WO2015174348A1 - 導電ペースト、タッチパネル及び導電パターンの製造方法 - Google Patents
導電ペースト、タッチパネル及び導電パターンの製造方法 Download PDFInfo
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- WO2015174348A1 WO2015174348A1 PCT/JP2015/063352 JP2015063352W WO2015174348A1 WO 2015174348 A1 WO2015174348 A1 WO 2015174348A1 JP 2015063352 W JP2015063352 W JP 2015063352W WO 2015174348 A1 WO2015174348 A1 WO 2015174348A1
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- Prior art keywords
- conductive paste
- compound
- conductive
- conductive pattern
- pattern
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Images
Classifications
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- 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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/10—Esters
- C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
- C08F222/102—Esters of polyhydric alcohols or polyhydric phenols of dialcohols, e.g. ethylene glycol di(meth)acrylate or 1,4-butanediol dimethacrylate
- C08F222/1025—Esters of polyhydric alcohols or polyhydric phenols of dialcohols, e.g. ethylene glycol di(meth)acrylate or 1,4-butanediol dimethacrylate of aromatic dialcohols
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- 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
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/0048—Photosensitive materials characterised by the solvents or agents facilitating spreading, e.g. tensio-active agents
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/027—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds
- G03F7/028—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds with photosensitivity-increasing substances, e.g. photoinitiators
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
- G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
- H05K1/095—Dispersed materials, e.g. conductive pastes or inks for polymer thick films, i.e. having a permanent organic polymeric binder
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/30—Assembling printed circuits with electric components, e.g. with resistor
- H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
- H05K3/34—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by soldering
- H05K3/3457—Solder materials or compositions; Methods of application thereof
- H05K3/3485—Applying solder paste, slurry or powder
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/03—Conductive materials
- H05K2201/032—Materials
- H05K2201/0323—Carbon
Definitions
- the present invention relates to a method for producing a conductive paste and a conductive pattern.
- Patent Documents 1 and 2 a conductive paste in which a conductive filler is dispersed in an organic component capable of producing a fine conductive pattern by photolithography has been developed (Patent Documents 1 and 2), and in particular, with a transparent electrode such as ITO.
- a conductive paste characterized by high connection reliability has been developed (Patent Document 1).
- the present invention provides a conductive paste capable of stably maintaining contact resistance even after environmental changes such as high humidity and high heat, and capable of producing a fine and low specific resistance conductive pattern. With the goal.
- the present invention provides a conductive paste, a touch panel, and a method for manufacturing a conductive pattern described in the following (1) to (6).
- the conductive paste has a mass ratio of the metal particles (A) to 20 to 1900.
- the electrically conductive paste as described in said (1) containing an oxime ester type compound as said photoinitiator (D).
- the volume average particle diameter of the metal particles (A) is 0.1 to 10 ⁇ m, and the volume average particle diameter of primary particles of the carbon particles (B) is 0.005 to 0.5 ⁇ m.
- a method for producing a conductive pattern comprising applying the conductive paste according to any one of (1) to (4) above on a substrate, drying, exposing and developing, and then curing at 100 to 300 ° C.
- an increase in contact resistance can be suppressed even after an environmental change such as high humidity and high heat, and a fine conductive pattern having a low specific resistance can be manufactured.
- the conductive paste of the present invention contains metal particles (A), carbon particles (B), a compound having an unsaturated double bond (C), a photopolymerization initiator (D), and a solvent (E), and The mass ratio of the metal particles (A) to the carbon particles (B) is 20 to 1900.
- the conductive pattern obtained by the conductive paste of the present invention is a composite of an organic component and an inorganic component, and the metal particles (A) are brought into contact with each other by curing shrinkage during curing. To do.
- the conductive paste of the present invention contains metal particles (A).
- metal particles (A) As the metal constituting the metal particles (A), silver (hereinafter “Ag”), gold (hereinafter “Au”), copper, platinum, lead, tin, nickel, aluminum, tungsten, molybdenum, chromium, titanium, or Indium or an alloy of these metals may be mentioned, but Ag, Au or copper is preferable from the viewpoint of conductivity, and Ag is more preferable from the viewpoint of cost and stability.
