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WO2010082428A1 - Électrode transparente, son procédé de production et élément électroluminescent organique - Google Patents

Électrode transparente, son procédé de production et élément électroluminescent organique Download PDF

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Publication number
WO2010082428A1
WO2010082428A1 PCT/JP2009/071121 JP2009071121W WO2010082428A1 WO 2010082428 A1 WO2010082428 A1 WO 2010082428A1 JP 2009071121 W JP2009071121 W JP 2009071121W WO 2010082428 A1 WO2010082428 A1 WO 2010082428A1
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WIPO (PCT)
Prior art keywords
transparent electrode
layer
metal nanowire
metal
conductive
Prior art date
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Ceased
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PCT/JP2009/071121
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English (en)
Japanese (ja)
Inventor
竹田　昭彦
昌紀 後藤
中村　和明
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Konica Minolta Inc
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Konica Minolta Inc
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Application filed by Konica Minolta Inc filed Critical Konica Minolta Inc
Priority to JP2010546570A priority Critical patent/JP5533669B2/ja
Publication of WO2010082428A1 publication Critical patent/WO2010082428A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • H10K30/821—Transparent electrodes, e.g. indium tin oxide [ITO] electrodes comprising carbon nanotubes
    • 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
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/80—Constructional details
    • H10K50/805—Electrodes
    • H10K50/81—Anodes
    • H10K50/816—Multilayers, e.g. transparent multilayers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the present invention relates to a transparent electrode, a method for producing the same, and an organic electroluminescent element, and more specifically, relates to a transparent electrode formed by coating without complicated processes, a method for producing the same, and an organic electroluminescent element.
  • organic EL organic electroluminescence
  • field emission field emission
  • the transparent electrode is an essential constituent technology.
  • transparent electrodes are an indispensable technical element in touch panels, mobile phones, electronic paper, various solar cells, and various electroluminescence light control elements.
  • various metal thin films such as Au, Ag, Pt, Cu, indium oxide doped with tin or zinc (ITO, IZO), zinc oxide doped with aluminum or gallium (AZO, GZO), fluorine, Metal oxide thin films such as tin oxide doped with antimony (FTO, ATO), conductive nitride thin films such as TiN, ZrN, and HfN, and conductive boride thin films such as LaB 6 are known and combinations thereof.
  • Various electrodes such as Bi 2 O 3 / Au / Bi 2 O 3 and TiO 2 / Ag / TiO 2 are also known.
  • transparent electrodes using CNTs (carbon nanotubes) and conductive polymers have also been proposed (see, for example, Non-Patent Document 1).
  • the metal thin film, nitride thin film, boron thin film and conductive polymer thin film described above cannot have both light transmission properties and conductive properties, special technical fields such as electromagnetic shielding and the like are relatively high. It was used only in the touch panel field where resistance values are allowed.
  • ITO is widely used as a transparent electrode for various optoelectronics because it has a good balance between light transmittance and conductivity and it is easy to form an electrode fine pattern by wet etching using an acid solution.
  • the conductive oxide typified by the above-mentioned ITO or the like forms a transparent conductive film on the substrate surface by a vacuum process such as a sputtering method or a liquid phase method such as a sol-gel method. In order to form a transparent conductive film by a vacuum process such as sputtering, expensive equipment is required.
  • Patent Document 1 a method of forming a transparent conductive film by applying a conductive oxide or a composition containing a conductive polymer has been proposed (for example, Patent Document 1). 2).
  • Other transparent electrodes include a transparent electrode in which a mesh structure is formed by a metal pattern typified by an electromagnetic wave shielding film of a plasma display (for example, Patent Document 3), and a transparent electrode composed of a fine mesh using metal nanowires.
  • An electrode is disclosed (for example, Patent Document 4).
  • a metal mesh using silver both good conductivity and transparency can be achieved due to the inherent high conductivity of silver.
  • these transparent electrodes have a defect that the electrode surface is rough as compared with the above-mentioned electrodes such as ITO.
  • the transparent electrode is required to have excellent surface smoothness, and such an electrode with low surface smoothness causes luminance unevenness or the like. This causes a decrease in the function of the element.
  • Patent Document 4 In order to improve the surface smoothness of the transparent electrode, a method of forming a conductive layer using a metal nanowire on a highly smooth support and transferring it to another support has been proposed (Patent Document 4). It is difficult to adjust the balance between the adhesive used for transfer and the adhesion between the support and the conductive layer and the peelability, and complete transfer is difficult. Furthermore, there are many steps of applying and curing the adhesive layer, laminating and peeling the supports, peeling, and processes, and there is a problem of cost increase. Further, a method for directly forming the conductive layer pattern by a printing method is not described in detail.
