WO2016031426A1 - Procédé de fabrication de film conducteur - Google Patents

Procédé de fabrication de film conducteur Download PDF

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Publication number
WO2016031426A1
WO2016031426A1 PCT/JP2015/070559 JP2015070559W WO2016031426A1 WO 2016031426 A1 WO2016031426 A1 WO 2016031426A1 JP 2015070559 W JP2015070559 W JP 2015070559W WO 2016031426 A1 WO2016031426 A1 WO 2016031426A1
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Prior art keywords
light
conductive film
wavelength
base material
metal
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PCT/JP2015/070559
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English (en)
Japanese (ja)
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美里 佐々田
浩史 太田
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富士フイルム株式会社
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Priority to JP2016545049A priority Critical patent/JPWO2016031426A1/ja
Publication of WO2016031426A1 publication Critical patent/WO2016031426A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/12—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain a coating with specific electrical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D201/00—Coating compositions based on unspecified macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D201/00—Coating compositions based on unspecified macromolecular compounds
    • C09D201/02—Coating compositions based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups
    • C09D201/06—Coating compositions based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing oxygen atoms
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/02—Emulsion paints including aerosols
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/24—Electrically-conducting paints
    • 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
    • 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
    • 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

Definitions

  • the present invention relates to a method for producing a conductive film.
  • a metal film or a circuit board is obtained by applying a dispersion of metal particles or metal oxide particles to the base material by a printing method and then sintering by heat treatment or light irradiation treatment.
  • a technique for forming an electrically conductive portion such as a wiring in is known. Since the above method is simpler, energy-saving, and resource-saving than conventional high-heat / vacuum processes (sputtering) and plating processes, it is highly anticipated in the development of next-generation electronics.
  • Patent Document 1 there is a method for sintering nano metal particles, the method comprising: Depositing the nanometal particles on the substrate; and the nanometal particles on the substrate with a pulse width of 1 microsecond to 100 milliseconds so that the conductivity of the nanometal particles on the substrate is increased at least twice.
  • a method is disclosed wherein the substrate is PET and the nanometal particles are irradiated on the substrate in ambient air. Note that FIG. 6 of Patent Document 1 shows that light from a light source is directly applied to a product.
  • the conductive film is cracked due to the rapid evaporation of gas generated from the resin base material, organic matter contained in the conductive film forming composition, water, and the like. There was also a problem that defects such as these were likely to occur.
  • an object of the present invention is to provide a method of manufacturing a conductive film that can suppress the generation of defects and can form a conductive film exhibiting excellent conductivity.
  • the present inventors applied a composition for forming a conductive film containing metal or metal compound nanoparticles on a resin substrate to form a first coating film. And a second step of forming a conductive film by irradiating the coating film with light. In the second step, among the light irradiated to the coating film, the wavelength is 370 nm or less and the wavelength is 800 nm or more. It has been found that the above problem can be solved by a method for producing a conductive film that reduces at least one light intensity selected from the group consisting of: That is, it has been found that the above object can be achieved by the following configuration.
  • the manufacturing method of an electrically conductive film [2] The method for producing a conductive film according to [1], wherein the light intensity is reduced by an optical filter.
  • a composition for forming a conductive film comprises Cupric oxide nanoparticles having an average primary particle diameter of 2 to 25 nm; A polyol compound, The method for producing a conductive film according to any one of [1] to [3], comprising at least water.
  • a polyol compound The method for producing a conductive film according to any one of [1] to [3], comprising at least water.
  • the method for producing a conductive film according to any one of [1] to [4], wherein the light is pulsed light.
  • the resin base material is at least one selected from the group consisting of a polyethylene terephthalate base material, a polyethylene naphthalate base material, a cycloolefin polymer base material, and a polyimide base material.
  • a numerical range expressed using “to” means a range including numerical values described before and after “to” as a lower limit value and an upper limit value.
  • content of the said component refers to content of the sum total of 2 or more types of compounds.
  • the light intensity with a wavelength of 370 nm or less is synonymous with the intensity of light with a wavelength of 370 nm or less.
  • the intensity of light having a wavelength of 800 nm or more is synonymous with the intensity of light having a wavelength of 800 nm or more.
  • the method for producing the conductive film of the present invention comprises: A first step of applying a conductive film-forming composition containing metal or metal compound nanoparticles on a resin substrate to form a coating film; Having a second step of forming a conductive film by irradiating light to the coating film, In the second step, in the method for producing a conductive film, at least one light intensity selected from the group consisting of a wavelength of 370 nm or less and a wavelength of 800 nm or more is reduced among the light irradiated on the coating film.
  • the temperature applied to the resin substrate is high when forming the conductive film, gas is generated from the resin substrate, and the gas may cause cracks in the conductive film.
  • a dimming means that reduces at least one light intensity selected from the group consisting of a wavelength of 370 nm or less and a wavelength of 800 nm or more among the light irradiated on the coating film.
  • the heat applied to the resin base material can be reduced. Therefore, generation
  • This step is a step of forming a coating film by applying a conductive film-forming composition containing metal or metal compound nanoparticles on a resin substrate.
