WO2019109711A1 - 柔性透明导电电极 - Google Patents

柔性透明导电电极 Download PDF

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WO2019109711A1
WO2019109711A1 PCT/CN2018/107054 CN2018107054W WO2019109711A1 WO 2019109711 A1 WO2019109711 A1 WO 2019109711A1 CN 2018107054 W CN2018107054 W CN 2018107054W WO 2019109711 A1 WO2019109711 A1 WO 2019109711A1
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parts
silver nanowire
solvent
flexible
transparent conductive
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夏厚君
杨晓明
江叔福
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Zhejiang Ouren New Materials Co Ltd
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Zhejiang Ouren New Materials Co Ltd
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Priority to EP18886729.5A priority Critical patent/EP3547332B1/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/30—Drying; Impregnating
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports

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  • the invention relates to the technical field of silver nanowires, and in particular to a flexible transparent conductive electrode.
  • Metal oxides especially ITO, have high light transmittance and low resistivity in the visible region, and have been the focus of research and application of transparent conductive electrodes for the past 50 years.
  • the metal oxide itself has limited conductivity, is brittle and fragile, and is not easily deformed.
  • raw material resources are increasingly scarce and expensive, and it has been unable to meet the needs of the development of modern optoelectronic devices.
  • transparent A new field of conductive electrode development is two-dimensional micro-nano new materials and structural thin film electrodes, such as high polymer conductive film, carbon nanotube film, graphene film and metal nano wire film.
  • Graphene film has good flexibility due to its special morphology, and also has good carrier mobility, but mass production technology is not yet mature; carbon nanotube film requires large aspect ratio, and carbon tube The uniform dispersion and ohmic resistance problems between the carbon tubes limit the in-plane conductivity of the film.
  • the transparent conductive film requires excellent light transmittance in addition to excellent electrical conductivity, and the nano metallic silver wire electrode has excellent electrical conductivity and light transmittance. Since silver is a good conductor and has good electrical conductivity, the micro-nano silver wire can be used as an electrode material to reduce energy consumption (relative to the oxide film electrode).
  • the micro-nano silver wire electrode is suitable for flexible, large-area and low-cost production. Therefore, the micro-nano silver wire electrode will become an advantageous substitute for the current ITO transparent conductive electrode.
  • the choice of additives in the micro-nano silver wire coating solution determines the performance of the product. Therefore, in order to obtain better performance, attempts have been made to prepare coating liquids of different properties with various additives. Indicators such as conductivity and bending resistance of silver nanowire films formed by existing formulations still need to be improved, and how to overcome the above technical problems and improve them has become a direction of efforts of those skilled in the art.
  • the object of the present invention is to provide a flexible transparent conductive electrode, wherein the silver nanowire slurry in the flexible transparent conductive electrode can reduce the content of silver nanowires, effectively disperse the nano silver wire, reduce the electrical resistivity, and improve the bending resistance.
  • the number of bends exceeded 5,000.
  • the technical solution adopted by the present invention is: a flexible transparent conductive electrode composed of a transparent flexible substrate and a silver nanowire coating coated on the surface of the transparent flexible substrate, the silver The nanowire coating has a thickness of 20 to 100 micrometers, and the silver nanowire coating is obtained by drying a silver nanowire slurry, and the silver nanowire slurry is composed of the following components by weight: silver nanowire aqueous dispersion 100 Parts, water-based acrylic resin 5-8 parts, triethylenetetramine 2-5 parts, p-methylsulfone toluene 1-2 parts, polyvinyl alcohol aqueous solution 0.2-0.5 parts, alkyl alcohol amide 0.2-0.4 parts, isopropoxy 0.3 to 0.5 parts of base ethanol, 0.1 to 0.3 parts of hydrogenated castor oil, and 30 to 40 parts of a composite solvent;
  • the flexible transparent conductive electrode is obtained by the following steps:
  • Step 1 100 parts of silver nanowire aqueous dispersion, 5-8 parts of aqueous acrylic resin, 2-5 parts of triethylenetetramine, 0.1-0.3 parts of hydrogenated castor oil, 30-40 parts of compound solvent; added to vacuum mixer Vacuum defoaming and mixing uniformly to obtain a mixed liquid, wherein the concentration of the aqueous silver nanowire dispersion is 2 to 10 mg/mL, and the composite solvent is prepared by mixing an alcohol solvent and a ketone solvent;
  • Step 2 adding 1 to 2 parts of p-methylsulfone toluene and 0.2 to 0.5 parts of polyvinyl alcohol aqueous solution in the mixture under stirring, and then stirring for about 10 minutes to make the mixture fully mixed.
