductive carbon black coating used in the present invention is prepared from a conductive carbon black coating solution, which has conductivity and thermal changeability, and can react at a low T g . When the external temperature changes, its thermal expansion performance As a result, it is deformed, and even under unstable voltage conditions, local heating can be suppressed, thereby avoiding fire.
本发明的导电薄膜包含上述导电炭黑涂层，其具有热可变型性，耐久性且电阻低。The conductive film of the present invention includes the above-mentioned conductive carbon black coating, which has thermal changeability, durability and low electrical resistance.
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，并可依照说明书的内容予以实施，以下以本发明的较佳实施例并配合附图详细说明如后。The above description is only an overview of the technical solution of the present invention. In order to understand the technical means of the present invention more clearly and implement it in accordance with the content of the description, the preferred embodiments of the present invention are described in detail below with the accompanying drawings.
附图说明Description of the drawings
图1是本发明导电薄膜的剖面结构示意图；Figure 1 is a schematic cross-sectional structure diagram of a conductive film of the present invention;
图2是不同导电材料的SEM表征结果；Figure 2 is the SEM characterization results of different conductive materials;
附图标记说明：Description of reference signs:
1-第一离型膜层；2-导电炭黑涂层；3-电沉积铜箔层；4-导电胶黏剂层；5-第二离型膜层。1- first release film layer; 2- conductive carbon black coating; 3- electrodeposited copper foil layer; 4- conductive adhesive layer; 5- second release film layer.
具体实施方式detailed description
下面结合附图和实施例，对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明，但不用来限制本发明的范围。The specific embodiments of the present invention will be described in further detail below in conjunction with the drawings and embodiments. The following examples are used to illustrate the present invention, but not to limit the scope of the present invention.
本发明以下实施例中，密氨树脂的制备方法如下：In the following embodiments of the present invention, the preparation method of melamine resin is as follows:
在装有搅拌器、温度计、回流装置的反应釜中，加入甲醛水溶液(37％)和乌洛托品，搅拌溶解。在搅拌下加入三聚氰胺，慢慢升温至80℃，待完全溶解后，测试沉淀比，沉淀比达到2：2时，加入三乙醇胺调节PH值为8。In a reactor equipped with a stirrer, a thermometer and a reflux device, add the aqueous formaldehyde solution (37%) and urotropine and stir to dissolve. Add melamine under stirring and slowly raise the temperature to 80°C. After it is completely dissolved, test the precipitation ratio. When the precipitation ratio reaches 2:2, add triethanolamine to adjust the pH to 8.
实施例1Example 1
本发明的一种导电炭黑涂布液，其粘度为16,000cps，以其总重为基准，包括以下质量分数的各组分：The conductive carbon black coating liquid of the present invention has a viscosity of 16,000 cps, based on its total weight, and includes the following components in mass fractions:
导电填料25份，导电填料中含有25％质量分数的炭黑以及75％质量分数的碳纳米管，炭黑的平均粒径为20nm左右。25 parts of conductive filler, the conductive filler contains 25% by mass of carbon black and 75% by mass of carbon nanotubes, and the average particle size of the carbon black is about 20 nm.
酸性聚酯聚酰胺溶液1.5份，其溶剂为二甲苯，酸性聚酯聚酰胺溶液的pH值为5。1.5 parts of the acidic polyester polyamide solution, the solvent of which is xylene, and the pH value of the acidic polyester polyamide solution is 5.
N-2-(氨基乙磺酸)-3-氨丙基三乙氧基硅烷1.0份；1.0 part of N-2-(aminoethanesulfonic acid)-3-aminopropyltriethoxysilane;
聚二甲基硅氧烷(分子量3000g/mol)0.5份；0.5 part of polydimethylsiloxane (molecular weight 3000g/mol);
甲乙酮肟封闭六甲基二异氰酸酯2.0份；2.0 parts of methyl ethyl ketoxime blocked hexamethyl diisocyanate;
2-苯基咪唑1.5份；1.5 parts of 2-phenylimidazole;
密氨树脂(分子量5000g/mol)1.5份；1.5 parts of melamine resin (molecular weight 5000g/mol);
涤纶树脂67份。67 parts of polyester resin.