  • JP 2008-95015 A Japanese Patent Laid-Open No. 2008-4501 JP 2004-221564 A US Patent Application Publication No. 2007 / 0074316A1
  • An object of the present invention is made in view of the above circumstances, and is to provide a transparent electrode excellent in surface smoothness, conductivity, and transparency, and having high productivity, and a method for producing the same.
  • an object of the present invention is to provide an organic electroluminescence device with less luminance unevenness by using the transparent electrode manufactured in this way.
  • a transparent electrode having a conductive layer composed of a metal nanowire layer and a conductive polymer layer on a transparent support, a cross-linked product of a water-soluble polymer, a cross-linked product of a polymer latex, and a curable resin in the metal nanowire layer
  • a transparent electrode comprising at least one selected from the cured products.
  • the water-soluble polymer cross-linked product or polymer latex cross-linked product is cross-linked with at least one cross-linking agent selected from aldehyde, melamine, epoxy, and isocyanate cross-linking agents.
  • An organic electroluminescence device comprising the transparent electrode according to any one of 1 to 4 above.
  • a transparent electrode having surface smoothness, conductivity, and transparency. Furthermore, by using silver nanowires as metal nanowires, both conductivity and transparency are achieved.
  • a transparent electrode can be provided.
  • the transparent electrode of the present invention as the electrode of the organic electroluminescence element, it was possible to provide an organic electroluminescence element with little uneven emission luminance.
  • a plastic film, a plastic plate, glass or the like can be used as the transparent support.
  • polyesters such as polyethylene terephthalate (PET) and polyethylene naphthalate
  • polyolefins such as polyethylene (PE), polypropylene (PP), polystyrene, and EVA
  • polyvinyl chloride and polychlorinated chloride.
  • vinyl resins such as vinylidene, polyether ether ketone (PEEK), polysulfone (PSF), polyether sulfone (PES), polycarbonate (PC), polyamide, polyimide, acrylic resin, triacetyl cellulose (TAC), etc. Can do.
  • the support is preferably excellent in surface smoothness.
  • the smoothness of the surface is preferably an arithmetic average roughness Ra of 5 nm or less and a maximum height Rz of 50 nm or less, more preferably Ra of 2 nm or less and Rz of 30 nm or less, and still more preferably Ra of 1 nm or less. Rz is 20 nm or less.
  • the surface of the support may be smoothed by applying an undercoat layer such as a thermosetting resin, an ultraviolet curable resin, an electron beam curable resin, or a radiation curable resin, or may be smoothed by mechanical processing such as polishing. You can also.
  • a surface treatment using corona or plasma, or an easy adhesion layer may be formed.
  • the smoothness of the surface can be determined according to a surface roughness standard (JIS B 0601-2001) from measurement using an atomic force microscope (AFM) or the like.
  • a gas barrier layer for the purpose of blocking oxygen and moisture in the atmosphere.
  • metal oxides such as silicon oxide, silicon nitride, silicon oxynitride, aluminum nitride, and aluminum oxide, and metal nitrides can be used. These materials have an oxygen barrier function in addition to a water vapor barrier function.
  • silicon nitride and silicon oxynitride having favorable barrier properties, solvent resistance, and transparency are preferable.
  • the barrier layer may have a multilayer structure as necessary.
  • a resistance heating vapor deposition method As a method for forming the gas barrier layer, a resistance heating vapor deposition method, an electron beam vapor deposition method, a reactive vapor deposition method, an ion plating method, or a sputtering method can be used depending on the material.
  • each inorganic layer constituting the gas barrier layer is not particularly limited, but typically it is preferably in the range of 5 nm to 500 nm per layer, and more preferably 10 nm to 200 nm per layer.
  • the gas barrier layer is provided on at least one surface of the support, and more preferably on both surfaces.
  • the conductive layer in the present invention is composed of a metal nanowire layer and a conductive polymer layer, and the conductive polymer layer may be in contact with the surface of the metal nanowire layer or may be impregnated inside.
  • the method for forming these conductive layers is not particularly limited as long as it is a liquid phase film forming method in which a dispersion containing metal nanowires and a conductive polymer is applied and dried to form a film.
  • Application methods such as dip coating, spin coating, casting, die coating, blade coating, bar coating, gravure coating, curtain coating, spray coating, and doctor coating can be used.
  • direct pattern formation may be performed by an inkjet printing method, gravure, screen printing method, or the like, and printing may be performed a plurality of times depending on the concentration of the dispersion and the target coating amount.
  • the metal nanowire layer according to the present invention is formed by applying and drying a dispersion containing a metal nanowire and a water-soluble polymer or polymer latex or a curable resin as a binder. Further, the water-soluble polymer or polymer latex that is a binder is crosslinked by a crosslinking agent described later, and the curable resin is cured and fixed by heat, light, electron beam, or radiation. Thereby, the applicability
  • stabilizers such as plasticizers, antioxidants and antisulfurizing agents, surfactants, dissolution accelerators, polymerization inhibitors, and colorants such as dyes and pigments
  • solvents for example, water, organic solvents such as alcohols, glycols, cellosolves, ketones, esters, ethers, amides, hydrocarbons, etc.