  • the water-soluble resin liquid is water-soluble polymerization. Ester resin liquid;
  • Step 3 adding 0.2-0.4 parts of alkyl alcohol amide according to the amount, adding 0.3-0.5 parts of isopropoxyethanol to a vacuum mixer, and stirring uniformly, thereby obtaining a silver nanowire slurry based on silver nanowires;
  • Step 4 PET is used as a transparent flexible substrate, and the silver nanowire slurry is uniformly coated on PET by wire bar coating, wherein the wire rod spacing is 15 ⁇ m, the roller coating speed is 80 cm/min, and the surface of the substrate is Forming a uniform wet film;
  • Step 5 Dry the wet film in a vacuum oven at 150 ° C for 3 to 10 minutes, and completely evaporate in the wet film, and take out the flexible transparent conductive electrode.
  • the silver nanowires in the silver nanowire aqueous dispersion have a diameter of 20 to 150 nm, and the nano silver wire has a length of 50 to 500 mm.
  • the alcohol solvent is one of methanol, ethanol and isopropanol.
  • the ketone solvent is one of acetone, methyl ethyl ketone, cyclohexanone, and isophorone.
  • the complex solvent is prepared by mixing an alcohol solvent and a ketone solvent in a weight ratio of 10: (2 to 4).
  • the present invention has the following advantages and effects compared with the prior art:
  • the flexible transparent conductive electrode of the present invention comprises 100 parts of a silver nanowire aqueous dispersion, 5-8 parts of an aqueous acrylic resin, 0.2 to 0.5 parts of a polyvinyl alcohol aqueous solution, 0.2 to 0.4 parts of an alkyl alcohol amide, and 0.3 isopropoxyethanol. Further adding 2 to 5 parts of triethylenetetramine and 1 to 2 parts of p-methylsulfone toluene in 0.5 parts of the system can reduce the content of silver nanowires, effectively disperse the nano silver wire, reduce the electrical resistivity, and improve the electrical resistivity.
  • the formulation is further mixed with isopropoxyethanol 0.3-0.5 parts and mixed with an alcohol solvent and a ketone solvent according to 10: (2 to 4) parts by weight.
  • the composite solvent effectively adjusts the viscosity and drying speed of the coating liquid, further avoids the accumulation of silver nanowires, ensures uniformity of electrical conductivity, and improves light transmittance.
  • Embodiments 1-4 A flexible transparent conductive electrode comprising a transparent flexible substrate and a silver nanowire coating applied to the surface of the transparent flexible substrate, the silver nanowire coating having a thickness of 20 ⁇ 100 ⁇ m, the silver nanowire coating is obtained by drying a silver nanowire slurry, and the silver nanowire slurry is composed of the following parts by weight, as shown in Table 1:
  • Example 1 Example 2 Example 3 Example 4 Silver nanowire aqueous dispersion 100 copies 100 copies 100 copies 100 copies 100 copies Waterborne acrylic resin 6 servings 5 servings 6.2 copies 7 servings Triethylenetetramine 3 copies 2.2 servings 5 servings 4 parts M-methylsulfone toluene 1.8 copies 1 serving 1.5 servings 1.2 servings Polyvinyl alcohol aqueous solution 0.24 parts 0.4 parts 0.3 parts 0.45 parts Alkyl alcohol amide 0.3 parts 0.35 parts 0.4 parts 0.26 parts Isopropoxyethanol 0.4 parts 0.5 parts 0.35 parts 0.42 parts Hydrogenated castor oil 0.15 parts 0.25 parts 0.1 parts 0.2 parts Compound solvent 35 copies 32 copies 38 servings 35 copies ;
  • the complex solvent is prepared by mixing methanol and cyclohexanone in an amount of 10:2 parts by weight.
