EP3547332B1 - Électrode conductrice transparente souple - Google Patents

Électrode conductrice transparente souple Download PDF

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Publication number
EP3547332B1
EP3547332B1 EP18886729.5A EP18886729A EP3547332B1 EP 3547332 B1 EP3547332 B1 EP 3547332B1 EP 18886729 A EP18886729 A EP 18886729A EP 3547332 B1 EP3547332 B1 EP 3547332B1
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EP
European Patent Office
Prior art keywords
parts
coating
mixture
flexible
silver nanowire
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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EP18886729.5A
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German (de)
English (en)
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EP3547332A1 (fr
EP3547332A4 (fr
Inventor
Houjun XIA
Xiaoming Yang
Shufu JIANG
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Zhejiang Ouren New Materials Co Ltd
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Zhejiang Ouren New Materials Co Ltd
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Classifications

    • 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
    • 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

Definitions

  • the present invention discloses a flexible transparent conductive electrode.
  • the flexible transparent conductive electrode is made of transparent flexible base materials and a transparent flexible substrate coated with a silver nanowire coating.
  • the process of fabricating the flexible transparent conductive electrode comprises a few steps as followings: adding silver nanowire aqueous dispersion, aqueous acrylic resin, triethylenetetramine, 1-2 parts of p-methylsulfonyl toluene, 0.1-0.3 pars of hydrogenated castor oil and a mixture solvent into a vacuum mixer where evenly mixed, vacuum defoamed, and thus the coating is prepared.
  • the concentration of the silver nanowire in the coating is 2-10mg/mL and the mixture solvents used are the mixture of alcohol and ketone.
  • the film is coated with above coating and moved into a vacuum dryer to be dried at 150°C for 3-10min so that the solvents in the coating are completely volatilized and the flexible transparent conductive electrode is obtained.
  • the flexible transparent conductive electrode of the invention has characteristics of the lower conductive resistivity, less stacks of silver nanowires, higher uniformity of conductivity and better optical transmittance comparison with the existing products.
  • the present invention relates to a technology of silver nanowires, particularly relates to a flexible transparent conductive electrode. insert content of description insertion page 1a here
  • US 2015/166798 A1 discloses a transparent conductive film including metal nanowires and a colored compound adsorbed by the metal nanowires.
  • the metal nanowires are a material which absorbs light in the visible light region, and also each has a functional group which is bound to a metal constituting the metal nanowire.
  • Metal oxides especially ITO, has the characteristics of good optical transmittance in visible region and low resistivity which have been hot spots in researches and applications of transparent conductive electrodes in the past 5 decades.
  • metal oxides have the disadvantages as limited conductivity, brittle and hard to deform.
  • Concurrently, scarce resources and risen prices are unable to meet the requirements for developing the modern optoelectronic devices.
  • Two dimensional micro-nano new materials and structured thin film electrodes are new fields of transparent conductive electrodes with the development of micro nanotechnology in recent years, such as conductive thin film of polymers, carbon nanotube film, graphene film and metal nanowire film.
  • Transparent conductive film has advantages of not only great conductivity but also good optical transmission while nanometallic silver wire electrode's are excellent.
  • Micro-nano silver wires can be used as electrode materials with less energy consumption (compared with electrode of oxide thin film) since silver is an electric conductor with great electrical conductivity.
  • micro nano structure of metal with plasma effect increases transmittance while diameters of micro silver nanowires' particles are smaller than the incident wavelength of visible light, and perfect photoelectric properties are achieved for electrodes.
