EP2729973A1 - Electrode transparente conductrice multicouche et procédé de fabrication associé - Google Patents
Electrode transparente conductrice multicouche et procédé de fabrication associéInfo
- Publication number
- EP2729973A1 EP2729973A1 EP12737735.6A EP12737735A EP2729973A1 EP 2729973 A1 EP2729973 A1 EP 2729973A1 EP 12737735 A EP12737735 A EP 12737735A EP 2729973 A1 EP2729973 A1 EP 2729973A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- nanofilaments
- particles
- layer
- metal
- transparent electrode
- 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.)
- Withdrawn
Links
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
- H01B13/0013—Apparatus or processes specially adapted for manufacturing conductors or cables for embedding wires in plastic layers
-
- 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
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022466—Electrodes made of transparent conductive layers, e.g. TCO, ITO layers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/0274—Optical details, e.g. printed circuits comprising integral optical means
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/80—Constructional details
- H10K30/81—Electrodes
- H10K30/82—Transparent electrodes, e.g. indium tin oxide [ITO] electrodes
-
- H—ELECTRICITY
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- H10K30/81—Electrodes
- H10K30/82—Transparent electrodes, e.g. indium tin oxide [ITO] electrodes
- H10K30/821—Transparent electrodes, e.g. indium tin oxide [ITO] electrodes comprising carbon nanotubes
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- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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Definitions
- the present invention relates to a transparent conductive electrode and its method of manufacture, in the general field of organic electronics.
- Transparent conductive electrodes having both high transmittance and electrical conductivity properties are currently undergoing considerable development in the field of electronic equipment, this type of electrodes being increasingly used for devices such as cells Photovoltaic, liquid crystal displays, organic light-emitting diodes (OLEDs) or polymeric light-emitting diodes (PLEDs), as well as touch screens.
- a multilayer conductive transparent electrode initially comprising a substrate on which a bonding layer, a bonding network, a bonding layer is deposited.
- metal nanofilaments and a conductive polymer encapsulation layer such as, for example, a poly (3,4-ethylenedioxythiophene) (PEDOT) and sodium poly (styrene sulfonate) (PSS) mixture, forming the so-called PEDOT: PSS .
- PEDOT poly (3,4-ethylenedioxythiophene)
- PSS sodium poly (styrene sulfonate)
- US2009 / 0129004 discloses a conductive transparent electrode according to this multilayer construction.
- this type of multilayer conductive transparent electrode composition is not entirely satisfactory, especially since the PEDOT: PSS encapsulation layer, having an acid PH, can oxidize the metal nanofilaments and thus reduce the electrical conductivity of the electrode.
- One of the aims of the invention is therefore to at least partially overcome the disadvantages of the prior art and to provide a multilayer conductive transparent electrode having high transmittance and electrical conductivity properties, as well as its manufacturing process.
- the multilayer conductive transparent electrodes according to the invention and obtained according to the manufacturing method according to the invention satisfy the following requirements and properties:
- the present invention relates to a multilayer conductive transparent electrode, comprising a substrate layer, an adhesion layer, a percolating network of metal nanofilaments, an electric homogenization layer, said electric homogenization layer comprising:
- the electric homogenization layer also comprises crosslinked or non-crosslinked polymer particles chosen from functionalized or non-functionalized particles of polystyrene, polycarbonate and polymethylenemelamine, said particles of non-crosslinked polymer having a temperature. glass transition Tg greater than 80 ° C, glass particles, silica particles, and / or metal oxide particles selected from the following metal oxides: ZnO, MgO, MGA1 2 0 4 , borosilicate particles.
- the multilayer conductive transparent electrode has a mean transmittance on the visible spectrum greater than 75%.
- the multilayer conductive transparent electrode has a surface resistance of less than 1000 ⁇ / ⁇ .
- the adhesion layer is made of nitrile rubber.
- the percolating network of metal nanofilaments is multilayer.
- the metal nanofilament network has a metal nanofilament density of between 0.01 ⁇ g / cm 2 and 1 mg / cm 2 .
- the metal nanofilaments are nanofilaments of noble metals.
- the metal nanofilaments are nanofilaments of non-noble metals.
- the substrate is selected from glass and transparent flexible polymers.
- the invention also relates to a method for manufacturing a multilayer conductive transparent electrode, comprising the following steps:
- composition forming the electric homogenization layer comprising:
- the electric homogenization layer also comprises particles of crosslinked or non-crosslinked polymer chosen from functionalized or non-functionalized particles of polystyrene, polycarbonate and polymethylenemelamine, said particles of non-crosslinked polymer having a temperature.
- glass transition Tg greater than 80 ° C, glass particles, silica particles, and / or metal oxide particles selected from the following metal oxides: ZnO, MgO, MGA1 2 0 4 , borosilicate particles.
- the substrate is selected from glass and transparent flexible polymers.
- the adhesion layer is made of nitrile rubber.