本发明的导电填料由炭黑以及碳纳米管组成，图2是不同导电材料的SEM表征结果，图2a、b、c分别为炭黑、碳纳米管和石墨的形貌测试结果，结果表明，炭黑因为其自身构造，不仅难以实现低的电阻值，而且所制成的涂布液的物性差，会出现剥离的现象。故，本发明中混合了与片状石墨形成管状并具有网状构造的多层碳纳米管，来确保导电涂布液的构造上的稳定性，同时实现了低的电阻值。The conductive filler of the present invention is composed of carbon black and carbon nanotubes. Figure 2 is the SEM characterization results of different conductive materials. Figures 2a, b, and c are the morphology test results of carbon black, carbon nanotubes and graphite, respectively. The results show that, Because of its own structure, carbon black is not only difficult to achieve a low resistance value, but also the physical properties of the prepared coating liquid are poor, and peeling may occur. Therefore, in the present invention, multi-layer carbon nanotubes formed into a tube shape with flake graphite and have a network structure are mixed to ensure the structural stability of the conductive coating solution while achieving a low resistance value.
实施例2Example 2
本发明的一种导电炭黑涂布液，其粘度为15,000cps，以其总重为基准，包括以下质量分数的各组分：The conductive carbon black coating solution of the present invention has a viscosity of 15,000 cps, based on its total weight, and includes the following components in mass fractions:
导电填料23份，导电填料中含有20％质量分数的炭黑以及80％质量分数的碳纳米管，炭黑的平均粒径为70nm左右。There are 23 parts of conductive filler. The conductive filler contains 20% by mass of carbon black and 80% by mass of carbon nanotubes. The average particle size of the carbon black is about 70 nm.
酸性聚酯聚酰胺溶液1.5份，其溶剂为二甲苯，酸性聚酯聚酰胺溶液的pH值为6.0。1.5 parts of the acidic polyester polyamide solution, the solvent of which is xylene, and the pH of the acidic polyester polyamide solution is 6.0.
N-2-(氨基乙磺酸)-3-氨丙基三乙氧基硅烷0.8份；0.8 parts of N-2-(aminoethanesulfonic acid)-3-aminopropyltriethoxysilane;
聚二甲基硅氧烷(分子量10000g/mol)0.5份；0.5 part of polydimethylsiloxane (molecular weight 10000g/mol);
甲乙酮肟封闭六甲基二异氰酸酯1.8份；1.8 parts of methyl ethyl ketoxime blocked hexamethyl diisocyanate;
2-苯基咪唑1.3份；1.3 parts of 2-phenylimidazole;
密氨树脂(分子量10000g/mol)1.5份；1.5 parts of melamine resin (molecular weight 10000g/mol);
涤纶树脂69.6份。69.6 parts of polyester resin.
实施例3Example 3
本发明的一种导电炭黑涂布液，其粘度为16,000cps，以其总重为基准，包括以下质量分数的各组分：The conductive carbon black coating liquid of the present invention has a viscosity of 16,000 cps, based on its total weight, and includes the following components in mass fractions:
导电填料24份，导电填料中含有22％质量分数的炭黑以及78％质量分数的碳纳米管，炭黑的平均粒径为100nm左右。There are 24 parts of conductive filler. The conductive filler contains 22% by mass of carbon black and 78% by mass of carbon nanotubes. The average particle size of the carbon black is about 100 nm.
酸性聚酯聚酰胺溶液1.2份，其溶剂为乙酸丁酯，酸性聚酯聚酰胺溶液的pH值为6.5。1.2 parts of the acid polyester polyamide solution, the solvent of which is butyl acetate, and the pH value of the acid polyester polyamide solution is 6.5.
N-2-(氨基乙磺酸)-3-氨丙基三乙氧基硅烷0.9份；0.9 parts of N-2-(aminoethanesulfonic acid)-3-aminopropyltriethoxysilane;
聚二甲基硅氧烷(分子量6000g/mol)0.5份；0.5 part of polydimethylsiloxane (molecular weight 6000g/mol);
甲乙酮肟封闭六甲基二异氰酸酯1.9份；1.9 parts of methyl ethyl ketoxime blocked hexamethyl diisocyanate;
2-苯基咪唑1.4份；1.4 parts of 2-phenylimidazole;
密氨树脂(分子量8000g/mol)1.5份；1.5 parts of melamine resin (molecular weight 8000g/mol);
涤纶树脂68.6份。68.6 parts of polyester resin.