- the present inventors have made extensive studies to obtain a desired conductive paste. And attention was paid to the carbon particles (B). Hitherto, it has been known to add carbon particles in order to increase the dispersibility of metal particles in the conductive paste or to adjust the conductivity. However, for that purpose, a considerable amount of carbon particles must be added, and the conductivity is lowered, that is, the specific resistance is increased.
- the present inventors paid attention to the mass ratio of the metal particles (A) to the carbon particles (B). Then, further investigations were made, and it was found that the contact resistance can be stably maintained even through environmental changes such as high humidity and high heat by adding a small amount of carbon particles. That is, the mass ratio of the metal particles (A) to the carbon particles (B) needs to be 20 to 1900, more preferably 30 to 1000.
- the contact probability between the carbon particles (B) and the transparent electrode is improved, and the contact resistance between the manufactured conductive pattern and the transparent electrode is high humidity and high heat environment. It remains stable and low even after change.
- the mass ratio of the metal particles (A) is 20 or more, the contact probability between the metal particles (A) is improved, and the specific resistance of the manufactured conductive pattern is sufficiently low.
- the volume average particle diameter of the metal particles (A) is preferably 0.1 to 10 ⁇ m, more preferably 0.5 to 6 ⁇ m.
- the volume average particle diameter is 0.1 ⁇ m or more, the contact probability between the metal particles (A) in the curing step is improved, and the specific resistance and disconnection probability of the manufactured conductive pattern are lowered.
- exposure light can smoothly pass through the coating film obtained by applying the conductive paste, facilitating fine patterning.
- the volume average particle diameter is 10 ⁇ m or less, the surface smoothness, pattern accuracy, and dimensional accuracy of the manufactured conductive pattern are improved.
- the volume average particle diameter of the metal particles (A) can be measured by a Coulter counter method.
- the addition amount of the metal particles (A) is preferably 60 to 95% by mass with respect to the total solid content in the conductive paste.
- the addition amount with respect to the total solid content is 60% by mass or more, the contact probability between the metal particles (A) during curing is improved, and the specific resistance and disconnection probability of the manufactured conductive pattern are lowered.
- the addition amount with respect to the total solid content is 95% by mass or less, the exposure light can be transmitted more smoothly through the coating film obtained by applying the conductive paste in the exposure process, and fine patterning can be performed. Becomes easy.
- the total solid content means all components of the conductive paste excluding the solvent.
- the conductive paste of the present invention contains carbon particles (B).
- the carbon particles are particles having a carbon ratio of 50% by mass or more in the whole particles.
- the carbon particles contained in the conductive paste have good wettability with ITO, particularly among transparent electrodes, so that carbon particles gather at the interface between the conductive paste and ITO, increasing the number of contact points and increasing the conductive path. Therefore, the effect of making it possible to stably maintain contact resistance even after environmental changes such as high humidity and high heat is increased.
- Examples of the carbon particles (B) include MA77, 7, 8, 11, 100, 100R, 100S, 230, 14, 220 or 600 or # 2650, 2600, 2350, 2300, 1000, 1000N, 980, 970, 960. 950, 900, 850, 750B, 650B, 52, 47, 45, 45L, 44, 40, 32, 30, 30L, 25, 20, 10, 5, 95, 85, 260, 4000B, 3030B, 3050B, 3230B Alternatively, 3400B (all manufactured by Mitsubishi Chemical Corporation), Talker Black # 8500 / F, 8300 / F, 7550SB / F, 7400, 7360SB, 7350 / F, 7270SB, 7100F, 7050, 5500, 4500, 4400, 4300 , 3855, 3845 or 3 00 (all are manufactured by Tokai Carbon Co., Ltd.), Asahi # 78, 80, 70, 70L, 66, 65, 60HN, 60H, 60U, 60,
- the volume average particle diameter of the primary particles of the carbon particles (B) is preferably 0.005 to 0.5 ⁇ m.
- the volume average particle diameter of the primary particles is 0.005 ⁇ m or more, the dispersibility and dispersion stability in the conductive paste are further increased, and the generation of aggregates can be suppressed.