  • micro silver nanowire electrode is benefit for flexible industries and large scale productions with lower cost. Therefore, the micro silver nanowire electrode will be a favorable alternative to ITO transparent conductive electrode.
  • the additives for preparing coating fluid of micro silver nanowires determines performances of the electrode. Therefore, various additives are used to prepare different coating fluid for different properties in order to get better performances. Properties as conductivity and flexural endurance are still to be improved by using current formula. To overcome the problems and go on improving in the prior art are directions for those skilled in this field.
  • the object of the present invention is to provide a flexible transparent conductive electrode, in which silver nanowire coating is used. It can not only reduce the content of silver nanowires, effectively disperse silver nanowires, reduce the conductive resistivity, but also improve the bending resistance to be more than 5000 bending times .
  • the present invention is defined in independent claim 1.
  • the dependent claims define embodiments of the invention.
  • the technical scheme adopted by the present invention is a flexible transparent conductive electrode consisting of a transparent flexible substrate and a silver nanowire coating, which the coating is coated on the surface of the transparent flexible substrate and the thickness of the silver nanowire coating is 20-100 microns after dried.
  • the silver nanowire coating comprises following compounds by weight: 100 parts of silver nanowire aqueous dispersion, 5-8 parts of aqueous acrylic resin, 2-5 parts of triethylenetetramine, 1-2 parts of p-methylsulfonyl toluene, 0.2-0.5 parts of polyvinyl alcohol aqueous solution, 0.2-0.4 parts of alkanolamide, 0.3-0.5 parts of isopropoxyethanol, 0.1-0.3 parts of hydrogenated castor oil, 30-40 parts of mixture solvents.
  • the process of fabricating the flexible transparent conductive electrode comprises a few steps as followings:
  • the flexible transparent conductive electrode of the invention contains 100 parts of silver nanowire aqueous dispersion, 5-8 parts of water-borne acrylic resin, 0.2-0.5 parts of polyvinyl alcohol aqueous solution, 0.2-0.4 parts of alkyholamide, 0.3-0.5 parts of isopropoxyethylanol as a primary formula, and further adds with 2-5 parts of triethylenetetramine and 1-2 parts of p-methylsulfonyl toluene which reduces the content of silver nanowires, effectively disperses the silver nanowires, reduces the resistivity and improve the bending resistance to be more than 5000 bending times.
  • formulations 1-4 a flexible transparent conductive electrode is comprised of a transparent flexible substrate coated with a silver nanowires coating at a thickness of 20-100 ⁇ m after the silver nanowire coating is dried.
  • the silver nanowire coating is consist of the following ingredients by weight as shown in Table 1: Table 1 Ingredients formulation 1 (parts) formulation 2 (parts) formulation 3 (parts) formulation 4 (parts) Silver Nanowire Aqueous Dispersion 100 100 100 100 aqueous Acrylic Resin 6 5 6.2 7 Triethylenetetramine 3 2.2 5 4 p-methylsulfonyl toluene 1. 8 1 1.5 1.2 PVA Aqueous Solution 0.24 0.4 0. 3 0. 45 Alkanolamide 0.3 0.35 0.4 0. 26 Isopropoxyethanol 0.4 0. 5 0.35 0.42 Hydrogenated Castor Oil 0. 15 0. 25 0.1 0.2 Mixture Solvents 35 32 38 35
  • the process of fabricating the flexible transparent conductive electrode comprises a few steps as followings:
  • the silver nanowires in the above coating have the diameters of 20-150nm and lengths of 50-500mm:
  • Table 2 Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Resistance( ⁇ /square) (Four-probe Resistance Tester) 31 30 30 32 Adhesion(Vertical Pulled with 3M600) No shedding No shedding No shedding No shedding Transmittance(%)(WG W Optical Haze Meter) 92 92 91 92 Haze(WGW Optical Haze Meter) 1. 2 1. 3 1. 2 1. 3 Flexural Endurance(time) >5000 >5000 >5000 >5000
  • the characteristics of the flexible transparent electrode which is provided in the present invention have thus been shown in Table 2 to be achieved in reducing the content of silver nanowires, effectively dispersing the silver nanowires, reducing resistivity and improve the bending resistance to be more than 5000 bending times; and effectively adjusting the viscosity and drying rate of coating fluid, further avoiding stacks of the silver nanowires, ensuring uniformity of the conductivity and improving transmittance.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Non-Insulated Conductors (AREA)
  • Conductive Materials (AREA)
  • Manufacturing Of Electric Cables (AREA)