  • the precursor film before the reduction treatment is obtained in this step.
  • the composition for electrically conductive film formation used for this invention contains the nanoparticle (A) of a metal or a metal compound.
  • the metal that the nanoparticles can contain include silver, copper, gold, platinum, palladium, tin, antimony, indium, and lead.
  • the metal compound that can be contained in the nanoparticles is not particularly limited as long as it can be converted into a metal by light baking. Examples thereof include metal oxides, metal hydroxides, and metal halides.
  • the metal include the same metals as those contained in the conductive film forming composition.
  • the electroconductivity of the electrically conductive film formed is more excellent, and a copper oxide is preferable at the point which can suppress generation
  • the metal or metal compound is a nanoparticle.
  • nano means that the dimension is less than about 1 micron. This dimension is preferably less than about 500 nm, more preferably less than about 100 nm.
  • the composition for forming a conductive film may contain at least one selected from the group consisting of primary particles and secondary particles of metal or metal compound nanoparticles.
  • the average primary particle of the metal or metal compound nanoparticles is preferably 2 to 25 nm, and more preferably 5 to 25 nm, from the viewpoint that the conductivity of the conductive film to be formed is superior and the generation of defects can be further suppressed. Is more preferable.
  • the average primary particle diameter is equivalent to a circle of at least 400 nanoparticles by observation with a transmission electron microscope (abbreviation of TEM) or scanning electron microscope (abbreviation of scanning electron microscope). Measure the diameters and find the arithmetic average of them.
  • the equivalent circle diameter means the diameter of a circle corresponding to the same area as the two-dimensional shape of the observed nanoparticles.
  • the volume average secondary particle diameter of the metal or metal compound nanoparticles is preferably from 20 to 200 nm, more preferably from 20 to 150 nm, from the viewpoint that the conductivity of the conductive film to be formed is more excellent and defects can be further suppressed. More preferably.
  • the volume average secondary particle diameter can be determined by a measurement method using a dynamic light scattering method. More specifically, the measurement is performed using a nanotrack particle size distribution analyzer UPA-EX150 (manufactured by Nikkiso Co., Ltd.).
  • the conductive film forming composition can be used as it is or diluted with water or the like.
  • the metal or metal compound nanoparticles (A) may be a commercially available product or may be produced by a known production method.
  • a method for producing metal or metal compound nanoparticles (A) for example, there are a method of performing granulation in a gas phase (gas phase method) and a method of performing granulation in a wet method (wet method).
  • the metal or metal compound nanoparticles (A) are preferably produced by a wet process. It is because it becomes possible to control to a desired particle shape by granulating by a wet method.
  • a divalent salt such as copper nitrate is reacted with a base to produce water.
  • a method of producing copper oxide and granulating the copper oxide by heat dehydration is preferable. According to this method, it is possible to synthesize the metal or metal compound nanoparticles (A) at a lower temperature and in a shorter time, and the desired particle shape / distribution can be controlled.
  • water or a polyhydric alcohol having a boiling point of 180 to 350 ° C. it is preferable because it does not volatilize during heating and dehydration and is excellent in dispersion stability of the produced metal or metal compound nanoparticles (A).
  • the content of the metal or metal compound nanoparticles (A) in the composition for forming a conductive film is not particularly limited, but it is easy to prepare a predetermined composition, and characteristics of the formed conductive film (defect suppression, conductivity) Is more preferably 3 to 80% by mass, and more preferably 10 to 60% by mass with respect to the total mass of the composition.
  • the composition for forming a conductive film can further contain a polyol compound (B).
  • the polyol compound is a compound having two or more hydroxy groups in one molecule.
  • the polyol compound can function as a so-called reducing agent.
  • polyol compound (B) examples include diols; trifunctional or higher functional polyols (alcohols having three or more hydroxy groups) such as 1,2,3-butanetriol, erythritol, pentaerythritol, and trimethylolpropane. It is done.
  • the polyol-based organic solvent is preferably diol or triol.
  • diol examples include alcohols having two hydroxy groups such as ethylene glycol and 2,3-butanediol; dialkylene glycols such as diethylene glycol; trialkylene glycols such as triethylene glycol.
  • dialkylene glycols such as diethylene glycol
  • trialkylene glycols such as triethylene glycol.
  • polyalkylene glycol such as dialkylene glycol and trialkylene glycol
  • its weight average molecular weight is less than 1,000.
  • the diol is preferably at least one selected from the group consisting of ethylene glycol, diethylene glycol, and triethylene glycol.
  • the boiling point of the (B) polyol compound is preferably 180 to 340 ° C., more preferably 190 to 300 ° C., from the viewpoint that the conductivity of the conductive film to be formed is superior and the generation of defects can be further suppressed. Is more preferable.
  • the above boiling point is under 1 atm.
  • the mass ratio of the metal or metal compound nanoparticles and the (B) polyol compound is sufficient in reducing power, more excellent in conductivity of the conductive film formed, and more capable of suppressing the occurrence of defects.