  • solvents for example, water, organic solvents such as alcohols, glycols, cellosolves, ketones, esters, ethers, amides, hydrocarbons, etc.
  • the dispersion containing metal nanowires may contain a conductive polymer.
  • water-soluble polymer examples include natural polymers such as starch, gelatin, and agar.
  • Semi-synthetic polymers such as carboxymethyl cellulose (CMC), hydroxyethyl cellulose (HEC), methyl cellulose (MC), and hydroxyethyl methyl cellulose (HEMC).
  • Cellulose derivatives such as hydroxypropylmethylcellulose (HPMC), synthetic polymer polyvinyl alcohol (PVA), polyacrylic acid polymer, polyacrylamide (PAM), polyethylene oxide (PEO), polyvinylpyrrolidone (PVP), etc.
  • HPMC hydroxypropylmethylcellulose
  • PVA synthetic polymer polyvinyl alcohol
  • PAM polyacrylamide
  • PEO polyethylene oxide
  • PVP polyvinylpyrrolidone
  • a part of the functional group may be modified.
  • a cellulose derivative and polyvinyl alcohol are preferable.
  • polymer latex examples include acrylic resins (acrylic silicon-modified resins, fluorine-modified acrylic resins, urethane-modified acrylic resins, epoxy-modified acrylic resins, etc.), polyester resins, polyurethane resins, vinyl acetate resins, and the like. Can be widely selected and used.
  • the curable resin according to the present invention may be an aqueous curable resin that is cured by heat, light, electron beam, or radiation.
  • silicone such as melamine acrylate, urethane acrylate, epoxy resin, polyimide resin, acrylic-modified silicate, etc. Resin or the like can be used.
  • the conductive polymer layer according to the present invention is formed by applying a metal nanowire layer and then crosslinking or curing the binder of the metal nanowire layer, and then applying and drying a dispersion containing the conductive polymer. .
  • the conductive polymer layer may be a single conductive polymer or a mixture of plural types of conductive polymers.
  • a non-conductive polymer and an additive may be included as long as both conductivity and transparency can be achieved.
  • non-conductive polymer a wide variety of natural polymer resins or synthetic polymer resins can be used.
  • a transparent thermoplastic resin for example, polyvinyl chloride, vinyl chloride-vinyl acetate copolymer, polymethyl methacrylate, nitrocellulose, chlorinated polyethylene, chlorinated polypropylene, vinylidene fluoride
  • Polymer latex and curable resin can be used.
  • Additives include plasticizers, stabilizers such as antioxidants and sulfurization inhibitors, surfactants, dissolution accelerators, polymerization inhibitors, and colorants such as dyes and pigments. Furthermore, from the viewpoint of improving workability such as coating properties, solvents (for example, water, organic solvents such as alcohols, glycols, cellosolves, ketones, esters, ethers, amides, hydrocarbons, etc.) are used. May be included.
  • the conductive polymer by coating and laminating a conductive polymer layer on a metal nanowire layer, in addition to conductivity due to contact between the metal nanowires, the conductive polymer enters between the metal nanowires, and the metal nanowire and the metal nanowire gap
  • the conductivity of the part can be made uniform. Furthermore, surface smoothness can be improved by forming the conductive polymer layer into a film.
  • the crosslinking agent according to the present invention is used for crosslinking a water-soluble polymer or polymer latex that is a binder in the metal nanowire layer, and an aldehyde-based, epoxy-based, melamine-based, or isocyanate-based crosslinking agent can be used.
  • the method of applying the crosslinking agent is to apply the coating solution of the crosslinking agent on the transparent substrate in advance and dry it, and then apply the metal nanowire layer to it, or apply and dry the metal nanowire layer, A crosslinking agent may be applied there, or two layers of the metal nanowire dispersion and the crosslinking agent may be applied simultaneously, or a mixture of these may be applied and dried.
  • the crosslinking agent solution may contain an acid, an alkali, or a salt as a pH adjuster, and is preferably an ammonia or ammonium salt because it can be easily removed by heating. Furthermore, it is preferable to heat at 100 to 150 ° C. in order to promote the crosslinking reaction.
  • the metal nanowire remover is patterned by an inkjet method, a screen, a gravure printing method, or the like.
  • the conductive layer can be patterned by printing, photolithography, or the like.
  • the metal nanowire layer or the conductive polymer layer may be directly patterned by an inkjet method, a gravure, a screen printing method, or the like.
  • the metal nanowire refers to a linear structure having a metal element as a main component.
  • the metal nanowire in the present invention means a structure in which a large number of linear structures having a diameter from the atomic scale to the nm size are formed in a mesh shape.