- the volume average particle diameter of the primary particles exceeds 0.5 ⁇ m, the number of primary particles per certain mass decreases and the contact probability with transparent electrodes such as ITO, silver nanowires, zinc oxide or tin oxide decreases. As a result, the contact resistance between the manufactured conductive pattern and the transparent electrode may increase.
- the volume average particle diameter of the primary particles of the carbon particles (B) was determined by observing 100 primary particles randomly selected using an electron microscope, measuring the maximum width of each primary particle, It can be calculated by obtaining an average value.
- the amount of carbon particles (B) added is preferably 0.05 to 3% by mass, more preferably 0.1 to 2% by mass, based on the total solid content in the conductive paste.
- the added amount with respect to the total solid content is 0.05% by mass or more, the contact probability between the carbon particles (B) and the transparent electrode is improved, and the contact resistance between the produced conductive pattern and the transparent electrode is high humidity and high heat. It becomes low stably even in the environment.
- the addition amount with respect to the total solid content is 3% by mass or less, the exposure light can smoothly pass through the coating film obtained by applying the conductive paste in the exposure step, and fine patterning can be performed. It becomes easy.
- the conductive paste of the present invention contains a compound (C) having an unsaturated double bond.
- the compound (C) having an unsaturated double bond include styrenes such as styrene, p-methylstyrene, o-methylstyrene, m-methylstyrene, ⁇ -methylstyrene, chloromethylstyrene or hydroxymethylstyrene, Examples include acrylic monomers, 1-vinyl-2-pyrrolidone, acrylic copolymers, and epoxycarboxylate compounds.
- acrylic monomers examples include acrylic acid, methyl acrylate, ethyl acrylate, 2-ethylhexyl acrylate, n-butyl acrylate, iso-butyl acrylate, iso-propane acrylate, glycidyl acrylate, butoxytriethylene glycol acrylate, and dicyclopentanyl.
- the acrylic copolymer refers to a copolymer containing an acrylic monomer in a monomer to be used, that is, a copolymer component.
- An alkali-soluble acrylic copolymer having a carboxyl group can be obtained by using an unsaturated acid such as an unsaturated carboxylic acid as a monomer.
- unsaturated acid include acrylic acid, methacrylic acid, itaconic acid, crotonic acid, maleic acid, fumaric acid, vinyl acetate, and acid anhydrides thereof.
- the acid value of the obtained acrylic copolymer can be adjusted by the amount of the unsaturated acid used.
- the epoxycarboxylate compound refers to a compound that can be synthesized using an epoxy compound and a carboxyl compound having an unsaturated double bond as starting materials.
- examples of the epoxy compound that can be a starting material include glycidyl ethers, alicyclic epoxy resins, glycidyl esters, glycidyl amines, or epoxy resins.
- the acid value of the epoxycarboxylate compound may be adjusted by reacting the epoxycarboxylate compound with the polybasic acid anhydride.
- the polybasic acid anhydride include succinic anhydride, phthalic anhydride, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, itaconic anhydride, 3-methyltetrahydrophthalic anhydride, 4-methyl-hexahydrophthalic anhydride, Examples include trimellitic anhydride or maleic anhydride.
- an epoxy carboxylate compound has by reacting the carboxyl group which the epoxy carboxylate compound made to react with the above-mentioned polybasic acid anhydride has, and the compound which has unsaturated double bonds, such as glycidyl (meth) acrylate, The amount of the unsaturated double bond may be adjusted.
- Urethane may be formed by reacting the hydroxy group of the epoxycarboxylate compound with a diisocyanate compound.
- the diisocyanate compound include hexamethylene diisocyanate, tetramethylxylene diisocyanate, naphthalene-1,5-diisocyanate, tridenic diisocyanate, trimethylhexamethylene diisocyanate, isophorone diisocyanate, allyl cyanide diisocyanate, and norbornane diisocyanate.
- the acid value of the compound (C) having an unsaturated double bond is preferably 30 to 250 mgKOH / g in order to optimize alkali solubility. If the acid value is less than 30 mgKOH / g, the solubility of the soluble part may be lowered. On the other hand, if the acid value exceeds 250 mgKOH / g, the allowable development width may be narrowed.