  • the ratio is preferably 1: 0.005 to 1: 2, and more preferably 1: 0.005 to 1: 0.5.
  • the composition for forming an electrically conductive film can further contain (C) a polyoxyalkylene compound.
  • (C) a polyoxyalkylene compound it is preferable from the viewpoint that the conductivity of the conductive film to be formed is more excellent and the occurrence of defects can be further suppressed.
  • the (C) polyoxyalkylene compound include polyethylene glycol and polypropylene glycol, and polyethylene glycol is preferable.
  • the weight average molecular weight of the polyoxyalkylene compound is preferably 1,000 or more from the viewpoint that the conductivity of the conductive film to be formed is more excellent and the occurrence of defects can be further suppressed. More preferably, it is 1,000.
  • the weight average molecular weight of the polyoxyalkylene compound is a polystyrene equivalent value obtained by GPC method (gel permeation chromatography, abbreviation for Gel Permeation Chromatography) (solvent: N-methylpyrrolidone).
  • the mass ratio of (A) metal or metal compound nanoparticles and (C) polyoxyalkylene compound is from 1: 0.01 to the point that the conductivity of the conductive film to be formed is superior and the occurrence of defects can be further suppressed. It is preferably 1: 0.5, and more preferably 1: 0.02 to 1: 0.4.
  • the composition for forming a conductive film can further contain an alcohol-based organic solvent or a ketone-based organic solvent (D).
  • an alcohol-based organic solvent or a ketone-based organic solvent (D) In this case, excellent printability can be obtained.
  • the surface tension of the alcohol organic solvent or ketone organic solvent (D) is preferably 40 mN / m or less, more preferably 20 to 30 mN / m or less. The surface tension is measured by a measurement method using a dropping method under the condition of 20 ° C.
  • the boiling point of the alcohol organic solvent or ketone organic solvent (D) is preferably 50 to 180 ° C, more preferably 70 to 150 ° C. The above boiling point is under 1 atm.
  • Examples of the alcohol organic solvent or ketone organic solvent (D) include ethanol (boiling point 78.37 ° C., surface tension 22.55 mN / m), 1-butanol (boiling point 117 ° C., surface tension 26 mN / m), and the like.
  • Alcohol-based organic solvents ketone-based organic solvents such as methyl ethyl ketone (boiling point 79.5 ° C., surface tension 24.6 mN / m), acetone (boiling point 56.5 ° C., surface tension 23.3 mN / m), and the like.
  • the amount of the alcohol-based organic solvent or the ketone-based organic solvent (D) is preferably 1 to 50% by mass, more preferably 1 to 40% by mass in the conductive film forming composition.
  • the composition for forming an electrically conductive film can further contain (E) a metal catalyst.
  • the metal catalyst (E) preferably contains at least one metal element (metal) selected from the group consisting of groups 8 to 11 of the periodic table.
  • the metal element is at least one metal element selected from the group consisting of gold, silver, copper, platinum, palladium, rhodium, iridium, ruthenium, osmium, and nickel in that the conductivity of the conductive film is more excellent.
  • it is more preferably at least one metal element selected from the group consisting of silver, platinum, palladium, and nickel, particularly preferably palladium or platinum, and most preferably palladium. That is, the metal catalyst (E) is preferably a metal catalyst containing palladium because the conductivity of the obtained conductive film is more excellent.
  • a palladium salt is preferable.
  • the kind of palladium salt is not particularly limited, and specific examples thereof include palladium hydrochloride, nitrate, sulfate, carboxylate, sulfonate, phosphate, phosphonate and the like.
  • carboxylate is preferable.
  • the number of carbon atoms of the carboxylic acid forming the carboxylate is not particularly limited, but is preferably 1 to 10, and more preferably 1 to 5.
  • the carboxylic acid forming the carboxylate may have a halogen atom (preferably a fluorine atom).
  • the metal catalyst (E) is preferably at least one compound selected from the group consisting of palladium acetate, palladium trifluoroacetate and tetrakis (triphenylphosphine) palladium, and more preferably palladium acetate.
  • the mass ratio of (A) metal or metal compound nanoparticles and (E) metal catalyst is 1: 0.001 to 1: from the viewpoint that the conductivity of the conductive film to be formed is better and the generation of defects can be further suppressed. 0.1 is preferable, and 1: 0.001 to 1: 0.05 is more preferable.
  • the composition for electrically conductive film formation can contain water further.
  • Water (A) functions as a dispersion medium for nanoparticles of metal or metal compound. Use of water as a solvent is preferable because of its excellent safety. As water, what has the purity of the level of ion-exchange water is preferable.
  • the water content can be 1 to 90% by mass with respect to the total mass of the conductive film-forming composition.
  • the composition for forming a conductive film can further contain components other than (A) to (E) and water.
  • components other than the above include additives such as water-soluble polymers, surfactants, and thixotropic agents.
  • the kind and amount of the additive can be appropriately selected within a range that does not hinder the object and effect of the present invention.
  • composition for forming a conductive film for example, Cupric oxide nanoparticles having an average primary particle diameter of 2 to 25 nm;
  • a polyol compound is a composition containing at least water.