  • the metal nanowire according to the present invention preferably has an average length of 3 ⁇ m or more, more preferably 3 to 500 ⁇ m, particularly 3 to 300 ⁇ m in order to form a long conductive path with one metal nanowire. It is preferable.
  • the relative standard deviation of the length is preferably 40% or less.
  • an average diameter is small from a transparency viewpoint, On the other hand, the larger one is preferable from an electroconductive viewpoint.
  • the average diameter of the metal nanowire is preferably 10 to 300 nm, and more preferably 30 to 200 nm.
  • the relative standard deviation of the diameter is preferably 20% or less.
  • a metal composition of the metal nanowire which concerns on this invention, although it can comprise from the 1 type or several metal of a noble metal element and a base metal element, noble metals (for example, gold, platinum, silver, palladium, rhodium, (Iridium, ruthenium, osmium, etc.) and at least one metal belonging to the group consisting of iron, cobalt, copper, and tin is preferable, and at least silver is more preferable from the viewpoint of conductivity. In order to achieve both conductivity and stability (sulfurization and oxidation resistance of metal nanowires and migration resistance), it is also preferable to include silver and at least one metal belonging to a noble metal other than silver. When the metal nanowire according to the present invention includes two or more kinds of metal elements, for example, the metal composition may be different between the inside and the surface of the metal nanowire, or the entire metal nanowire has the same metal composition. May be.
  • the means for producing the metal nanowire there are no particular limitations on the means for producing the metal nanowire, and for example, known means such as a liquid phase method and a gas phase method can be used. Moreover, there is no restriction
  • the conductive polymer according to the present invention is not particularly limited, and polypyrrole, polyindole, polycarbazole, polythiophene (including substituted and unsubstituted polythiophene, the same applies hereinafter), polyaniline, polyacetylene, polyfuran, poly Chain conductive polymers such as paraphenylene vinylene, polyazulene, polyparaphenylene, polyparaphenylene sulfide, polyisothianaphthene, and polythiazyl, and polyacene conductive polymers can also be used.
  • polyethylene dioxythiophene (PEDOT) and polyaniline are preferable from the viewpoint of conductivity, transparency, and the like.
  • the long-chain sulfonic acid is preferable.
  • Examples of the long chain sulfonic acid include dinonyl naphthalene disulfonic acid, dinonyl naphthalene sulfonic acid, and dodecylbenzene sulfonic acid.
  • Examples of the halogen include Cl 2 , Br 2 , I 2 , ICl 3 , IBr, IF 5 and the like.
  • Examples of the Lewis acid include PF 5 , AsF 5 , SbF 5 , BF 3 , BCl 3 , BBr 3 , SO 3 , GaCl 3 and the like.
  • Examples of the protonic acid include HF, HCl, HNO 3 , H 2 SO 4 , HBF 4 , HClO 4 , FSO 3 H, ClSO 3 H, CF 3 SO 3 H, and the like.
  • the transition metal halide NbF 5, TaF 5, MoF 5, WF 5, RuF 5, BiF 5, TiCl 4, ZrCl 4, MoCl 5, MoCl 3, WCl 5, FeCl 3, TeCl 4, SnCl 4, SeCl 4 , FeBr 3 , SnI 5 and the like.
  • the transition metal compound AgClO 4, AgBF 4, La (NO 3) 3, Sm (NO 3) 3 and the like.
  • Examples of the alkali metal include Li, Na, K, Rb, and Cs.
  • Examples of the alkaline earth metal include Be, Mg, Ca, Sc, and Ba.
  • the dopant for the conductive polymer may be introduced into fullerenes such as hydrogenated fullerene, hydroxylated fullerene, and sulfonated fullerene. It is preferable that 0.001 mass part or more of the said dopant is contained with respect to 100 mass parts of conductive polymers. Furthermore, it is more preferable that 0.5 mass part or more is contained.
  • the transparent conductive composition of the present embodiment is a long-chain sulfonic acid, a polymer of long-chain sulfonic acid (for example, polystyrene sulfonic acid), halogen, Lewis acid, proton acid, transition metal halide, transition metal compound, Both at least one dopant selected from the group consisting of alkali metals, alkaline earth metals, MClO 4 , R 4 N + , and R 4 P + and fullerenes may be included.
  • the conductive polymer according to the present invention is 2nd.
  • a water-soluble organic compound may be contained as a dopant.
  • an oxygen containing compound is mentioned suitably.
  • the oxygen-containing compound is not particularly limited as long as it contains oxygen, and examples thereof include a hydroxyl group-containing compound, a carbonyl group-containing compound, an ether group-containing compound, and a sulfoxide group-containing compound.
  • the hydroxyl group-containing compound include ethylene glycol, diethylene glycol, propylene glycol, trimethylene glycol, 1,4-butanediol, glycerin and the like.