- the steps of applying a suspension of metal nanofilaments on the adhesion layer in an organic solvent and of evaporation of the organic solvents of the suspension of metal nanofilaments are carried out several times successively. to obtain a percolating network of multilayer metal nanofilaments.
- the metal nanofilaments are nanofilaments of noble metals.
- the metal nanofilaments are nanofilaments of non-noble metals.
- FIG. 1 shows a flowchart of the various steps of the manufacturing method according to the invention
- FIG. 2 shows a diagrammatic perspective representation in an exploded view of the various layers of the multilayer conductive transparent electrode
- FIG. 3 shows a schematic representation in perspective of the various layers of the multilayer conductive transparent electrode
- FIGS. 4 and 5 show photos produced by scanning electron microscope of a section of a multilayer conductive transparent electrode.
- the present invention thus relates to a method of manufacturing a multilayer conductive transparent electrode, comprising steps i), ii), iii), iv), and v), as follows:
- this substrate 1 In order to preserve the transparent nature of the electrode, this substrate 1 must be transparent. It can be flexible or rigid and advantageously chosen from glass in the case where it must be rigid, or else chosen from transparent flexible polymers such as polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polyethersulfone (PES) , polycarbonate (PC), polysulfone (PSU), phenolic resins, epoxy resins, polyester resins, polyimide resins, polyether ester resins, polyether amide resins, polyvinyl acetate, cellulose nitrate, cellulose acetate, polystyrene, polyolefins, polyamide, aliphatic polyurethanes, polyacrylonitrile, polytetrafluoroethylene (PTFS), polymethyl methacrylate (PMMA), polyarylate, polyetherimides, polyether ketones (PEK), polyether ether ketones (PEEK) and polyvinylidene fluoride (PVDF), the
- the substrate 1 is covered with an adhesion layer 2.
- This adhesion layer 2 is intended to improve the adhesion between the substrate 1 and the upper layer to said layer of adhesive. accession 2.
- This adhesion layer 2 is also transparent in order to maintain a high transmittance and sufficiently resistant to the application of the overlying layer, especially if this application involves solvents.
- the adhesion layer 2 may be, especially if the substrate is flexible, also made of a flexible material, for example nitrile rubber (NBR), styrene-butadiene rubber (SBR), natural rubber (NR) or dissolutions polymers or other latices such as polyvinyl acetate (PVA), polyurethane (PU) or polyvinyl pyrrolidone (PVP).
- NBR nitrile rubber
- SBR styrene-butadiene rubber
- NR natural rubber
- dissolutions polymers or other latices such as polyvinyl acetate (PVA), polyurethane (PU) or polyvinyl pyrrolidone (PVP).
- the adhesion layer 2 may be deposited on the substrate 1, according to any method known to those skilled in the art, the most used techniques being spray coating, inkjet deposition, the deposit dip coating, spin-coater deposition, impregnation deposition, slot-die deposition, doctor blade deposition, or flexo-etching. This deposit being followed by a drying and crosslinking phase of said adhesion layer 2.
- a suspension of metal nanofilaments 3 is applied to the adhesion layer 2.
- metal nanofilaments 3 are previously dispersed in an easily evaporable organic solvent (for example ethanol) or else dispersed in an aqueous medium in the presence of a surfactant (preferably an ionic conductor). It is this suspension of metal nanofilaments 3 in a solvent which is applied on the adhesion layer 2.
- an easily evaporable organic solvent for example ethanol
- a surfactant preferably an ionic conductor
- the metal nanofilaments 3 may consist of noble metals, such as silver, gold or platinum.
- the metal nanofilaments 3 may also consist of non-noble metals, such as for example copper, iron or nickel.
- the suspension of metal nanofilaments 3 can be deposited on the substrate 1, according to any method known to those skilled in the art, the most used techniques being the spray coating, inkjet deposition, dip coating, film pulling, spin-coater deposition, impregnation deposition, slot-die deposition, doctor blade deposition, or flexo-etching .
- the solvents of the metal nanofilament suspension 3 are evaporated to form a network. percolating metallic nanofilaments 3 allowing the passage of the current.
- the quality of the dispersion of the metal nanofilaments 3 in the suspension conditions the quality of the network formed after evaporation.
- the concentration of the dispersion can be between 0.01 wt% and 10 wt%, preferably between 0.1 wt% and 2 wt%, in the case of a percolating network made in a single pass.
- the quality of the network formed after evaporation is also defined by the density of metal nanofilaments 3 present in the network, this density being between 0.01ug / cm 2 and 1mg / cm 2 , preferably between 0.01ug / cm 2 and 10ug / cm. 2 .
- the final network may consist of several layers of metal nanofilaments 3 superimposed. For this, simply repeat steps iii) and iv) as many times as it is desired to obtain metal nanofilament layers 3.
- the network of metal nanofilaments 3 may comprise from 1 to 800 superimposed layers, preferably less than 100 layers, with a dispersion of metallic nanofilaments 3 at 0.1 wt%.