本发明的导电涂布液在低的T g下(35℃)反应，在电阻上升比率测试过程中，当从常温(10℃)上升到80℃时，导电涂布液的电阻上升30％以上，表明本发明的导电涂布液在电压不稳条件下也能抑制局部的发热，从而避免火灾的发生。 The conductive coating solution of the present invention reacts at a low T g (35°C). During the resistance increase ratio test, when the temperature rises from normal temperature (10°C) to 80°C, the resistance of the conductive coating solution increases by more than 30% This indicates that the conductive coating liquid of the present invention can also suppress local heat generation under unstable voltage conditions, thereby avoiding fires.
实施例4Example 4
本实施例提供了一种导电薄膜，包括依次设置的第一离型膜层1、导电炭黑涂层2、电沉积铜箔层3、导电胶黏剂层4和第二离型膜层5；导电炭黑涂层2由本发明的实施例1中的导电炭黑涂布液涂布后得到。第一离型膜层1和第二离型膜层5呈透明状，所述第一离型膜层1和第二离型膜层5的材质优选为PET。第一离型膜层1可为无色或蓝色。导电胶黏剂层由丙烯酸胶粘剂和镍粉组成。其中，丙烯酸胶粘剂占导电胶黏剂层质量分数的88％；镍粉占占导电胶黏剂层质量分数12％。This embodiment provides a conductive film, which includes a first release film layer 1, a conductive carbon black coating 2, an electrodeposited copper foil layer 3, a conductive adhesive layer 4, and a second release film layer 5 sequentially arranged ; Conductive carbon black coating 2 is obtained by coating the conductive carbon black coating solution in Example 1 of the present invention. The first release film layer 1 and the second release film layer 5 are transparent, and the material of the first release film layer 1 and the second release film layer 5 is preferably PET. The first release film layer 1 can be colorless or blue. The conductive adhesive layer is composed of acrylic adhesive and nickel powder. Among them, acrylic adhesive accounts for 88% of the mass fraction of the conductive adhesive layer; nickel powder accounts for 12% of the mass fraction of the conductive adhesive layer.
第一离型膜层1的厚度为25μm；所述导电炭黑涂层2的厚度为15μm；所述电沉积铜箔3层的厚度为9μm；所述导电胶黏剂层4的厚度为10μm；所述第二离型膜层5的厚度为25μm。The thickness of the first release film layer 1 is 25 μm; the thickness of the conductive carbon black coating 2 is 15 μm; the thickness of the electrodeposited copper foil 3 layer is 9 μm; the thickness of the conductive adhesive layer 4 is 10 μm The thickness of the second release film layer 5 is 25 μm.
实施例5Example 5
本实施例提供了一种导电薄膜，包括依次设置的第一离型膜层1、导电炭黑涂层2、电沉积铜箔层3、导电胶黏剂层4和第二离型膜层5；导电炭黑涂层2由本发明的实施例1中的导电炭黑涂布液涂布后得到。第一离型膜层1和第二离型膜层5呈透明状，所述第一离型膜层1和第二离型膜层5的材质优选为PET。第一离型膜层1可为无色或蓝色。导电胶黏剂层由丙烯酸胶粘剂和镍粉组成。其中，丙烯酸胶粘剂占导电胶黏剂层质量分数的90％；镍粉占占导电胶黏剂层质量分数的10％。第一离型膜层1的厚度为60μm；所述导电炭黑涂层2的厚度为30μm；所述电沉积铜箔3层的厚度为30μm；所述导电胶黏剂层4的厚度为35μm；所述第二离型膜层5的厚度为55μm。This embodiment provides a conductive film, which includes a first release film layer 1, a conductive carbon black coating 2, an electrodeposited copper foil layer 3, a conductive adhesive layer 4, and a second release film layer 5 sequentially arranged ; Conductive carbon black coating 2 is obtained by coating the conductive carbon black coating solution in Example 1 of the present invention. The first release film layer 1 and the second release film layer 5 are transparent, and the material of the first release film layer 1 and the second release film layer 5 is preferably PET. The first release film layer 1 can be colorless or blue. The conductive adhesive layer is composed of acrylic adhesive and nickel powder. Among them, acrylic adhesive accounts for 90% of the mass fraction of the conductive adhesive layer; nickel powder accounts for 10% of the mass fraction of the conductive adhesive layer. The thickness of the first release film layer 1 is 60 μm; the thickness of the conductive carbon black coating 2 is 30 μm; the thickness of the electrodeposited copper foil 3 layer is 30 μm; the thickness of the conductive adhesive layer 4 is 35 μm The thickness of the second release film layer 5 is 55 μm.