  • ethylene glycol and diethylene glycol are preferable.
  • the carbonyl group-containing compound include isophorone, propylene carbonate, cyclohexanone, and ⁇ -butyrolactone.
  • the ether group-containing compound include diethylene glycol monoethyl ether.
  • the sulfoxide group-containing compound include dimethyl sulfoxide. These may be used alone or in combination of two or more, but it is particularly preferable to use at least one selected from dimethyl sulfoxide, ethylene glycol, and diethylene glycol.
  • the 2nd In the conductive polymer according to the present invention, the 2nd.
  • the content of the dopant is preferably 0.001 part by mass or more, more preferably 0.01 to 50 parts by mass, and particularly preferably 0.01 to 10 parts by mass.
  • the transparent electrode of the present invention is preferably highly smooth because the surface roughness of the conductive layer affects the performance of the EL element and the like.
  • the arithmetic average roughness Ra is Ra ⁇ 5 nm. Is preferable, Ra ⁇ 3 nm is more preferable, and Ra ⁇ 1 nm is further more preferable.
  • the maximum height Ry is preferably Ry ⁇ 50 nm, more preferably Ry ⁇ 40 nm, and further preferably Ry ⁇ 30 nm.
  • the total light transmittance of the conductive layer containing metal nanowires is 60% or more, preferably 70% or more, particularly preferably 80% or more.
  • the total light transmittance can be measured according to a known method using a spectrophotometer or the like.
  • the electrical resistance value of the conductive layer containing metal nanowires is preferably 10 3 ⁇ / ⁇ or less, more preferably 10 2 ⁇ / ⁇ or less, as the surface specific resistance, It is particularly preferably 10 ⁇ / ⁇ or less.
  • the surface specific resistance can be measured, for example, according to JIS K6911, ASTM D257, etc., and can be easily measured using a commercially available surface resistivity meter.
  • the surface specific resistance only needs to satisfy the surface specific resistance in the state of the metal nanowire alone, and the metal nanowire functions as a bus electrode. Therefore, even if the surface specific resistance of the conductive polymer is high, the metal nanowire-containing conductive layer Can be made uniform.
  • the surface specific resistance of the conductive polymer is 10 4 ⁇ / ⁇ or more and 10 9 ⁇ / ⁇ or less, which can make the conductivity of the metal nanowire-containing conductive layer uniform without affecting current leakage between the metal nanowire-containing conductive layers. It is preferable that it is 10 6 ⁇ / ⁇ or more and 10 9 ⁇ / ⁇ or less.
  • An anchor coat or a hard coat can be applied to the transparent electrode of the present invention. If necessary, a conductive layer containing a conductive polymer or a metal oxide may be further provided.
  • the transparent electrode of the present invention can be used for transparent electrodes such as LCDs, electroluminescent elements, plasma displays, electrochromic displays, solar cells, touch panels, electronic paper, and electromagnetic wave shielding materials, etc., but has excellent conductivity and transparency. In addition, since it has high smoothness, it is preferably used for an organic EL device.
  • a pattern electrode is formed by pattern-printing a metal nanowire remover on a portion to be a non-pattern part of the conductive layer, and then performing a water washing treatment to remove the metal nanowire remover and the metal nanowire in the non-pattern part. can do.
  • composition of the metal nanowire remover according to the present invention a bleach-fixing agent used for development processing of a silver halide color photographic light-sensitive material can be preferably used.
  • a bleaching agent used in the bleach-fixing agent a known bleaching agent can be used.
  • an organic complex salt of iron (III) for example, a complex salt of aminopolycarboxylic acids
  • an organic compound such as citric acid, tartaric acid, malic acid, Acid, persulfate, hydrogen peroxide and the like are preferable.
  • organic complex salts of iron (III) are particularly preferred from the viewpoint of rapid processing and prevention of environmental pollution.
  • aminopolycarboxylic acids useful for forming organic complex salts of iron (III), or salts thereof include biodegradable ethylenediamine disuccinic acid (SS form), N- (2-carboxylate ethyl) -L-aspartic acid, ⁇ -alanine diacetic acid, methyliminodiacetic acid, ethylenediaminetetraacetic acid, diethylenetriaminepentaacetic acid, 1,3-diaminopropanetetraacetic acid, propylenediaminetetraacetic acid, nitrilotriacetic acid, cyclohexanediaminetetraacetic acid, iminodiacetic acid
  • compounds represented by general formula (I) or (II) of European Patent 0789275 can be mentioned.
  • These compounds may be sodium, potassium or ammonium salts.
  • the diacetic acid is preferably its iron (III) complex salt.
  • ferric ion complex salts may be used in the form of complex salts, and ferric salts such as ferric sulfate, ferric chloride, ferric nitrate, ferric ammonium sulfate, and ferric phosphate.