- FIG. 4 shows a photograph taken under an electron microscope of a multilayer conductive transparent electrode at the end of the preceding steps.
- the multilayer conductive transparent electrode here comprises a substrate layer 1, an adhesion layer 2 of nitrile rubber and a network of metal nanofilaments 3 formed of 15 layers.
- composition forming the electric homogenization layer 4 comprises:
- nano-conductive or semi-conductive fillers in one or two dimensions dispersed or suspended in water and / or in a solvent, said fillers preferably having a form factor (length / diameter ratio)> 10 .
- the electric homogenization layer 4 can also comprise:
- cross-linked or non-crosslinked polymer particles selected from functionalized or non-functionalized particles of polystyrene, polycarbonate, polymethylenemelamine, said non-crosslinked polymer particles having a glass transition temperature Tg> 80 ° C, glass particles , silica particles, and / or metal oxide particles selected from the following metal oxides: ZnO, MgO, MgAl 2 0 4 , the borosilicate particles, said particles (d) may be in the form of of powder, either as a dispersion in water and / or in a solvent.
- composition forming the electric homogenization layer 4 may comprise each of the constituents (a), (b), (c) and (d) in the proportions by weight (for a total of 100% by weight) of:
- the composition forming the electrical homogenization layer 4 comprises at least one dispersion or suspension (a) of elastomer, said elastomer preferably being chosen from polybutadiene, polyisoprene, acrylic polymers, polychloroprene , the latter possibly being a sulphonated polychloroprene, polyurethane, terpolymers hexafluoropropene / difluoropropene / tetraflu
- the composition forming the electrical homogenization layer 4 can comprise at least one dispersion or suspension (a) of thermoplastic polymer, said thermoplastic polymer being chosen from polyesters, polyamides, polypropylene, polyethylenes , chlorinated polymers such as polyvinyl chloride and vinylidene, fluorinated polymers such as polyvinylidene fluoride (PVDF), polyacetates, polycarbonates, poly (ethers ether ketones) (PEEK), polysulfides, ethylene copolymers / vinyl acetate.
- thermoplastic polymer being chosen from polyesters, polyamides, polypropylene, polyethylenes , chlorinated polymers such as polyvinyl chloride and vinylidene, fluorinated polymers such as polyvinylidene fluoride (PVDF), polyacetates, polycarbonates, poly (ethers ether ketones) (PEEK), polysulfides, ethylene copolymers / vinyl acetate.
- the composition forming the electrical homogenization layer 4 may comprise at least one polymer dissolution (a), said polymer being chosen from polyvinyl alcohols (PVOH), vinyl polyacetates (PVA), polyvinyl pyrrolidones (PVP), polyethylene glycols.
- a polymer dissolution
- said polymer being chosen from polyvinyl alcohols (PVOH), vinyl polyacetates (PVA), polyvinyl pyrrolidones (PVP), polyethylene glycols.
- Said elastomer and / or said thermoplastic polymer are used in the form of a dispersion or a suspension in water and / or in a solvent, said solvent preferably being an organic solvent chosen from dimethylsulfoxide (DMSO), N-methyl-2-pyrrolidone (NMP), ethylene glycol, tetrahydrofuran (THF), dimethylacetate (DMAc) or dimethylformamide (DMF).
- DMSO dimethylsulfoxide
- NMP N-methyl-2-pyrrolidone
- THF tetrahydrofuran
- DMAc dimethylacetate
- DMF dimethylformamide
- the elastomer and / or the thermoplastic polymer are dispersed or suspended in water.
- the conductive polymer (b) is a polythiophene, the latter being one of the most thermally and electronically stable polymers.
- a preferred conductive polymer is poly (3,4-ethylenedioxythiophene) -poly (styrenesulfonate) (PEDOT: PSS), the latter being stable to light and heat, easy to disperse in water, and free of water. environmental disadvantages.
- the conductive polymer (b) may be in the form of granules, a dispersion or a suspension in water and / or in a solvent, said solvent preferably being a polar organic solvent chosen from dimethylsulfoxide (DMSO ), N-methyl-2-pyrrolidone (NMP), ethylene glycol, tetrahydrofuran (THF), dimethylacetate (DMAc), dimethylformamide (DMF), the conductive polymer (b) being preferably in dispersion or in suspended in water, dimethylsulfoxide (DMSO) or ethylene glycol.
- DMSO dimethylsulfoxide
- NMP N-methyl-2-pyrrolidone
- THF tetrahydrofuran
- DMAc dimethylacetate
- DMF dimethylformamide
- the conductive polymer (b) being preferably in dispersion or in suspended in water, dimethylsulfoxide (DMSO) or ethylene glycol.
- Organic compounds also called “conductivity enhancers", the latter to improve conductivity electrically conductive polymer, can also be added to the composition forming the electric homogenization layer 4. These compounds may in particular be carrying dihydroxy, polyhydroxy, carboxylic, amide and / or lactam functions, such as the compounds mentioned in the US patents 5,766,515 and US 6,984,341, which are here incorporated by reference.