  • the manufacturing method in particular of the composition for electrically conductive film formation is not restrict
  • the mixing method is not particularly limited.
  • a homogenizer for example, an ultrasonic homogenizer, a high-pressure homogenizer
  • a mill for example, a bead mill, a ball mill, a tower mill, a three roll mill
  • a mixer for example, a planetary mixer, a disper mixer, a hen
  • a method of mixing and dispersing using a sill mixer, a kneader, a Clare mix, a self-revolving mixer (stirring deaerator), and the like it is preferable to use an ultrasonic homogenizer or a bead mill in that the dispersibility of the nanoparticles is more excellent.
  • the resin base material used in the first step is a resin base material.
  • a transparent resin substrate is preferable as the resin substrate.
  • the transparent resin base material intends a resin base material having a total light transmittance of 70% or more.
  • the total light transmittance of the resin base material is preferably 80% or more, and more preferably 85% or more.
  • the total light transmittance of the resin base material can be measured according to JIS K 7361-1.
  • the resin base material may absorb at least one light selected from the group consisting of a wavelength of 370 nm or less and a wavelength of 800 nm or more.
  • the resin base material examples include a polyethylene terephthalate base material, a polyethylene naphthalate base material, a cycloolefin polymer base material, and a polyimide base material.
  • the thickness of the resin substrate is not particularly limited, and can be 30 to 500 ⁇ m.
  • the method for applying the conductive film-forming composition onto the resin substrate is not particularly limited, and a known method can be adopted.
  • coating methods such as a screen printing method, a dip coating method, a spray coating method, a spin coating method, and an ink jet method can be used.
  • the shape of application is not particularly limited, and may be a planar shape covering the entire surface of the resin base material or a pattern shape (for example, a wiring shape or a dot shape).
  • the coating amount of the composition for forming a conductive film on the resin substrate may be appropriately adjusted according to the desired film thickness of the conductive film.
  • the film thickness of the coating film is preferably 0.01 to 5000 ⁇ m. 0.1 to 1000 ⁇ m is more preferable, and 1 to 100 ⁇ m is even more preferable.
  • the conductive film-forming composition may be applied to the resin substrate and then dried to remove the solvent. By removing the remaining solvent, it is possible to suppress the generation of minute cracks and voids due to the vaporization and expansion of the solvent in the conductive film forming step described later. It is preferable in terms of adhesion.
  • a warm air dryer or the like can be used as a method for the drying treatment.
  • the temperature for the drying treatment is preferably 40 ° C. to 200 ° C., more preferably 50 ° C. or more and less than 150 ° C., and further preferably 50 ° C. to 120 ° C.
  • the drying time is not particularly limited, but it is preferably 10 seconds to 60 minutes because the adhesion between the resin substrate and the conductive film becomes better.
  • This step is a step of forming a conductive film by irradiating the coating film with light.
  • the light irradiated to the coating film is selected from the group consisting of a wavelength of 370 nm or less and a wavelength of 800 nm or more. Reducing at least one light intensity; The light intensity is reduced by the light reducing means. That is, in this step, the light intensity of the light in the predetermined wavelength range among the light emitted from the predetermined light source toward the conductive film is reduced by using the dimming means, and the light in the specific wavelength range is emitted.
  • This is a step of irradiating the coating film.
  • the dimming means is usually arranged between the light source that emits light and the coating film, and when the light emitted from the light source passes through the dimming means, An embodiment in which the strength decreases is preferable.
  • the metal compounds are reduced to form metal particles, and the generated metal particles are fused together to form grains. Are bonded and fused to form a conductive thin film containing metal.
  • the metal nanoparticles are fused together to form grains, and the grains are bonded and fused together to form a conductive thin film containing metal.
  • the resin base material is prevented from generating heat by absorbing the light intensity in the predetermined wavelength range.
  • production of the gas from a base material is suppressed and generation
  • the dimming means only needs to reduce at least one light intensity selected from the group consisting of a wavelength of 370 nm or less and a wavelength of 800 nm or more, among the light irradiated on the coating film.
  • the wavelength is 370 nm or less.
  • a light reducing member that reduces the light intensity of the light, a light reducing member that decreases the light intensity at a wavelength of 800 nm or more, or a light reducing member that decreases the light intensity at a wavelength of 370 nm or less and a wavelength of 800 nm or more can be used.
  • the light reducing member that reduces the light intensity of the wavelength of 800 nm or more can further reduce the light intensity of the wavelength of 300 nm or less.
  • the dimming means may be a combination of a plurality of dimming members that reduce the intensity of light in a predetermined wavelength range. For example, when reducing the light intensity of both light having a wavelength of 370 nm or less and light having a wavelength of 800 nm or more, the light reducing member for reducing the light intensity of a wavelength of 370 nm or less and the light intensity having a wavelength of 800 nm or more are reduced.
  • a dimming member to be used may be used in combination.