  • the complex solvent is prepared by mixing isopropanol and methyl ethyl ketone in an amount of 10:2.5 parts by weight.
  • the solvent was prepared by mixing ethanol and cyclohexanone in an amount of 10:3 parts by weight.
  • the complex solvent was mixed with methanol and isophorone in an amount of 10:3.8 parts by weight.
  • the flexible transparent conductive electrode is obtained by the following steps:
  • Step 1 100 parts of silver nanowire aqueous dispersion, 5-8 parts of aqueous acrylic resin, 2-5 parts of triethylenetetramine, 0.1-0.3 parts of hydrogenated castor oil, 30-40 parts of compound solvent; added to vacuum mixer Vacuum defoaming, mixing uniformly, obtaining a mixed liquid, the concentration of the silver nanowire aqueous dispersion is 2-10 mg/mL; the composite solvent is prepared by mixing an alcohol solvent and a ketone solvent;
  • Step 2 adding 1 to 2 parts of p-methylsulfone toluene and 0.2 to 0.5 parts of polyvinyl alcohol aqueous solution in the mixture under stirring, and then stirring for about 10 minutes to make the mixture fully mixed.
  • the water-soluble resin liquid is water-soluble polymerization. Ester resin liquid;
  • Step 3 adding 0.2-0.4 parts of alkyl alcohol amide according to the amount, adding 0.3-0.5 parts of isopropoxyethanol to a vacuum mixer, and stirring uniformly, thereby obtaining a silver nanowire slurry based on silver nanowires;
  • Step 4 PET is used as a transparent flexible substrate, and the silver nanowire slurry is uniformly coated on PET by wire bar coating, wherein the wire rod spacing is 15 ⁇ m, the roller coating speed is 80 cm/min, and the surface of the substrate is Forming a uniform wet film;
  • Step 5 Dry the wet film in a vacuum oven at 150 ° C for 3 to 10 minutes, and completely evaporate in the wet film, and take out the flexible transparent conductive electrode.
  • the silver nanowire aqueous dispersion has a diameter of 20 to 150 nm and a nano silver wire length of 50 to 500 mm.
  • the flexible transparent conductive electrode of the present invention when used, it can reduce the content of silver nanowires, effectively disperse the nano silver wire, reduce the electrical resistivity, and improve the bending resistance, and the number of bending times exceeds 5000 times; secondly, it effectively adjusts the viscosity and drying speed of the coating liquid, further avoids the accumulation of silver nanowires, ensures uniformity of electrical conductivity, and improves light transmittance.