实施例6Example 6
本实施例提供了一种导电薄膜，包括依次设置的第一离型膜层1、导电炭黑涂层2、电沉积铜箔层3、导电胶黏剂层4和第二离型膜层5；导电炭黑涂层2由本发明的实施例1中的导 电炭黑涂布液涂布后得到。第一离型膜层1和第二离型膜层5呈透明状，所述第一离型膜层1和第二离型膜层5的材质优选为PET。第一离型膜层1可为无色或蓝色。导电胶黏剂层由丙烯酸胶粘剂和镍粉组成。其中，丙烯酸胶粘剂占导电胶黏剂层质量分数的92％；镍粉占占导电胶黏剂层质量分数的8％。This embodiment provides a conductive film, which includes a first release film layer 1, a conductive carbon black coating 2, an electrodeposited copper foil layer 3, a conductive adhesive layer 4, and a second release film layer 5 sequentially arranged ; Conductive carbon black coating 2 is obtained by coating the conductive carbon black coating solution in Example 1 of the present invention. The first release film layer 1 and the second release film layer 5 are transparent, and the material of the first release film layer 1 and the second release film layer 5 is preferably PET. The first release film layer 1 can be colorless or blue. The conductive adhesive layer is composed of acrylic adhesive and nickel powder. Among them, acrylic adhesive accounts for 92% of the mass fraction of the conductive adhesive layer; nickel powder accounts for 8% of the mass fraction of the conductive adhesive layer.
第一离型膜层1的厚度为100μm；所述导电炭黑涂层2的厚度为50μm；所述电沉积铜箔3层的厚度为50μm；所述导电胶黏剂层4的厚度为50μm；所述第二离型膜层5的厚度为100μm。The thickness of the first release film layer 1 is 100 μm; the thickness of the conductive carbon black coating 2 is 50 μm; the thickness of the electrodeposited copper foil 3 layer is 50 μm; the thickness of the conductive adhesive layer 4 is 50 μm The thickness of the second release film layer 5 is 100 μm.
在电阻上升比率测试过程中，当从常温(10℃)上升到80℃时，本发明的导电薄膜的电阻上升30％以上，表明本发明的导电薄膜在电压不稳条件下也能抑制局部的发热，从而避免火灾的发生。During the resistance rise ratio test, when the temperature rises from normal temperature (10°C) to 80°C, the resistance of the conductive film of the present invention rises by more than 30%, indicating that the conductive film of the present invention can also suppress local Heat to avoid fire.
以上所述仅是本发明的优选实施方式，并不用于限制本发明，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变型，这些改进和变型也应视为本发明的保护范围。The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. It should be pointed out that for those of ordinary skill in the art, several improvements can be made without departing from the technical principles of the present invention. And modifications, these improvements and modifications should also be regarded as the protection scope of the present invention.