Claims (5)

  1. Electrode conductrice transparente flexible, caractérisée en ce que l'électrode conductrice transparente flexible comprend un substrat flexible transparent et un revêtement de nanofils d'argent qui est appliqué sur la surface du substrat; le revêtement sur la surface du substrat flexible transparent est séché dans un four et l'épaisseur du revêtement de nanofils d'argent est de 20 à 100 µm après séchage. Le revêtement de nanofils d'argent comprend les ingrédients suivants en poids: 100 parties de dispersion aqueuse de nanofils d'argent, 5-8 parties de résine acrylique aqueuse, 2-5 parties de triéthylènetétramine, 1-2 parties de p-méthyl-sulfonyltoluène, 0,2-0,5 partie de solution aqueuse d'alcool polyvinylique (PVA), 0,2-0,4 partie d'alcanolamide, 0,3-0,5 partie d'isopropoxyéthanol, 0,1-0,3 partie d'huile de ricin hydrogénée et 30-40 parties d'un mélange de solvants;
    le procédé de fabrication de l'électrode conductrice transparente flexible comprend les étapes suivantes:
    étape 1 - 100 parties de dispersion aqueuse de nanofils d'argent, 5 à 8 parties de résine acrylique aqueuse, 2 à 5 parties de triéthylènetétramine, 0,1 à 0,3 partie d'huile de ricin hydrogénée et 30 à 40 parties d'un mélange de solvants sont toutes ajoutées dans un mélangeur sous vide où elles sont mélangées uniform-mément, démoussées sous vide, puis la solution de mélange est préparée, dans laquelle la concentration de nanofils d'argent dans la dispersion aqueuse est de 2 à 10 mg/ml et le solvant du mélange est un mélange de solvant alcoolique et de solvant cétonique;
    étape 2 - 1-2 parties de p-méthylsulfonyl toluène et 0,2-0,5 parties de solution aqueuse d'alcool polyvinylique sont ajoutées dans la solution de mélange pendant le processus d'agitation. Le fluide de résine soluble dans l'eau est un fluide de résine polyester soluble dans l'eau après avoir été mélangé uniformément pendant 10 minutes d'agitation;
    étape 3 - 0,2-0,4 parties d'alcanolamide et 0,3-0,5 parties d'isopropoxyéthanol sont ajoutées dans un mélangeur sous vide pour être continuellement agitées et mélangées uniformément. Le revêtement à base de nanofils d'argent est préparé;
    étape 4 - le substrat flexible transparent est un film PET qui est uniformément revêtu du revêtement de nanofils d'argent en utilisant un procédé de laminage de tige de fil. Les distances entre le fil et la tige sont de 15 µmi et la vitesse de roulement pour le revêtement est de 80 cm/min, un film humide uniforme est formé sur la surface du substrat flexible transparent;
    étape 5 - le film humide revêtu de l'enduit ci-dessus est complètement volatilisé après avoir été séché dans un séchoir à vide à 150° C pendant 3-10 min, et l'électrode conductrice transparente flexible est obtenue.
  2. Film conducteur flexible selon la revendication 1, dans lequel : les nanofils d'argent de la dispersion aqueuse de nanofils d'argent ont des diamètres de 20-150 nm et des longueurs de 50-500 mm.
  3. Film conducteur flexible selon la revendication 1, dans lequel : le solvant alcoolique est l'un des méthanol, éthanol et isopropanol.
  4. Film conducteur flexible selon la revendication 1, dans lequel : le solvant cétonique est l'un des solvants suivants : acétone, butanone, cyclohexanone et isophorone.
  5. Film conducteur flexible selon la revendication 1, dans lequel : le solvant du mélange est un mélange de solvant alcoolique et de solvant cétonique de 10 :(2-4) en poids.
EP18886729.5A 2017-12-07 2018-09-21 Électrode conductrice transparente souple Active EP3547332B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201711280783.3A CN108417294A (zh) 2017-12-07 2017-12-07 柔性透明导电电极
PCT/CN2018/107054 WO2019109711A1 (fr) 2017-12-07 2018-09-21 Électrode conductrice transparente souple

Publications (3)

Publication Number Publication Date
EP3547332A1 EP3547332A1 (fr) 2019-10-02
EP3547332A4 EP3547332A4 (fr) 2020-09-16
EP3547332B1 true EP3547332B1 (fr) 2022-03-16

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EP18886729.5A Active EP3547332B1 (fr) 2017-12-07 2018-09-21 Électrode conductrice transparente souple

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EP (1) EP3547332B1 (fr)
CN (1) CN108417294A (fr)
WO (1) WO2019109711A1 (fr)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108417294A (zh) * 2017-12-07 2018-08-17 浙江欧仁新材料有限公司 柔性透明导电电极
CN110183700A (zh) * 2019-05-30 2019-08-30 中国科学技术大学 银纳米线柔性透明导电电极的制备方法、电致变色器件及其制备方法
CN114989472B (zh) * 2021-03-02 2023-04-14 天津理工大学 导电油墨在降低柔性极板多次弯折后电阻率中的应用
CN115073792B (zh) * 2022-04-29 2023-08-04 湖北大学 一种银纳米线与二维锑烯复合导电薄膜及其柔性透明超级电容器

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US7727578B2 (en) * 2007-12-27 2010-06-01 Honeywell International Inc. Transparent conductors and methods for fabricating transparent conductors
KR101489161B1 (ko) * 2010-07-30 2015-02-06 주식회사 잉크테크 투명 도전막의 제조방법 및 이에 의해 제조된 투명 도전막
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Publication number Publication date
WO2019109711A1 (fr) 2019-06-13
CN108417294A (zh) 2018-08-17
EP3547332A1 (fr) 2019-10-02
EP3547332A4 (fr) 2020-09-16

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