  • a dimming means for reducing the intensity of light having a wavelength of 800 nm or the intensity of light having a wavelength of 800 nm or more for example, a first dimming member that reduces the intensity of light having a wavelength of 800 to 1000 nm and light having a wavelength of more than 1000 nm
  • a second dimming member that reduces the strength may be used in combination.
  • the dimming means can be disposed between the light source and the coating film.
  • two or more kinds of light reducing members are used in combination as the light reducing means as described above, there is no particular limitation on the order in which the two or more light reducing members are arranged between the light source and the coating film.
  • the upper light reducing member and the lower light reducing member may be in close contact with each other or may be arranged with a gap therebetween.
  • the light reduction mechanism in the light reduction means is not particularly limited as long as it can absorb or reflect light having a wavelength of 370 nm or less or a wavelength of 800 nm or more.
  • the dimming means include an absorption filter containing an absorbent (for example, a dye or a pigment) that can absorb at least light in a predetermined wavelength range; a reflective filter such as a band-pass filter (dielectric multilayer film). It is done.
  • the dimming means include a filter (for example, an optical filter).
  • the filter includes a liquid layer.
  • the filter is not particularly limited as long as it has light shielding properties in a predetermined wavelength region. Commercial products can be used.
  • filters that reduce the light intensity (wavelength of infrared light) having a wavelength of 800 nm or more include, for example, heat absorption filters HA30, HA5, HA15 manufactured by HOYA CANDEO OPTRONICS, and Techspec hot mirrors and UV hot mirrors manufactured by Edmund. IR cut filter, heat absorbing glass (KG-1) and the like.
  • filters that reduce the light intensity at a wavelength of 370 nm or less include, for example, Sharp Cut Filters SCF-50S-37L, SCF-50S-38L, SCF-50S-39L manufactured by Sigma Koki Co., Ltd. Etc.
  • the dimming means can preferably reduce (cut) the light intensity in a predetermined wavelength range by 30 to 100%, more preferably 40 to 100%.
  • the transmittance of the light having a wavelength of 370 nm of the light reducing means is preferably 70% or less, and more preferably 50% or less. Although a minimum in particular is not restrict
  • the dimming means decreases the light intensity having a wavelength of 800 nm or more
  • the transmittance of light with a wavelength of 900 nm of the dimming means is preferably 70% or less, and more preferably 50% or less. Although a minimum in particular is not restrict
  • the light attenuation means preferably has a light transmittance of at least 70% or more and more preferably 75% or more in a wavelength range of more than 450 nm and less than 650 nm. Further, the transmittance of light having a wavelength of 500 nm of the dimming means is preferably 70% or more, and more preferably 75% or more. Although an upper limit in particular is not restrict
  • the light transmittance of the dimming means can be measured by, for example, a spectrophotometer.
  • a spectrophotometer used for the measurement include Hitachi spectrophotometer U-4100.
  • FIG. 1 is a cross-sectional view showing an embodiment of the second step using the dimming means.
  • the first filter 105 constitutes a dimming means.
  • a coating film 103 made of a conductive film forming composition is formed on a resin base material 101.
  • One first filter 105 is disposed between the coating 103 and a light source (not shown).
  • the first filter 105 is a filter that absorbs (or reflects) light having a wavelength of 370 nm or less and a wavelength of 800 nm or more among light transmitted through the first filter 105.
  • Light 110 emitted from a light source (not shown) passes through the filter 105 to become light 112, and the light 112 is irradiated onto the coating film 103.
  • the light intensity with a wavelength of 370 nm or less and a wavelength of 800 nm or more is reduced to become light 112.
  • the first filter that absorbs (or reflects) light having a wavelength of 370 nm or less and a wavelength of 800 nm or more is used.
  • the present invention is applicable to any one of light having a wavelength of 370 nm or less and light having a wavelength of 800 nm or more.
  • a filter that absorbs (or reflects) only light having a wavelength of 370 nm or less or a filter that absorbs (or reflects) only light having a wavelength of 800 nm or more may be used.
  • FIG. 2 is a cross-sectional view showing another embodiment of the second step using the dimming means.
  • the second filter 205 and the third filter 207 constitute a dimming unit.
  • a coating film 203 made of a conductive film forming composition is formed on a resin base material 201.
  • a second filter 205 and a third filter 207 are arranged between the coating film 203 and a light source (not shown).
  • the second filter 205 is a filter that absorbs (or reflects) light having a wavelength of 370 nm or less out of light transmitted through itself
  • the third filter 207 is a wavelength of 800 nm or more out of light transmitted through itself. It is a filter that absorbs (or reflects) light.
  • Light 210 emitted from a light source passes through the second filter 205 and the third filter 207 to become light 212, and the light 212 is irradiated onto the coating film 203.
  • the light 210 passes through the second filter 205 and the third filter 207, whereby the light intensity with a wavelength of 370 nm or less and a wavelength of 800 nm or more is reduced to become light 212.
  • FIG. 3 is a sectional view showing another embodiment of the second step using the dimming means.
  • the liquid layer 307 constitutes a dimming means.
  • a coating film 303 made of a conductive film forming composition is formed on a resin base material 301.