- the acid value of the compound (C) having an unsaturated double bond can be measured according to JIS K 0070 (1992).
- the conductive paste of the present invention contains a photopolymerization initiator (D).
- the photopolymerization initiator (D) include 1,2-octanedione-1- [4- (phenylthio) -2- (O-benzoyloxime)], 2,4,6-trimethylbenzoyl-diphenyl-phosphine.
- Oxide bis (2,4,6-trimethylbenzoyl) -phenylphosphine oxide, ethanone-1- [9-ethyl-6-2 (2-methylbenzoyl) -9H-carbazol-3-yl] -1- (O— Acetyloxime), benzophenone, methyl o-benzoylbenzoate, 4,4′-bis (dimethylamino) benzophenone, 4,4′-bis (diethylamino) benzophenone, 4,4′-dichlorobenzophenone, 4-benzoyl-4 ′ -Methyl diphenyl ketone, dibenzyl ketone, fluorenone, 2,2'-diethoxyacetoph Non, 2,2-dimethoxy-2-phenylacetophenone, 2-hydroxy-2-methylpropiophenone, pt-butyldichloroacetophenone, thioxanthone, 2-methylthioxanthone, 2-chlorothioxan
- the amount of the photopolymerization initiator (D) added is preferably 0.05 to 30 parts by mass with respect to 100 parts by mass of the compound (C) having an unsaturated double bond.
- the added amount with respect to 100 parts by mass of the compound (C) having an unsaturated double bond is 0.05 parts by mass or more, the cured density of the exposed part increases and the residual film ratio after development can be increased.
- the addition amount with respect to 100 parts by mass of the compound (C) having an unsaturated double bond is 30 parts by mass or less, the photopolymerization initiator (D) at the upper part of the coating film obtained by applying the conductive paste Excessive light absorption due to) is suppressed. As a result, a decrease in adhesion with the substrate due to the manufactured conductive pattern having an inversely tapered shape is suppressed.
- the conductive paste of the present invention may contain a sensitizer together with the photopolymerization initiator (D).
- sensitizer examples include 2,4-diethylthioxanthone, isopropylthioxanthone, 2,3-bis (4-diethylaminobenzal) cyclopentanone, 2,6-bis (4-dimethylaminobenzal) cyclohexanone, 2 , 6-bis (4-dimethylaminobenzal) -4-methylcyclohexanone, Michler's ketone, 4,4-bis (diethylamino) benzophenone, 4,4-bis (dimethylamino) chalcone, 4,4-bis (diethylamino) chalcone P-dimethylaminocinnamylidene indanone, p-dimethylaminobenzylidene indanone, 2- (p-dimethylaminophenylvinylene) isonaphthothiazole, 1,3-bis (4-dimethylaminophenylvinylene) isonaphthothiazole,
- the addition amount of the sensitizer is preferably 0.05 to 10 parts by mass with respect to 100 parts by mass of the compound (C) having an unsaturated double bond.
- Photosensitivity improves that the addition amount with respect to 100 mass parts of compound (C) which has an unsaturated double bond is 0.05 mass part or more.
- the addition amount with respect to 100 parts by mass of the compound (C) having an unsaturated double bond is 10 parts by mass or less, excessive light absorption at the upper part of the coating film obtained by applying the conductive paste is suppressed. Is done. As a result, a decrease in adhesion with the substrate due to the manufactured conductive pattern having an inversely tapered shape is suppressed.
- the conductive paste of the present invention contains a solvent (E).
- the solvent (E) include N, N-dimethylacetamide, N, N-dimethylformamide, N-methyl-2-pyrrolidone, dimethylimidazolidinone, dimethyl sulfoxide, ⁇ -butyrolactone, ethyl lactate, 1-methoxy -2-propanol, 1-ethoxy-2-propanol, ethylene glycol mono-n-propyl ether, diacetone alcohol, tetrahydrofurfuryl alcohol, propylene glycol monomethyl ether acetate, diethylene glycol monoethyl ether acetate, diethylene glycol monomethyl ether, diethylene glycol monoethyl Ether acetate (hereinafter “DMEA”), diethylene glycol monobutyl ether, diethylene glycol monobutyl ether acetate, triethylene glycol Chi glycol dimethyl ether, or 2,2,4, - but-trimethyl-1,3
- the conductive paste of the present invention is a non-photosensitive polymer or plasticizer that does not have an unsaturated double bond in the molecule, a leveling agent, a surfactant, a silane coupling agent, as long as the desired properties are not impaired. You may contain additives, such as an antifoamer or a pigment.