  • a chelating agent such as aminopolycarboxylic acid may be used to form a ferric ion complex salt in a solution. Moreover, you may use a chelating agent in excess rather than forming a ferric ion complex salt.
  • iron complexes aminopolycarboxylic acid iron complexes are preferable, and the addition amount is 0.01 to 1.0 mol / liter, preferably 0.05 to 0.50 mol / liter, and more preferably 0.10 to 0. 50 mol / liter, more preferably 0.15 to 0.40 mol / liter.
  • Fixing agents used for the bleach-fixing agent are known fixing agents, that is, thiosulfates such as sodium thiosulfate and ammonium thiosulfate, thiocyanates such as sodium thiocyanate and ammonium thiocyanate, ethylenebisthioglycolic acid, 3, These are water-soluble silver halide solubilizers such as thioether compounds such as 6-dithia-1,8-octanediol and thioureas, and these can be used alone or in combination.
  • a special bleach-fixing agent comprising a combination of a fixing agent described in JP-A-55-155354 and a large amount of a halide such as potassium iodide can also be used.
  • a halide such as potassium iodide
  • the amount of fixing agent per liter is preferably 0.3 to 2 mol, more preferably 0.5 to 1.0 mol.
  • the pH range of the bleach-fixing agent used in the present invention is preferably 3 to 8, and more preferably 4 to 7.
  • hydrochloric acid, sulfuric acid, nitric acid, bicarbonate, ammonia, caustic potash, caustic soda, sodium carbonate, potassium carbonate and the like can be added as necessary.
  • bleach-fixing agent can contain various other antifoaming agents or surfactants, and organic solvents such as polyvinylpyrrolidone and methanol.
  • Bleach fixers use sulfites (eg, sodium sulfite, potassium sulfite, ammonium sulfite, etc.), bisulfites (eg, ammonium bisulfite, sodium bisulfite, potassium bisulfite, etc.), metabisulfite as preservatives.
  • sulfite ion releasing compounds such as salts (for example, potassium metabisulfite, sodium metabisulfite, ammonium metabisulfite, etc.), arylsulfinic acids such as p-toluenesulfinic acid, m-carboxybenzenesulfinic acid, and the like. Is preferred. These compounds are preferably contained in an amount of about 0.02 to 1.0 mol / liter in terms of sulfite ion or sulfinate ion.
  • ascorbic acid in addition to the above, ascorbic acid, a carbonyl bisulfite adduct, or a carbonyl compound may be added. Furthermore, you may add a buffering agent, a chelating agent, an antifoamer, an antifungal agent, etc. as needed.
  • the pattern printing of the composition containing the metal nanowire remover includes letterpress (letter) printing, stencil (screen) printing, lithographic (offset) printing, intaglio (gravure) printing, spray printing, and inkjet.
  • letterpress letter
  • stencil screen
  • lithographic offset
  • intaglio gravure
  • spray printing and inkjet.
  • a printing method such as a printing method can be used, the gravure printing method and the screen printing method are particularly preferable.
  • the organic EL element in the present invention has the transparent electrode of the present invention.
  • the organic EL element in the present invention uses the transparent electrode of the present invention as an anode, and the organic light-emitting layer and the cathode can be made of any material and configuration generally used in organic EL elements.
  • the element configuration of the organic EL element is as follows: anode / organic light emitting layer / cathode, anode / hole transport layer / organic light emitting layer / electron transport layer / cathode, anode / hole injection layer / hole transport layer / organic light emitting layer / electron transport layer / Cathode, anode / hole injection layer / organic light emitting layer / electron transport layer / electron injection layer / cathode, anode / hole injection layer / organic light emitting layer / electron injection layer / cathode, etc. it can.
  • the organic light emitting layer is prepared by a known method using the above materials and the like, and examples thereof include vapor deposition, coating, and transfer.
  • the thickness of the organic light emitting layer is preferably 0.5 to 500 nm, particularly preferably 0.5 to 200 nm.
  • the organic EL element in the present invention can be used for a self-luminous display, a liquid crystal backlight, illumination, and the like. Since the organic EL element of the present invention can emit light uniformly and without unevenness, it is preferably used for lighting purposes.
  • the reaction solution containing the core particles after the ripening was kept at 170 ° C. while stirring, and 1000 ml of an ethylene glycol solution of silver nitrate (silver nitrate concentration: 1.0 ⁇ 10 ⁇ 1 mol / l) and ethylene glycol of polyvinylpyrrolidone. 1000 ml of a solution (vinyl pyrrolidone concentration conversion: 5.0 ⁇ 10 ⁇ 1 mol / l) was added at a constant flow rate for 100 minutes using a double jet method.