Claims (10)

  1. 一种导电炭黑涂布液，其特征在于，以其总重为基准，包括以下质量分数的各组分：A conductive carbon black coating liquid, characterized in that, based on its total weight, it includes the following components in mass fractions:
    导电填料23-25份，所述导电填料中含有炭黑；23-25 parts of conductive filler, said conductive filler containing carbon black;
    酸性聚酯聚酰胺溶液1-1.5份；1-1.5 parts of acidic polyester polyamide solution;
    N-2-(氨基乙磺酸)-3-氨丙基三乙氧基硅烷0.8-1.0份；其结构式如下：0.8-1.0 parts of N-2-(aminoethanesulfonic acid)-3-aminopropyltriethoxysilane; its structural formula is as follows:
    Figure PCTCN2020070611-appb-100001
    Figure PCTCN2020070611-appb-100001
    聚二甲基硅氧烷0.5份；0.5 part of polydimethylsiloxane;
    一液型封端异氰酸酯1.8-2.0份；1.8-2.0 parts of one-component blocked isocyanate;
    2-苯基咪唑1.3-1.5份；1.3-1.5 parts of 2-phenylimidazole;
    密氨树脂1.5份；所述密氨树脂的结构式如下：1.5 parts of melamine resin; the structural formula of the melamine resin is as follows:
    Figure PCTCN2020070611-appb-100002
    Figure PCTCN2020070611-appb-100002
    余量为热塑性树脂。The balance is thermoplastic resin.
  2. 根据权利要求1所述的导电炭黑涂布液，其特征在于：所述导电填料中炭黑的质量分数为20-25份。The conductive carbon black coating liquid according to claim 1, wherein the mass fraction of carbon black in the conductive filler is 20-25 parts.
  3. 根据权利要求1所述的导电炭黑涂布液，其特征在于：所述酸性聚酯聚酰胺溶液中的溶剂为二甲苯或乙酸丁酯，所述酸性聚酯聚酰胺溶液的pH值为5-6.5。The conductive carbon black coating liquid of claim 1, wherein the solvent in the acidic polyester polyamide solution is xylene or butyl acetate, and the pH of the acidic polyester polyamide solution is 5 -6.5.
  4. 根据权利要求1所述的导电炭黑涂布液，其特征在于：所述聚二甲基硅氧烷的分子量为3000-10000g/mol。The conductive carbon black coating liquid according to claim 1, wherein the molecular weight of the polydimethylsiloxane is 3000-10000 g/mol.
  5. 根据权利要求1所述的导电炭黑涂布液，其特征在于：所述一液型封端异氰酸酯为甲乙酮肟封闭六甲基二异氰酸酯。The conductive carbon black coating liquid according to claim 1, wherein the one-component blocked isocyanate is methyl ethyl ketoxime blocked hexamethyl diisocyanate.
  6. 根据权利要求1所述的导电炭黑涂布液，其特征在于：所述密氨树脂的分子量为5000-10000g/mol。The conductive carbon black coating liquid according to claim 1, wherein the molecular weight of the melamine resin is 5000-10000 g/mol.
  7. 根据权利要求1所述的导电炭黑涂布液，其特征在于：所述热塑性树脂为涤纶树脂。The conductive carbon black coating liquid of claim 1, wherein the thermoplastic resin is a polyester resin.
  8. 一种导电薄膜，其特征在于：包括依次设置的第一离型膜层、导电炭黑涂层、电沉积铜箔层、导电胶黏剂层和第二离型膜层；所述导电炭黑涂层包括权利要求1-7中任一项所 述的导电炭黑涂布液。A conductive film, characterized in that it comprises a first release film layer, a conductive carbon black coating, an electrodeposited copper foil layer, a conductive adhesive layer and a second release film layer arranged in sequence; the conductive carbon black The coating layer comprises the conductive carbon black coating liquid according to any one of claims 1-7.
  9. 根据权利要求8所述的导电薄膜，其特征在于：所述第一离型膜层和第二离型膜层呈透明状，所述第一离型膜层和第二离型膜层的材质独立的选自PET。The conductive film according to claim 8, wherein the first release film layer and the second release film layer are transparent, and the materials of the first release film layer and the second release film layer Independently selected from PET.
  10. 根据权利要求8所述的导电薄膜，其特征在于：所述导电胶黏剂层的材质包括丙烯酸胶粘剂和镍粉。9. The conductive film of claim 8, wherein the conductive adhesive layer is made of acrylic adhesive and nickel powder.
PCT/CN2020/070611 2019-08-14 2020-01-07 Conductive carbon black coating liquid and conductive thin film WO2021027246A1 (en)

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