  • One liquid layer 307 is disposed between the coating film 303 and a light source (not shown).
  • the liquid layer 307 is a liquid layer, and the liquid layer 307 is placed in the water tank 305.
  • the liquid layer 307 absorbs light having a wavelength of 370 nm or less and a wavelength of 800 nm or more among light transmitted through the liquid layer 307.
  • Light 310 emitted from a light source passes through the liquid layer 307 to become light 312, and the light 312 is irradiated onto the coating film 303. As the light 310 passes through the liquid layer 307, the light intensity with a wavelength of 370 nm or less and a wavelength of 800 nm or more is reduced to become light 312.
  • Light irradiation also referred to as light irradiation treatment
  • this step enables reduction and sintering to metal by irradiating light at a room temperature for a short time to a portion to which a coating film has been applied.
  • the resin base material is not deteriorated by heating, and the adhesion of the conductive film to the resin base material becomes better.
  • the light source used in the light irradiation treatment is not particularly limited, and examples thereof include a mercury lamp, a metal halide lamp, a xenon lamp, a chemical lamp, and a carbon arc lamp.
  • Examples of radiation include electron beams, X-rays, ion beams, and far infrared rays.
  • g-line wavelength 436 nm
  • i-line wavelength 365 nm
  • deep ultraviolet light Deep-UV light
  • high-density energy beam laser beam
  • Specific examples of preferred embodiments include scanning exposure with an infrared laser, high-illuminance flash exposure such as a xenon discharge lamp, and infrared lamp exposure.
  • the wavelength range of the light emitted from the light source or the light irradiated on the coating film is preferably at least 200 to 1200 nm.
  • An example of a light source that can emit such light is a xenon lamp.
  • the light emitted from the light source described above often includes at least one light selected from the group consisting of a wavelength of 370 nm or less and a wavelength of 800 nm or more.
  • the light by light irradiation is preferably light from a flash lamp, and more preferably pulsed light.
  • the light irradiation is preferably light irradiation with a flash lamp, and more preferably pulsed light irradiation (eg, pulsed light irradiation with a xenon (Xe) flash lamp).
  • Irradiation with high-energy pulsed light can concentrate and heat the surface of the portion to which the coating film has been applied in a very short time, so that the influence of heat on the resin substrate can be extremely reduced.
  • the irradiation energy of the pulsed light is preferably 1 to 100 J / cm 2 and more preferably 1 to 30 J / cm 2 .
  • the pulse width is preferably 1 ⁇ sec to 100 msec, and more preferably 10 ⁇ sec to 10 msec.
  • the pulse light irradiation interval is preferably 0.5 msec to 10 sec, more preferably 0.5 msec to 5 sec, and even more preferably 1 to 5 sec.
  • the light irradiation is preferably performed a plurality of times, more preferably 2 to 10 times.
  • the atmosphere in which the light irradiation treatment is performed is not particularly limited, and examples thereof include an air atmosphere, an inert atmosphere, or a reducing atmosphere.
  • the inert atmosphere refers to an atmosphere filled with an inert gas such as argon, helium, neon, or nitrogen.
  • the reducing atmosphere refers to an atmosphere in which a reducing gas such as hydrogen or carbon monoxide exists.
  • a conductive film containing metal is obtained.
  • a metal copper film is obtained.
  • the film thickness of the conductive film is not particularly limited, and an optimum film thickness is appropriately adjusted according to the intended use. Of these, 0.01 to 1000 ⁇ m is preferable and 0.1 to 100 ⁇ m is more preferable from the viewpoint of printed wiring board use.
  • the film thickness is a value (average value) obtained by measuring three or more thicknesses at arbitrary points on the conductive film and arithmetically averaging the values.
  • the volume resistivity of the conductive film is preferably less than 1000 ⁇ ⁇ cm, more preferably less than 300 ⁇ ⁇ cm, and even more preferably less than 100 ⁇ ⁇ cm from the viewpoint of conductive characteristics.
  • the volume resistivity can be calculated by measuring the surface resistance value of the conductive film by the four-probe method and then multiplying the obtained surface resistance value by the film thickness.
  • the conductive film may be provided on the entire surface of the resin base material or in a pattern.
  • the patterned conductive film is useful as a conductor wiring (wiring) such as a printed wiring board.
  • a method for obtaining a patterned conductive film for example, a method for applying a composition for forming a conductive film to a resin substrate in a pattern and performing light irradiation treatment, or patterning a conductive film provided on the entire surface of the resin substrate. And a method of etching into a shape.
  • the etching method is not particularly limited, and for example, a known subtractive method or semi-additive method can be employed.
  • an insulating layer (insulating resin layer, interlayer insulating film, solder resist) is further laminated on the surface of the patterned conductive film, and further wiring (metal) is formed on the surface. Pattern) may be formed.
  • the material of the insulating film is not particularly limited.
  • epoxy resin glass epoxy resin, aramid resin, crystalline polyolefin resin, amorphous polyolefin resin, fluorine-containing resin (polytetrafluoroethylene, perfluorinated polyimide, perfluorinated) Amorphous resin), polyimide resin, polyether sulfone resin, polyphenylene sulfide resin, polyether ether ketone resin, liquid crystal resin, and the like.