  • the reaction solution was sampled every 20 minutes in the particle growth process and confirmed with an electron microscope, the silver nanoparticles formed in the nucleation process grew mainly in the long axis direction of the nanowires over time. No new core particles were observed in the grain growth process.
  • the reaction solution was cooled to room temperature, filtered using a filter, and the silver nanowires separated by filtration were redispersed in ethanol. Filtration of silver nanowires with a filter and redispersion in ethanol were repeated 5 times, and finally an aqueous dispersion of silver nanowires was prepared to produce silver nanowires.
  • a small amount of the obtained dispersion was collected and confirmed with an electron microscope, and it was confirmed that silver nanowires having an average diameter of 85 nm and an average length of 7.4 ⁇ m were formed.
  • Baytron PH510 manufactured by HC Starck
  • PEDOT: PSS polystyrene sulfonic acid
  • UL-1 surfactant
  • Transparent Electrode 104 Similar to the production of the transparent electrode 101, after the silver nanowire layer was formed, it was overcoated with a saturated solution so that the coating amount of the crosslinking agent glyoxal was 10% of the binder mass in the coating film. This was subjected to heat treatment and the formation of a conductive polymer layer in the same manner as the transparent electrode 103 to produce a transparent electrode 104.
  • the crosslinking agent is an epoxy-based crosslinking agent EX512 (manufactured by Nagase ChemteX), and the conductive polymer is changed to PEDOT: PSS Denatron P-502S (manufactured by Nagase ChemteX). Performed the same operation to produce a transparent electrode 108.
  • Transparent Electrode 109 [Preparation of Transparent Electrode 109; Present Invention 7]
  • the binder was changed to hydroxypropylmethylcellulose (HPMC)
  • the crosslinking agent was changed to melamine-based crosslinking agent Becamine M3 and Catalyst ACX (made by DIC)
  • the conductive polymer was changed to P-502S.
  • the transparent electrode 109 was produced.
  • transparent electrode 110 Invention 8
  • the binder was HPMC
  • the cross-linking agent was Becamine M3 and Catalist ACX
  • the conductive polymer was changed to PEDOT: PSS Denatron P-5002CW (manufactured by Nagase ChemteX).
  • a transparent electrode 110 was produced.
  • a thermosetting resin-containing PEDOT Denatron G-2001A manufactured by Nagase ChemteX
  • P-5002CW was applied as a conductive polymer to produce a transparent electrode 113.
  • metal nanowire removal solution BF-1 Ethylenediaminetetraacetic acid ferric ammonium 60g Ethylenediaminetetraacetic acid 2g Sodium metabisulfite 15g 70g ammonium thiosulfate Maleic acid 5g Finished to 1 L with pure water and adjusted to pH 5.5 with sulfuric acid or ammonia water, metal nanowire removal liquid BF-1 was prepared.
  • PET polyethylene terephthalate film
  • Konica Minolta CMC carboxymethylcellulose
  • PEDOT poly-3,4-ethylenediothiophene
  • H.M. C. Made by Starck (trade name: PH510)
  • PSS polystyrene sulfonic acid
  • Stark PVA203 polyvinyl alcohol
  • Kuraray Denatron P-502S (trade name of the above PEDOT and PSS mixture): Nagase ChemteX HPMC (hydroxypropylmethylcellulose): Sigma Aldrich Becamine M3 (melamine cross-linking agent) ): Catalyst ACX (resin catalyst) manufactured by DIC: Denatron P-5002CW (trade name of the above PEDOT and PSS mixture) manufactured by DIC: P-502S (trade name of the above PEDOT and PSS mixture) manufactured by Nagase ChemteX Corporation: EX512 (epoxy-based crosslinking agent Denacol) manufactured by Nagase ChemteX Corp .: P-5002CW manufactured by Nagase ChemteX Corp.
  • a commercially available atomic force microscope (AFM) can be used, and measurement was performed by the following method.
  • an SPI 3800N probe station and SPA400 multifunctional unit manufactured by Seiko Instruments Inc. as the AFM set the sample cut to a size of about 1 cm square on a horizontal sample stage on the piezo scanner, and place the cantilever on the sample surface.
  • scanning is performed in the XY direction, and the unevenness of the sample at that time is captured by the displacement of the piezo in the Z direction.
  • a piezo scanner that can scan XY 20 ⁇ m and Z 2 ⁇ m is used.
  • the cantilever is a silicon cantilever SI-DF20 manufactured by Seiko Instruments Inc., which has a resonance frequency of 120 to 150 kHz and a spring constant of 12 to 20 N / m, and is measured in a DFM mode (Dynamic Force Mode). A measurement area of 80 ⁇ 80 ⁇ m is measured at a scanning frequency of 1 Hz.
  • Table 1 shows the results of measurement and evaluation.
  • the transparent electrode of the present invention has excellent smoothness Ra and Ry.