- non-photosensitive polymer examples include an epoxy resin, a novolac resin, a phenol resin, a polyimide precursor, and a closed ring polyimide.
- plasticizer examples include dibutyl phthalate, dioctyl phthalate, polyethylene glycol, and glycerin.
- leveling agent examples include a special vinyl polymer or a special acrylic polymer.
- silane coupling agent examples include methyltrimethoxysilane, dimethyldiethoxysilane, phenyltriethoxysilane, hexamethyldisilazane, 3-methacryloxypropyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, and vinyltrimethoxysilane. Methoxysilane is mentioned.
- the conductive paste of the present invention is manufactured using a dispersing machine or a kneader such as a three-roller, ball mill or planetary ball mill.
- the method for producing a conductive pattern of the present invention is characterized in that the conductive paste of the present invention is applied onto a substrate, dried, exposed and developed, and then cured at 100 to 300 ° C.
- a coating film is obtained by applying the conductive paste of the present invention on a substrate.
- Examples of the substrate to which the conductive paste of the present invention is applied include a polyethylene terephthalate film (hereinafter referred to as “PET film”), a polyimide film, a polyester film, an aramid film, an epoxy resin substrate, a polyetherimide resin substrate, and a polyetherketone resin substrate. And a polysulfone resin substrate, a glass substrate, a silicon wafer, an alumina substrate, an aluminum nitride substrate, a silicon carbide substrate, a decorative layer forming substrate, and an insulating layer forming substrate.
- PET film polyethylene terephthalate film
- Examples of the method for applying the conductive paste of the present invention to a substrate include spin coating using a spinner, spray coating, roll coating, screen printing, or coating using a blade coater, die coater, calendar coater, meniscus coater, or bar coater. Is mentioned.
- the film thickness of the coating film to be obtained may be appropriately determined according to the coating method or the total solid content concentration or viscosity of the conductive paste, but the film thickness after drying is preferably 0.1 to 50 ⁇ m. .
- the film thickness can be measured using a stylus step meter such as Surfcom (registered trademark) 1400 (manufactured by Tokyo Seimitsu Co., Ltd.). More specifically, the film thicknesses at three randomly selected positions are measured with a stylus type step gauge (measurement length: 1 mm, scanning speed: 0.3 mm / sec), and the average value thereof is obtained. Can be calculated.
- the obtained coating film is dried to evaporate the solvent.
- Examples of the method for drying the coating film to volatilize and remove the solvent include heat drying or vacuum drying using an oven, a hot plate, infrared rays, or the like.
- the heating temperature is preferably 50 to 180 ° C., and the heating time is preferably 1 minute to several hours.
- the coating film after drying is exposed by a photolithography method through an arbitrary pattern forming mask.
- a light source for exposure i-line (365 nm), h-line (405 nm) or g-line (436 nm) of a mercury lamp is preferable.
- the coated film after exposure is developed using a developer, and unexposed portions are dissolved and removed to obtain a desired pattern.
- the developer used for alkali development include tetramethylammonium hydroxide, diethanolamine, diethylaminoethanol, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, triethylamine, diethylamine, methylamine, dimethylamine, and dimethyl acetate.
- Aminoethyl, dimethylaminoethanol, dimethylaminoethyl methacrylate, cyclohexylamine, ethylenediamine or hexamethylenediamine aqueous solutions may be mentioned.
- aqueous solutions include N-methyl-2-pyrrolidone, N, N-dimethylformamide, N, N -Polar solvents such as dimethylacetamide, dimethylsulfoxide or ⁇ -butyrolactone; alcohols such as methanol, ethanol or isopropanol; Esters such as Le or propylene glycol monomethyl ether acetate, may be added to ketones or surfactants such as cyclopentanone, cyclohexanone, isobutyl ketone or methyl isobutyl ketone.