- the most preferred organic compounds or “conductivity enhancers” are DMSO (dimethyl sulfoxide), sorbitol, ethylene glycol and glycerine.
- the fillers (c) may be conductive fillers chosen from nanoparticles and / or nanofilaments of silver, gold, platinum and / or ITO (Indium Tin Oxide), and / or selected semi-conductive fillers. among carbon nanotubes and nanoparticles based on graphene.
- the fillers (c) are carbon nanotubes dispersed in water and / or in a solvent chosen from the following polar organic solvents: dimethylsulfoxide (DMSO), N-methyl-2 pyrrolidone (NMP), ethylene glycol, dimethylacetate (DMAc), dimethylformamide (DMF), acetone and alcohols such as methanol, ethanol, butanol and isopropanol, or a mixture thereof solvents.
- DMSO dimethylsulfoxide
- NMP N-methyl-2 pyrrolidone
- DMAc dimethylacetate
- DMF dimethylformamide
- acetone and alcohols such as methanol, ethanol, butanol and isopropanol, or a mixture thereof solvents.
- the crosslinked or non-crosslinked polymer particles (d) have an average diameter of between 30 and 1000 nm, and even more preferably are chosen from polystyrene particles having a mean diameter of between 30 and 1000 nm.
- the size distribution of these polymer particles may be multimodal, and preferably bimodal.
- Said polymer particles (d) may be used in the form of a powder, or a dispersion or a suspension in water and / or in a solvent chosen from the following polar organic solvents: dimethylsulfoxide (DMSO), N-methyl-2-pyrrolidone (NMP), ethylene glycol, dimethylacetate (DMAc), dimethylformamide (DMF), acetone and alcohols such as methanol, ethanol, butanol and isopropanol , or a mixture of these solvents.
- DMSO dimethylsulfoxide
- NMP N-methyl-2-pyrrolidone
- DMAc dimethylacetate
- DMF dimethylformamide
- alcohols such as methanol, ethanol, butanol and isopropanol , or a mixture of these solvents.
- the ratio by weight between the elastomer and / or the thermoplastic polymer and / or the polymer (a) and the particles (d) may be between 0.1 and 10,000, and preferably between 1 and 1000.
- the ratio by weight between the conductive polymer (b) and the particles (d) can, for its part, be between 0.01 and 10,000, and preferably between 0.1 and 500.
- this ratio can be between 1 and 1000, and preferably between 50 and 500. All the mass ratios indicated are given by weight of dry matter.
- Additives such as ionic or nonionic surfactants, wetting agents, rheological agents, such as thickening agents or fluidifying agents, adhesion promoters, dyes, crosslinking agents, may also be added to the composition. of the invention, to improve or modify the performance according to the intended end application.
- the electric homogenization layer 4 can be deposited on a support, according to any method known to those skilled in the art, the most used techniques being the spray coating, inkjet deposition, dip coating, film pulling, spin-coater deposition, impregnation deposition, slot-die depositing, doctor blade deposition, or flexogravure, so as to obtain a film whose thickness can be between 50 nm and 15 ⁇ . vi) Evaporation of the solvents of the composition forming the electric homogenization layer 4.
- this drying is carried out at a temperature of between 25 and 80 ° C., said drying temperature necessarily having to be, when the polymer particles (d) are non-crosslinked polymer particles, being less than the glass transition temperature Tg of said uncrosslinked polymer particles contained in the composition applied in the previous step.
- the electric homogenization layer 4 is also crosslinked during this step, for example by vulcanization at a temperature of 150 ° C. for a period of 5 minutes.
- FIG. 5 shows a photograph taken with a scanning electron microscope of a multilayer conductive transparent electrode at the end of the preceding steps.
- the multilayer conductive transparent electrode therefore comprises a substrate layer 1, an adhesion layer 2 of nitrile rubber and a network of metal nanofilaments 3 formed of 15 layers and an electric homogenization layer 4.
- Another object of the invention is therefore also a multilayer conductive transparent electrode.
- This type of electrode preferably having a thickness of between 0.5 ⁇ and 20 ⁇ .
- This multilayer conductive transparent electrode is represented in FIGS. 2, 3 and 5 and comprises a substrate layer 1, an adhesion layer 2, a metal nanofilament network 3, an electrical homogenization layer 4, said electric homogenization layer 4 comprising:
- the electric homogenization layer 4 can also comprise crosslinked or non-crosslinked polymer particles chosen from functionalized or non-functionalized particles of polystyrene, polycarbonate and polymethylenemelamine, said non-crosslinked polymer particles having a glass transition temperature Tg higher than 80 ° C, glass particles, silica particles, and / or metal oxide particles selected from the following metal oxides: ZnO, MgO, MGA1 2 0 4 , borosilicate particles.
- This multilayer conductive transparent electrode in particular derived from the manufacturing process described above, thus has a high transmittance, a low surface electrical resistance and a low roughness of less than 100 nm.