  • an epoxy resin, a polyimide resin, or a liquid crystal resin and more preferably an epoxy resin. Specific examples include ABF GX-13 manufactured by Ajinomoto Fine Techno Co., Ltd.
  • solder resist which is a kind of insulating layer material used for wiring protection, is described in detail in, for example, Japanese Patent Application Laid-Open No. 10-204150 and Japanese Patent Application Laid-Open No. 2003-222993. These materials can also be applied to the present invention if desired.
  • solder resist commercially available products may be used. Specific examples include PFR800 manufactured by Taiyo Ink Manufacturing Co., Ltd., PSR4000 (trade name), SR7200G manufactured by Hitachi Chemical Co., Ltd., and the like.
  • the resin base material (resin base material with a conductive film) having the conductive film obtained above can be used for various applications.
  • a printed wiring board a TFT (thin film transistor, an abbreviation for Thin (Transistor), an FPC (an abbreviation for Flexible Printed Circuits), RFID (an abbreviation for radio frequency identifier), and the like can be given.
  • Cupric oxide nanoparticles 1 Cupric oxide nanoparticles with an average primary particle diameter of 28 nm prepared by vapor phase method (12 parts by mass) and polyethylene glycol (weight average molecular weight 20000, Wako Pure Chemical Industries, Ltd.) (The same applies hereinafter.) (2 parts by mass), ethylene glycol (0.6 parts by mass), palladium acetate (0.12 parts by mass) as a catalyst, acetone (5.88 parts by mass), Ion exchange water is added to and mixed with ethanol (30 parts by mass) so that the total composition becomes 100 parts by mass, and the mixture is processed for 5 minutes with a rotation revolution mixer (manufactured by THINKY, Awatori Kentaro ARE-250). Thus, a conductive film forming composition 1 was produced.
  • a polyethylene naphthalate (PEN) base material Q65HA, thickness 125 ⁇ m, manufactured by Teijin DuPont
  • the conductive film-forming composition 1 manufactured as described above was applied with a bar so that the wet thickness was 12 ⁇ m.
  • a coating film was obtained by drying at 0 ° C. for 1 minute. Thereafter, the obtained coating film was irradiated with pulsed light (pulse width 2 ms) at intervals of 3 seconds at an irradiation energy and the number of irradiations shown in Table 1 using a Xenon light sintering apparatus Sinteron 2000. Obtained.
  • pulsed light pulse width 2 ms
  • an optical filter 1 (UV hot mirror manufactured by Edmund) as a light reducing means is placed between the light source and the conductive film forming composition 1, and the optical filter is applied to the conductive film forming composition 1.
  • the light transmitted through 1 was irradiated.
  • the optical filter 1 can reduce light having a wavelength of 800 nm or more by 70% or more.
  • the transmittance of light with a wavelength of 900 nm of the optical filter 1 is 15% or less.
  • the optical filter 1 can transmit 75% or more of light having a wavelength in the range of more than 450 nm and less than 650 nm.
  • the transmittance of light having a wavelength of 500 nm of the optical filter 1 is 80% or more.
  • the transmittance of light having a wavelength of 370 nm is 80% or more.
  • ⁇ Defect evaluation> The obtained conductive film was observed at a magnification of 450 times using an optical microscope, and the presence or absence of defects and the state of defects were evaluated based on the following criteria. Practically, it is preferably A to B. The results are shown in Table 1. “A”: There was no crack (defect) having a width of 20 ⁇ m or more in 1 mm 2 of the conductive film. “B”: There were less than 10 cracks (defects) having a width of 20 ⁇ m or more in 1 mm 2 of the conductive film. “C”: There were 10 or more cracks (defects) having a width of 20 ⁇ m or more in 1 mm 2 of the conductive film.
  • volume resistivity was measured using the four-probe method resistivity meter, and electroconductivity was evaluated.
  • the evaluation criteria are as follows. In practice, it is required to be A, B or C.
  • the results are shown in Table 1. “A”: Volume resistivity was less than 100 ⁇ ⁇ cm. “B”: Volume resistivity was 100 ⁇ ⁇ cm or more and less than 300 ⁇ ⁇ cm. “C”: Volume resistivity was 300 ⁇ ⁇ cm or more and less than 1000 ⁇ ⁇ cm. “D”: Volume resistivity was 1000 ⁇ ⁇ cm or more.
  • Example 2 A conductive film was produced in the same manner as in Example 1 except that the optical filter 2 (KG-1 manufactured by Edmund) was used instead of the optical filter 1.
  • the optical filter 2 can reduce light having a wavelength of 300 nm or less and a wavelength of 800 nm or more by 60% or more.
  • the transmittance of light having a wavelength of 370 nm of the optical filter 2 is 90% or more.
  • the transmittance of light with a wavelength of 900 nm of the optical filter 2 is 10% or less.