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Abstract

一种柔性透明导电电极，所述柔性透明导电电极由透明柔性基材和涂覆于透明柔性基材表面的银纳米线涂层组成，包括以下步骤：将银纳米线水分散液、水性丙烯酸树脂、三乙烯四胺、对甲砜基甲苯1～2份、氢化蓖麻油0.1～0.3份、复合溶剂；加入到真空搅拌机中真空脱泡、混合均匀，获得混合液，所述银纳米线水分散液的浓度为2～10mg/mL，所述复合溶剂由醇类溶剂、酮类溶剂混合而成；将湿膜在150℃真空干燥箱干燥3～10min，待湿膜中完全挥发，取出即所述柔性透明导电电极。该电极降低了导电电阻率，也进一步避免了银纳米线堆积，保证了导电的均匀性，也改善了透光率。

Description

柔性透明导电电极 技术领域
本发明涉及一种银纳米线技术领域，特别涉及一种柔性透明导电电极。
背景技术
金属氧化物，特别是ITO，在可见光区具有较高的光透过率和较低的电阻率，在过去50年来一直是透明导电电极研究和应用的热点。然而金属氧化物本身导电性有限，且质脆易碎，不易变形等缺陷，同时原料资源日益稀缺，价格昂贵，已经无法满足现代光电子器件的发展的需求近年来随着微纳米技术的发展，透明导电电极开拓的一个新领域是二维微纳米新材料与结构薄膜电极，例如高聚物导电薄膜，碳纳米管膜，石墨烯膜以及金属纳米线膜。石墨烯薄膜因其本身特殊的形貌而具有很好的柔性，同时也具有很好的载流子迁移率，但量产技术尚未成熟；碳纳米管薄膜需要较大长径比，且碳管的均匀分散和碳管之间的欧姆电阻问题限制了薄膜的面内导电性。透明导电薄膜除了优良的导电性，还需要优良的光透射率，而纳米金属银线电极具有出色的导电性和光透射率。由于银是电良导体，导电性好，因而微纳米银线用作电极材料可以降低能耗(相对于氧化物薄膜电极)。同时微纳米银线的粒径小于可见光入射波长时，金属微纳米结构的等离子效应增强光透射率，使电极具有很好的光电性能。同时微纳米银线电极适合柔性、大面积低成本生产。因而微纳米银线电极将成为现在ITO透明导电电极的有利替代者。而微纳米银线涂覆液中助剂的选择则决定了产品的性能。因此，为得到较佳性能，人们尝试用各种不同助剂配制了不同性能的涂覆液。现有配方形成的银纳米线薄膜导电性和耐折弯性能等指标仍有待改善，如何克服上述技术问题并改善，成为本领域普通技术人员努力的方向。
发明内容
本发明目的是提供一种柔性透明导电电极，此柔性透明导电电极中银纳米线浆料既可降低银纳米线含量，有效地分散纳米银线，降低了导电电阻率，也提高了耐折弯性能，折弯次数超过5000次。
为达到上述目的，本发明采用的技术方案是：一种柔性透明导电电极，所述柔性透明导电电极由透明柔性基材和涂覆于透明柔性基材表面的银纳米线涂层组成，此银纳米线涂层厚度为20～100微米，所述银纳米线涂层由银纳米线浆料烘干获得，此银纳米线浆料由以下重量份的组分组成：银纳米线水分散液100份、水性丙烯酸树脂5～8份、三乙烯四胺2～5份、对甲砜基甲苯1～2份、聚乙烯醇水溶液0.2～0.5份、烷基醇酰胺0.2～0.4份、异丙氧基乙醇0.3～0.5份、氢化蓖麻油0.1～0.3份、复合溶剂30～40份；
所述柔性透明导电电极通过以下步骤获得：
步骤一、将银纳米线水分散液100份、水性丙烯酸树脂5～8份、三乙烯四胺2～5份、氢化 蓖麻油0.1～0.3份、复合溶剂30～40份；加入到真空搅拌机中真空脱泡、混合均匀，获得混合液，所述银纳米线水分散液的浓度为2～10mg/mL，所述复合溶剂由醇类溶剂、酮类溶剂混合而成；
步骤二、在搅拌下在混合液加入对甲砜基甲苯1～2份、聚乙烯醇水溶液0.2～0.5份，后继续搅拌约10分钟，使充分混合均匀，此水溶性树脂液为水溶性聚酯树脂液；