- the devices are generally multilayer devices.
- the multilayer conductive transparent electrode according to the invention composes one of these extremely thin layers.
- it is essential to have the lowest possible roughness.
- the substrate layer 1 in order to preserve the transparent nature of the electrode, must be transparent.
- Said substrate layer 1 may be flexible or rigid and advantageously chosen from glass in the case where it must be rigid, or else chosen from transparent flexible polymers such as polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polyethersulfone (PES), polycarbonate (PC), polysulfone (PSU), phenolic resins, epoxies, polyesters, polyimides, polyetheresters, polyetheramides, polyvinyl (acetate), cellulose nitrate, cellulose acetate, polystyrene , polyolefins, polyamide, aliphatic polyurethanes, polyacrylonitrile, polytetrafluoroethylene (PTFS), polymethyl methacrylate (PMMA), polyarylate, polyetherimides, polyether ketones (PEK), polyether ether ketones (PEEK) and polyfluoride vinylidene (PVDF), the most preferred
- the adhesion layer 2 is also transparent in order to maintain a high transmittance and sufficiently resistant to the application of the overlying layer, especially if this application involves solvents.
- the adhesion layer 2 may be, especially if the substrate is flexible, also made of a flexible material, for example nitrile rubber (NBR).
- NBR nitrile rubber
- the network of metal nanofilaments 3 may be made of noble metals, such as silver, gold or platinum. It may also consist of non-noble metals, such as copper, iron or nickel.
- the network of metal nanofilaments 3 may consist of one or more layers of superimposed metallic nanofilaments 3 thus forming a conductive percolating network and having a metal nanofilament density of between 0.01 ⁇ g / cm 2 and 1 mg / cm 2 .
- the elastomer that may be contained in the electrical homogenization layer 4 is preferably chosen from polybutadiene, polyisoprene, acrylic polymers, polychloroprene, the latter possibly being a sulphonated polychloroprene, polyurethane, terpolymers hexafluoropropene / difluoropropene / tetrafluoroethylene, copolymers based on chlorobutadiene and methacrylic acid or based on ethylene and vinyl acetate, copolymers SBR (Styrene Butadiene Rubber), SBS (Styrene Butadiene Styrene), SIS (Styrene Isoprene Styrene) and SEBS (Styrene Ethylene Butylene Styrene), isobutylene / isoprene copolymers, butadiene / acrylonitrile copolymers, butadiene / acryl
- the elastomer is chosen from acrylic polymers, polychloroprene, SBR copolymers and butadiene / acrylonitrile copolymers.
- the electric homogenization layer 4 may comprise at least one thermoplastic polymer, said thermoplastic polymer being chosen from polyesters, polyamides, polypropylene, polyethylene, chlorinated polymers such as polyvinyl chlorides and vinylidene, fluorinated polymers such as polyvinylidene fluoride (PVDF), polyacetates, polycarbonates, polyether ether ketones (PEEK), polysulfides, ethylene / vinyl acetate copolymers.
- PVDF polyvinylidene fluoride
- PVDF polyacetates
- polycarbonates polyether ether ketones
- PEEK polyether ether ketones
- the electric homogenization layer 4 can comprise at least one polymer, said polymer being chosen from polyvinyl alcohols (PVOH), vinyl polyacetates (PVA), polyvinyl pyrrolidones (PVP), polyethylene glycols .
- PVOH polyvinyl alcohols
- PVA vinyl polyacetates
- PVP polyvinyl pyrrolidones
- polyethylene glycols polyethylene glycols
- the conductive polymer that may be contained in the electric homogenization layer 4 is preferably a polythiophene, the latter being one of the most thermally and electronically stable polymers.
- a preferred conductive polymer is poly (3,4-ethylenedioxythiophene) -poly (styrenesulfonate) (PEDOT: PSS), the latter being stable to light and heat, easy to disperse in water, and free of water. environmental disadvantages.
- Organic compounds also known as "conductivity enhancers", the latter making it possible to improve the electrical conductivity of the conducting polymer, can also be included in the electric homogenization layer 4. These compounds can in particular be carrying dihydroxy, polyhydroxy, carboxylic, amide and / or lactam, such as the compounds mentioned in US Pat. Nos. 5,766,515 and 6,984,341, which are here incorporated by reference.
- the most preferred organic compounds or “conductivity enhancers” are sorbitol, ethylene glycol, glycerin or DMSO (dimethyl tallow oxide).
- the crosslinked or non-crosslinked polymer particles that may be contained in the electrical homogenization layer 4 preferably have a mean diameter of between 30 and 1000 nm, and even more preferably are chosen from polystyrene particles having an average diameter of between 30 and 1000 nm.
- the size distribution of these polymer particles may be multimodal, and preferably bimodal.
- the conductive fillers that may be contained in the electrical homogenization layer 4 are preferably chosen from nanoparticles and / or nanofilaments of silver, gold, platinum and / or ITO (Indium Tin Oxide), and or semiconductor charges selected from carbon nanotubes and nanoparticles based on graphene.