  • organic element (organic EL element)
  • transparent electrodes 101 to 116 As the first electrode, organic EL elements 201 to 216 were produced in the following procedure, respectively.
  • the red dopant material Btp 2 Ir (acac) is 1% by mass and the green dopant material Ir (ppy) 3 is 2% with respect to polyvinylcarbazole (PVK) as the host material.
  • % And blue dopant material FIr (pic) are mixed so as to be 3% by mass, respectively, and dissolved in 1,2-dichloroethane so that the total solid concentration of PVK and the three dopants is 1% by mass.
  • the coating liquid for layer formation was applied with a spin coater and then dried at 100 ° C. for 10 minutes to form a light emitting layer having a thickness of 60 nm.
  • LiF was deposited as an electron transport layer forming material under a vacuum of 5 ⁇ 10 ⁇ 4 Pa to form an electron transport layer having a thickness of 0.5 nm.
  • Second electrode On the formed electron transport layer, Al was deposited as a second electrode forming material under a vacuum of 5 ⁇ 10 ⁇ 4 Pa to form a second electrode having a thickness of 100 nm.
  • ⁇ 90% or more emits uniformly ⁇ : 80% or more emits uniformly ⁇ : 70% or more emits uniformly ⁇ : Less than 70% emits XX: no Does not emit light.

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  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Non-Insulated Conductors (AREA)
  • Manufacturing Of Electric Cables (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

L'invention concerne une électrode transparente qui présente un polissage de surface, une conductivité électrique et une transparence excellents, tout en présentant une forte productivité. L'électrode transparente comprend, sur un corps de support transparent, une couche conductrice qui est composée d'une couche de nanofils métalliques et d'une couche polymère conductrice, et est caractérisée en ce que la couche de nanofils métalliques contient au moins une substance sélectionnée parmi les produits réticulés de polymères solubles dans l'eau, les produits réticulés de latex polymères et les produits durcis de résines durcissables.
PCT/JP2009/071121 2009-01-19 2009-12-18 Électrode transparente, son procédé de production et élément électroluminescent organique Ceased WO2010082428A1 (fr)

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JP2011029036A (ja) * 2009-07-27 2011-02-10 Panasonic Electric Works Co Ltd 透明導電膜付き基材
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US20140106154A1 (en) * 2012-10-11 2014-04-17 Do Young Kim Transparent conductor, composition for preparing the same, and optical display apparatus including the same
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KR20140139015A (ko) * 2012-03-20 2014-12-04 시쉘 테크널러지, 엘엘씨 전도성 물질에 관한 혼합물, 방법 및 조성물
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WO2017018427A1 (fr) * 2015-07-30 2017-02-02 昭和電工株式会社 Procédé de production d'un film conducteur, et film conducteur
KR101802952B1 (ko) * 2014-10-28 2017-11-30 주식회사 엔앤비 투명 전도체 및 이의 제조방법
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JP2011029036A (ja) * 2009-07-27 2011-02-10 Panasonic Electric Works Co Ltd 透明導電膜付き基材
JP2011034711A (ja) * 2009-07-30 2011-02-17 Sumitomo Chemical Co Ltd 有機エレクトロルミネッセンス素子
CN102484925B (zh) * 2009-07-30 2016-07-06 住友化学株式会社 有机电致发光元件
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WO2011013618A1 (fr) * 2009-07-30 2011-02-03 住友化学株式会社 Elément électroluminescent organique
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US9401490B2 (en) 2010-10-29 2016-07-26 Lintec Corporation Transparent conductive film, electronic device, and method for manufacturing electronic device
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US8987720B2 (en) 2010-12-13 2015-03-24 Konica Minolta, Inc. Transparent surface electrode, organic electronic element, and method for manufacturing transparent surface electrode
JPWO2012093530A1 (ja) * 2011-01-06 2014-06-09 リンテック株式会社 透明導電性積層体および有機薄膜デバイス
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EP2681780B1 (fr) * 2011-03-04 2018-11-28 CAM Holding Corporation Procédé de syntonisation du travail d'extraction d'un conducteur transparent basé sur une nanostructure métallique
JP2014511551A (ja) * 2011-03-04 2014-05-15 カンブリオス テクノロジーズ コーポレイション 金属ナノ構造を基にした透明な導体の仕事関数を調整する方法
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DE102012016759A1 (de) * 2012-08-27 2014-02-27 Inoviscoat Gmbh Leuchtelement mit einer Leuchtschicht, die Elektrolumineszenzteilchen aufweist
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US9384865B2 (en) * 2012-10-11 2016-07-05 Cheil Industries, Inc. Transparent conductor, composition for preparing the same, and optical display apparatus including the same
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WO2015126052A1 (fr) * 2014-02-20 2015-08-27 주식회사 인포비온 Procédé de fabrication d'un film conducteur transparent à l'aide de nanofils conducteurs
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