  • the optical filter 2 can transmit 90% or more of light in the wavelength range of more than 450 nm and less than 650 nm.
  • the transmittance of light having a wavelength of 500 nm of the optical filter 2 is 90% or more.
  • Example 3 A conductive film was produced in the same manner as in Example 1 except that instead of the optical filter 1, an optical filter 3 (Sharp Cut Filter SCF-50S-37L manufactured by Sigma Kogyo Co., Ltd.) was used.
  • the optical filter 3 can reduce light having a wavelength of 370 nm or less by 40% or more.
  • the transmittance of light with a wavelength of 370 nm of the optical filter 3 is 40%, and the transmittance of light with a wavelength of 300 nm is 0%.
  • the optical filter 3 can transmit 85% or more of light having a wavelength in the range of more than 450 nm and less than 650 nm.
  • the transmittance of light with a wavelength of 500 nm of the optical filter 3 is 90% or more.
  • Example 4> (Synthesis of cupric oxide nanoparticles 2) A predetermined amount of copper nitrate (manufactured by Wako Pure Chemical Industries, Ltd.) was dissolved in purified water, and a 0.1 mol / l aqueous copper nitrate solution was prepared in advance. 100 ml of purified water was placed in a glass 200 ml flask and heated to 90 ° C. in an oil bath. 20 ml each of the copper nitrate aqueous solution and 0.2 mol / l sodium hydroxide aqueous solution were added thereto within 10 seconds and heated for 10 minutes to obtain cupric oxide fine particles.
  • the particles are recovered by centrifugation (10000 G, 30 minutes), redispersed in water, and then subjected to ultrafiltration to remove impurities, and then the copper oxide having a particle concentration of 40 mass% (wt%).
  • a paste was obtained.
  • XRD analysis strong diffraction peaks derived from the (002) and (111) planes were observed near 35.5 ° and 38 °, respectively, and it was confirmed that the obtained particles were cupric oxide.
  • the obtained cupric oxide nanoparticles 2 had an average primary particle size of 18 nm.
  • a conductive film was produced in the same manner as in Example 1 except that the conductive film forming composition 2 was used instead of the conductive film forming composition 1.
  • Example 5> A conductive film was produced in the same manner as in Example 4 except that the optical filter 3 was used instead of the optical filter 1.
  • “Near Infrared” means that light having a wavelength of 800 nm or more is cut out of the light transmitted through the optical filter.
  • the term “ultraviolet light” intends that light having a wavelength of 370 nm or less (optical filter 3) or a wavelength of 300 nm or less (optical filter 2) is cut out of the light transmitted through the optical filter.
  • Example 2 using the dimming means for reducing the light intensity at wavelengths of 300 nm or less and wavelengths of 800 nm or more was superior in conductivity to Examples 1 and 3.
  • Comparative Example 1 that did not use the light reduction means had lower conductivity than Examples 1 to 3, and many defects occurred. Further, Comparative Example 2 that did not use the dimming means had more defects than Examples 4 and 5. In Comparative Examples 1 and 2, since the resin base material absorbs light intensity having a wavelength of 370 nm or less and a wavelength of 800 nm or more due to the absence of a light-reducing means, the conductive film cracks in the conductive film due to generation of gas, etc. It is probable that this defect occurred.

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Abstract

L'objectif de la présente invention est de fournir un procédé de fabrication d'un film conducteur avec lequel il est possible de supprimer l'apparition de défauts et de former un film conducteur présentant une excellente conductivité. Ce procédé de fabrication d'un film conducteur comprend : une première étape de formation d'un film de revêtement par revêtement d'un substrat de résine avec une composition formant un film conducteur contenant des nanoparticules d'un métal ou d'un composé métallique ; et une seconde étape de formation d'un film conducteur par exposition du film de revêtement à de la lumière. De la lumière exposée sur le film de revêtement lors de la deuxième étape, au moins une intensité de lumière choisie dans le groupe constitué de longueurs d'onde inférieures ou égales à 370 nm et de longueurs d'onde supérieures ou égales à 800 nm est réduite.
PCT/JP2015/070559 2014-08-29 2015-07-17 Procédé de fabrication de film conducteur WO2016031426A1 (fr)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013206719A (ja) * 2012-03-28 2013-10-07 Fujifilm Corp 導電膜の製造方法
WO2013172399A1 (fr) * 2012-05-18 2013-11-21 コニカミノルタ株式会社 Procédé pour la fabrication d'un substrat conducteur, substrat conducteur, et élément électronique organique
JP2014148633A (ja) * 2013-02-04 2014-08-21 Fujifilm Corp 導電膜形成用組成物、導電膜の製造方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013206719A (ja) * 2012-03-28 2013-10-07 Fujifilm Corp 導電膜の製造方法
WO2013172399A1 (fr) * 2012-05-18 2013-11-21 コニカミノルタ株式会社 Procédé pour la fabrication d'un substrat conducteur, substrat conducteur, et élément électronique organique
JP2014148633A (ja) * 2013-02-04 2014-08-21 Fujifilm Corp 導電膜形成用組成物、導電膜の製造方法

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