- the ratio by weight between the elastomer and / or the thermoplastic polymer and / or the polymer and the particles may be between 0.1 and 10,000, and preferably between 1 and 1000.
- the ratio by weight between the conductive polymer and the As regards the weight ratio between the elastomer and / or the thermoplastic polymer and / or the polymer, the particle size may be between 0.01 and 10,000, and preferably between 0.1 and 500.
- this ratio can be between 1 and 1000, and preferably between 50 and 500. All the weight ratios indicated are given by weight of dry matter.
- the following experimental results show values obtained by a multilayer conductive transparent electrode according to the invention, for essential parameters such as the transmittance at the wavelength 550 nm T 550 , the average transmittance T av , the surface electrical resistance R as well as the density of metallic nanofilaments.
- the different layers were all applied by a similar method of spin coating.
- the total transmittance ie the light intensity passing through the film on the visible spectrum, is measured on 50 x 50 mm experiments using a Perkin Elmer Lambda 35 spectrophotometer on a UV spectrum. -visible [300 nm - 900 nm].
- the mean transmittance value T av on all the sp A of the visible this value corresponding to the average value of the transmittances on the visible spectrum. This value is measured every 10 nm. Measurement of surface electrical resistance.
- the surface electrical resistance (in ⁇ / D) can be defined by the following formula: p 1
- the average roughness Rq is measured using an atomic force microscope (AFM) (Digital Instrument Dimension 3100) in tapping mode on 50 x 50 mm probes.
- AFM atomic force microscope
- the measurements are performed twice on each test piece.
- the density of nanofilaments is determined by image analysis from images obtained after observation of the specimens using a scanning electron microscope (Supra 35 ⁇ field emission, Zeiss). The overall area of the photographs is 78506 ⁇ m 2 (28kV acceleration voltage, 60 ⁇ diaphragm, 1000x magnification). Chemical contrast image processing with Visilog ⁇ software (version 6.9) is performed on 10 images per test specimen. The characterization is done according to two algorithms known as "maximal” and "minimal”.
- the density of nanofilaments is defined by the following formula:
- NBR nitrile rubber
- PVP poly (vinylpyrrolidone)
- PVA polyvinyl alcohol
- NWs network of metallic nanofilaments
- PEDOT PSS: polythipohene (conductive polymer)
- TCO Hutchinson ⁇ electric homogenization layer according to the invention.
- an electrode according to the invention comprising only a single layer of metallic nanofilaments with a high transmittance, greater than 75% for the T 550 and 75% for the T av , as well as an electrical resistance of surface R less than 1000 ⁇ / D, of the order of 776 ⁇ / D.
- the surface electrical resistance R of the conductive multilayer transparent electrode according to the invention are much better than those of the prior art.
- the electric homogenization layer does not cause a significant increase in the surface electrical resistance, particularly because of the oxidation of metal nanofilaments by encapsulation with a single layer of PEDOT: PSS.
- TCO Hutchinson ⁇ an electric homogenization layer according to the invention, TCO Hutchinson ⁇ . Number of Density of Ag nanofilaments layers of TR (Ug / cm 2 )
- This example corresponds to a multilayer conductive transparent electrode according to the state of the art, without electric homogenization layer 4.
- composition A is prepared as follows:
- the properties of the transparent and conductive electrode are as follows:
- This example corresponds to a multilayer conductive transparent electrode according to the invention, with electric homogenization layer 4.
- composition B is prepared as follows:
- nitrile rubber NBR Nitrile Butadiene Rubber
- Synthomer, 5130 ® self-crosslinking and previously diluted to 15% with deionized water, is deposited on a PET planarized plastic substrate (Dupont de Nemour, ST504) using a spin coater (SPS, SPIN 150), according to the following parameters: acceleration 200 rpm, speed 2000 rpm for 100s. The latex film is then vulcanized at 150 ° C. for 5 min using an oven.
- SPS spin coater
- the mixture is then applied to the percolating network of silver nanofilaments using spin coater SPIN 150 (acceleration: 500 rpm, speed 5000 rpm, time 100s).
- the latter is vulcanized at 150 ° C. for a period of 5 minutes.
- the properties of the transparent and conductive electrode are as follows:
- composition C is prepared as follows:
- nitrile rubber NBR Nirile Butadiene Rubber, Synthomer, 5130 ®
- self-crosslinking and pre-diluted to 15% with déionizé water is deposited on a plastic substrate planarized PET (Dupont de Nemour, ST504) by using a spin coater (SPS, SPIN 150), according to the following parameters: acceleration 200 rpm, speed 2000 rpm for 100s.
- SPS spin coater
- the latex film is then vulcanized at 150 ° C. for 5 min using an oven.
- 8.5 mg of carbon nanotubes MWNTs Graphistrenght U100 3 ⁇ 4 are dispersed in 14.17 g of a dispersion of PEDOT: PSS Clevios PH500 3 ⁇ 4 having a solids content of 1.2% and 17.00 g of DMSO in using a high shear mixer (Siverson L5M) at a speed of 8000 rpm for 2 hours.