步骤三、按量加入烷基醇酰胺0.2～0.4份，异丙氧基乙醇0.3～0.5份加入到真空搅拌机中，继续搅拌均匀，即获得基于银纳米线为的银纳米线浆料；
步骤四、以PET为透明柔性基材，将所述银纳米线浆料以线棒滚涂的方式均匀涂覆于PET，其中线棒间距为15μm，滚涂速度为80cm/min，基材表面形成一层均匀的湿膜；
步骤五、将所述湿膜在150℃真空干燥箱干燥3～10min，待湿膜中完全挥发，取出即所述柔性透明导电电极。
上述技术方案中进一步改进技术方案如下：
1、上述方案中，所述银纳米线水分散液中银纳米线直径为20～150nm，纳米银线长度为50～500mm。
2、上述方案中，所述醇类溶剂为甲醇、乙醇和异丙醇中的一种。
3、上述方案中，所述酮类溶剂为丙酮、丁酮、环己酮、异佛尔酮中的一种。
4、上述方案中，所述复合溶剂由醇类溶剂、酮类溶剂按照10：(2～4)的重量份混合而成。
由于上述技术方案运用，本发明与现有技术相比具有下列优点和效果：
本发明柔性透明导电电极，其在银纳米线水分散液100份、水性丙烯酸树脂5～8份、聚乙烯醇水溶液0.2～0.5份、烷基醇酰胺0.2～0.4份、异丙氧基乙醇0.3～0.5份体系中进一步添加三乙烯四胺2～5份、对甲砜基甲苯1～2份，既可降低银纳米线含量，有效地分散纳米银线，降低了导电电阻率，也提高了耐折弯性能，折弯次数超过5000次；其次，其配方进一步采用异丙氧基乙醇0.3～0.5份和由醇类溶剂、酮类溶剂按照10：(2～4)的重量份混合而成复合溶剂，有效调节涂覆液的粘度和干燥速度，进一步避免了银纳米线堆积，保证了导电的均匀性，也改善了透光率。
具体实施方式
下面结合实施例对本发明作进一步描述：
实施例1～4：一种柔性透明导电电极，所述柔性透明导电电极由透明柔性基材和涂覆于透明柔性基材表面的银纳米线涂层组成，此银纳米线涂层厚度为20～100微米，所述银纳米线涂层由银纳米线浆料烘干获得，此银纳米线浆料由以下重量份的组分组成，如表1所示：
表1
  实施例1 实施例2 实施例3 实施例4
银纳米线水分散液 100份 100份 100份 100份
水性丙烯酸树脂 6份 5份 6.2份 7份
三乙烯四胺 3份 2.2份 5份 4份
对甲砜基甲苯 1.8份 1份 1.5份 1.2份
聚乙烯醇水溶液 0.24份 0.4份 0.3份 0.45份
烷基醇酰胺 0.3份 0.35份 0.4份 0.26份
异丙氧基乙醇 0.4份 0.5份 0.35份 0.42份
氢化蓖麻油 0.15份 0.25份 0.1份 0.2份
复合溶剂 35份 32份 38份 35份
；
实施例1中复合溶剂由甲醇、环己酮按照10：2重量份混合而成，实施例2中复合溶剂由异丙醇、丁酮按照10：2.5重量份混合而成，实施例3中复合溶剂由乙醇、环己酮按照10：3重量份混合而成，实施例4中复合溶剂由甲醇、异佛尔酮按照10：3.8重量份混合而成。
所述柔性透明导电电极通过以下步骤获得：
步骤一、将银纳米线水分散液100份、水性丙烯酸树脂5～8份、三乙烯四胺2～5份、氢化蓖麻油0.1～0.3份、复合溶剂30～40份；加入到真空搅拌机中真空脱泡、混合均匀，获得混合液，所述银纳米线水分散液的浓度为2～10mg/mL；所述复合溶剂由醇类溶剂、酮类溶剂混合而成；
步骤二、在搅拌下在混合液加入对甲砜基甲苯1～2份、聚乙烯醇水溶液0.2～0.5份，后继续搅拌约10分钟，使充分混合均匀，此水溶性树脂液为水溶性聚酯树脂液；
步骤三、按量加入烷基醇酰胺0.2～0.4份，异丙氧基乙醇0.3～0.5份加入到真空搅拌机中，继续搅拌均匀，即获得基于银纳米线为的银纳米线浆料；