- PEDOT: PSS Clevios PH500 3 ⁇ 4 having a solids content of 1.2% and 17.00 g of DMSO in using a high shear mixer (Siverson L5M) at a speed of 8000 rpm for 2 hours.
- a high shear mixer Siverson L5M
- the mixture is then applied to the percolating network of silver nanofibers using spin coater SPIN 150 (acceleration: 500 rpm, speed 5000 rpm, time 100s).
- the latter is vulcanized at 150 ° C. for a period of 5 minutes.
- the properties of the transparent and conductive electrode are as follows:
- the multilayer conductive transparent electrode according to the invention thus makes it possible, thanks to the presence of the electric homogenization layer, to protect the conducting network of metallic nanofilaments without damaging it, thereby lengthening the service life and the durability of the 'electrode.
- this electric homogenization layer allows a homogenization of the surface conductivity and a reduction in roughness, thereby increasing the performance of the multilayer conductive transparent electrode.
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- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Nanotechnology (AREA)
- Power Engineering (AREA)
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- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Optics & Photonics (AREA)
- Crystallography & Structural Chemistry (AREA)
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Abstract
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR1102113A FR2977712A1 (fr) | 2011-07-05 | 2011-07-05 | Electrode transparente conductrice multicouche et procede de fabrication associe |
FR1102255A FR2977713B1 (fr) | 2011-07-05 | 2011-07-19 | Electrode transparente conductrice multicouche et procede de fabrication associe |
PCT/EP2012/062853 WO2013004667A1 (fr) | 2011-07-05 | 2012-07-02 | Electrode transparente conductrice multicouche et procédé de fabrication associé |
Publications (1)
Publication Number | Publication Date |
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EP2729973A1 true EP2729973A1 (fr) | 2014-05-14 |
Family
ID=44681140
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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EP12737735.6A Withdrawn EP2729973A1 (fr) | 2011-07-05 | 2012-07-02 | Electrode transparente conductrice multicouche et procédé de fabrication associé |
Country Status (7)
Country | Link |
---|---|
US (1) | US20140238727A1 (fr) |
EP (1) | EP2729973A1 (fr) |
JP (1) | JP2014526117A (fr) |
KR (1) | KR20140044895A (fr) |
CN (1) | CN103959500A (fr) |
FR (2) | FR2977712A1 (fr) |
WO (1) | WO2013004667A1 (fr) |
Families Citing this family (24)
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US20130309482A1 (en) * | 2010-10-08 | 2013-11-21 | Nitto Denko Corporation | Thermally functional flame-retardant polymer member |
FR2977364B1 (fr) | 2011-07-01 | 2015-02-06 | Hutchinson | Collecteur de courant et procede de fabrication correspondant |
FR2996358B1 (fr) * | 2012-10-03 | 2016-01-08 | Hutchinson | Electrode transparente et procede de fabrication associe |
FR2996359B1 (fr) | 2012-10-03 | 2015-12-11 | Hutchinson | Electrode transparente conductrice et procede de fabrication associe |
CN103971788B (zh) * | 2013-02-04 | 2016-08-31 | 深圳欧菲光科技股份有限公司 | 透明导电体及其制备方法 |
CN103971787B (zh) * | 2013-02-04 | 2016-06-22 | 深圳欧菲光科技股份有限公司 | 透明导电体及其制备方法 |
FR3011973B1 (fr) | 2013-10-10 | 2016-01-01 | Commissariat Energie Atomique | Materiau multicouches comprenant des nanofils metalliques et un polymere non conducteur electriquement |
JP6371861B2 (ja) * | 2014-01-27 | 2018-08-08 | ユッチンソン | 電気エネルギー貯蔵システムのための、保護導電層を含むコレクタを有する電極および対応する製造方法 |
EP3134258A1 (fr) * | 2014-04-22 | 2017-03-01 | SABIC Global Technologies B.V. | Film conducteur transparent souple intégré |
CN106661255A (zh) | 2014-08-07 | 2017-05-10 | 沙特基础工业全球技术有限公司 | 用于热成型应用的导电多层片材 |
CN104485345A (zh) * | 2014-12-15 | 2015-04-01 | 京东方科技集团股份有限公司 | 一种柔性电极结构、其制作方法及柔性显示基板 |
WO2016114279A1 (fr) * | 2015-01-14 | 2016-07-21 | 東洋紡株式会社 | Pâte d'argent électroconductrice |
CN104681645B (zh) * | 2015-01-23 | 2016-09-21 | 华南师范大学 | 一种基于金属网格和金属纳米线制备复合透明导电电极的方法 |
WO2016147481A1 (fr) * | 2015-03-13 | 2016-09-22 | コニカミノルタ株式会社 | Électrode transparente, procédé de fabrication d'électrode transparente, et élément électroluminescent organique |
CN105185432B (zh) * | 2015-10-09 | 2017-10-27 | 重庆文理学院 | 一种多重保护的银纳米线透明导电薄膜 |
CN105185470B (zh) * | 2015-10-09 | 2017-11-17 | 重庆文理学院 | 一种即用即撕的银纳米线透明导电薄膜的制备方法 |
CN106594678B (zh) * | 2016-12-25 | 2019-03-05 | 厦门大学 | 一种金属纳米线的透明薄膜led调光器制备方法 |
CN107731939B (zh) * | 2017-09-22 | 2019-03-08 | 华中科技大学 | 一种基于光衍射的柔性透明碳电极制备方法 |
CN108470598A (zh) * | 2018-04-06 | 2018-08-31 | 天津工业大学 | 柔性透明导电薄膜及其制备方法 |
CN108598288A (zh) * | 2018-07-10 | 2018-09-28 | 上海大学 | 一种复合多功能oled电极及其制备方法 |
CN109950401B (zh) * | 2019-03-25 | 2020-09-22 | 南开大学 | 一种基于金属纳米线和碳化钛纳米片的柔性复合透明电极及其制备方法及用途 |
CN114799190B (zh) * | 2022-06-20 | 2023-04-28 | 杭州电子科技大学富阳电子信息研究院有限公司 | 一种金纳米棒薄膜及其合成方法 |
CN115590521B (zh) * | 2022-12-15 | 2023-03-31 | 季华实验室 | 一种高导电性透气水凝胶干电极及其制造方法 |
CN116583138A (zh) * | 2023-07-10 | 2023-08-11 | 四川京龙光电科技有限公司 | 一种强散热性的可拉伸显示器件及其制备方法 |
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US20110139253A1 (en) * | 2009-12-11 | 2011-06-16 | Konica Minolta Holdings, Inc. | Organic photoelectric conversion element and producing method of the same |
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CN1086929A (zh) * | 1992-09-04 | 1994-05-18 | 单一检索有限公司 | 挠性塑料电极及其制造方法 |
DE19507413A1 (de) | 1994-05-06 | 1995-11-09 | Bayer Ag | Leitfähige Beschichtungen |
US6984341B2 (en) | 2002-01-22 | 2006-01-10 | Elecon, Inc. | Mixtures comprising thiophene/anion dispersions and certain additives for producing coatings exhibiting improved conductivity, and methods related thereto |
WO2008127313A2 (fr) | 2006-11-17 | 2008-10-23 | The Regents Of The University Of California | Réseaux de nanofils électriquement conducteurs et optiquement transparents |
EP2414439B1 (fr) * | 2009-03-31 | 2014-03-26 | Hutchinson | Films ou revetements transparents conducteurs |
GB0908300D0 (en) * | 2009-05-14 | 2009-06-24 | Dupont Teijin Films Us Ltd | Polyester films |
JP5391932B2 (ja) * | 2009-08-31 | 2014-01-15 | コニカミノルタ株式会社 | 透明電極、透明電極の製造方法、および有機エレクトロルミネッセンス素子 |
CN102087886A (zh) * | 2009-12-08 | 2011-06-08 | 中国科学院福建物质结构研究所 | 基于银纳米线的透明导电薄膜及其制备方法 |
CN102087885A (zh) * | 2009-12-08 | 2011-06-08 | 中国科学院福建物质结构研究所 | 平坦化的银纳米线透明导电薄膜及其制备方法 |
-
2011
- 2011-07-05 FR FR1102113A patent/FR2977712A1/fr not_active Withdrawn
- 2011-07-19 FR FR1102255A patent/FR2977713B1/fr not_active Expired - Fee Related
-
2012
- 2012-07-02 CN CN201280043100.1A patent/CN103959500A/zh active Pending
- 2012-07-02 WO PCT/EP2012/062853 patent/WO2013004667A1/fr active Application Filing
- 2012-07-02 US US14/130,156 patent/US20140238727A1/en not_active Abandoned
- 2012-07-02 EP EP12737735.6A patent/EP2729973A1/fr not_active Withdrawn
- 2012-07-02 KR KR1020147003061A patent/KR20140044895A/ko not_active Application Discontinuation
- 2012-07-02 JP JP2014517763A patent/JP2014526117A/ja not_active Withdrawn
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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US20110139253A1 (en) * | 2009-12-11 | 2011-06-16 | Konica Minolta Holdings, Inc. | Organic photoelectric conversion element and producing method of the same |
Also Published As
Publication number | Publication date |
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KR20140044895A (ko) | 2014-04-15 |
CN103959500A (zh) | 2014-07-30 |
WO2013004667A1 (fr) | 2013-01-10 |
FR2977713A1 (fr) | 2013-01-11 |
FR2977712A1 (fr) | 2013-01-11 |
FR2977713B1 (fr) | 2013-08-16 |
US20140238727A1 (en) | 2014-08-28 |
JP2014526117A (ja) | 2014-10-02 |
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