步骤四、以PET为透明柔性基材，将所述银纳米线浆料以线棒滚涂的方式均匀涂覆于PET，其中线棒间距为15μm，滚涂速度为80cm/min，基材表面形成一层均匀的湿膜；
步骤五、将所述湿膜在150℃真空干燥箱干燥3～10min，待湿膜中完全挥发，取出即所述柔性透明导电电极。
上述银纳米线水分散液中银纳米线直径为20～150nm，纳米银线长度为50～500mm。
本实施例1～4柔性透明导电电极的测试结果，如表2所示：
表2
Figure PCTCN2018107054-appb-000001
从表格2可知，采用本发明柔性透明导电电极时，其，其既可降低银纳米线含量，有效地分散纳米银线，降低了导电电阻率，也提高了耐折弯性能，折弯次数超过5000次；其次，其有效调节涂覆液的粘度和干燥速度，进一步避免了银纳米线堆积，保证了导电的均匀性，也改善了透光率。
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。

Claims (5)

  1. 一种柔性透明导电电极，其特征在于：所述柔性透明导电电极由透明柔性基材和涂覆于透明柔性基材表面的银纳米线涂层组成，此银纳米线涂层厚度为20～100微米，所述银纳米线涂层由银纳米线浆料烘干获得，此银纳米线浆料由以下重量份的组分组成：银纳米线水分散液100份、水性丙烯酸树脂5～8份、三乙烯四胺2～5份、对甲砜基甲苯1～2份、聚乙烯醇水溶液0.2～0.5份、烷基醇酰胺0.2～0.4份、异丙氧基乙醇0.3～0.5份、氢化蓖麻油0.1～0.3份、复合溶剂30～40份；
    所述柔性透明导电电极通过以下步骤获得：
    步骤一、将银纳米线水分散液100份、水性丙烯酸树脂5～8份、三乙烯四胺2～5份、氢化蓖麻油0.1～0.3份、复合溶剂30～40份；加入到真空搅拌机中真空脱泡、混合均匀，获得混合液，所述银纳米线水分散液的浓度为2～10mg/mL；所述复合溶剂由醇类溶剂、酮类溶剂混合而成；
    步骤二、在搅拌下在混合液加入对甲砜基甲苯1～2份、聚乙烯醇水溶液0.2～0.5份，后继续搅拌约10分钟，使充分混合均匀，此水溶性树脂液为水溶性聚酯树脂液；
    步骤三、按量加入烷基醇酰胺0.2～0.4份，异丙氧基乙醇0.3～0.5份加入到真空搅拌机中，继续搅拌均匀，即获得基于银纳米线为的银纳米线浆料；
    步骤四、以PET为透明柔性基材，将所述银纳米线浆料以线棒滚涂的方式均匀涂覆于PET，其中线棒间距为15μm，滚涂速度为80cm/min，基材表面形成一层均匀的湿膜；
    步骤五、将所述湿膜在150℃真空干燥箱干燥3～10min，待湿膜中完全挥发，取出即所述柔性透明导电电极。
  2. 根据权利要求1所述的柔性导电薄膜用银纳米线浆料的制备工艺，其特征在于：所述银纳米线水分散液中银纳米线直径为20～150nm，纳米银线长度为50～500mm。
  3. 根据权利要求1所述的柔性导电薄膜用银纳米线浆料的制备工艺，其特征在于：所述醇类溶剂为甲醇、乙醇和异丙醇中的一种。
  4. 根据权利要求1所述的柔性导电薄膜用银纳米线浆料的制备工艺，其特征在于：所述酮类溶剂为丙酮、丁酮、环己酮、异佛尔酮中的一种。
  5. 根据权利要求1所述的柔性导电薄膜用银纳米线浆料的制备工艺，其特征在于：所述复合溶剂由醇类溶剂、酮类溶剂按照10：(2～4)的重量份混合而成。
PCT/CN2018/107054 2017-12-07 2018-09-21 柔性透明导电电极 Ceased WO2019109711A1 (zh)

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