- Examples of the developer for organic development include N-methyl-2-pyrrolidone, N-acetyl-2-pyrrolidone, N, N-dimethylacetamide, N, N-dimethylformamide, dimethyl sulfoxide or hexamethylphosphoryl
- Examples thereof include polar solvents such as amides or mixed solutions of these polar solvents and methanol, ethanol, isopropyl alcohol, xylene, water, methyl carbitol, or ethyl carbitol.
- a development method for example, a method of spraying a developer onto the coating film surface while the substrate is left standing or rotating, a method of immersing the substrate in the developer, or an ultrasonic wave while immersing the substrate in the developer The method of applying is mentioned.
- the pattern obtained by development may be rinsed with a rinse solution.
- a rinse solution examples include water or an aqueous solution in which an alcohol such as ethanol or isopropyl alcohol or an ester such as ethyl lactate or propylene glycol monomethyl ether acetate is added to water.
- the obtained pattern is cured at 100 to 300 ° C.
- the curing temperature is preferably 120 to 180 ° C.
- the curing temperature is less than 100 ° C., the volume shrinkage of the resin component is not increased and the specific resistance is not sufficiently lowered.
- the curing temperature exceeds 300 ° C., a conductive pattern cannot be produced on a material such as a substrate having low heat resistance.
- thermo drying for example, heat drying with an oven, an inert oven or a hot plate, an electromagnetic wave such as an ultraviolet lamp, an infrared heater, a halogen heater or a xenon flash lamp, or heat drying with microwaves, or Vacuum drying is mentioned.
- Heating increases the hardness of the laminated pattern to be manufactured, can suppress chipping or peeling due to contact with other members, and can improve adhesion to the substrate.
- the touch panel of the present invention includes a conductive pattern formed of the conductive paste of the present invention and a transparent electrode made of ITO, and the transparent electrode is connected to the conductive pattern.
- the conductive pattern manufactured using the conductive paste of the present invention is suitably used as a peripheral wiring for a touch panel provided with a transparent electrode made of ITO.
- the carbon particles contained in the conductive paste have good wettability with ITO, particularly among the transparent electrodes. Therefore, carbon particles gather at the interface between the conductive paste and ITO, increasing the number of contact points, and conducting. This is because the number of paths increases, thereby increasing the effect of stably maintaining contact resistance even after environmental changes such as high humidity and high heat.
- Examples of the touch panel system include a resistance film type, an optical type, an electromagnetic induction type, and a capacitance type. Since the capacitive touch panel requires particularly fine wiring, the conductive paste of the present invention is more preferably used.
- the capacitive touch panel since it is necessary to transmit an electric signal from the transparent electrode to the IC chip, it is necessary that at least a part of the surrounding wiring is formed on the transparent electrode.
- the conductive pattern produced using the conductive paste of the present invention is more preferably used because it has excellent connection reliability with ITO.
- a touch panel provided with a conductive pattern manufactured by the manufacturing method of the present invention as its peripheral wiring, and the peripheral wiring is 50 ⁇ m pitch (wiring width + inter-wiring width) or less
- the frame width can be reduced and the view area can be widened. can do.
- ⁇ Patternability evaluation method> The conductive paste was applied on a PET film so that the film thickness after drying was 7 ⁇ m, and the obtained coating film was dried in a drying oven at 100 ° C. for 5 minutes.
- a photomask having a straight line group arranged in a certain line and space hereinafter referred to as “L / S”
- L / S a photomask having a straight line group arranged in a certain line and space
- the coating film after drying was exposed and developed to obtain nine types of patterns with different L / S values. Thereafter, all the nine patterns obtained were cured in a drying oven at 140 ° C. for 30 minutes to obtain nine types of conductive patterns having different L / S values.
- the L / S value of each unit of the photomask is such that the line width ( ⁇ m) / interval ( ⁇ m) is 500/500, 250/250, 100/100, 50/50, 40/40, 30/30, 25/25, 20/20, 15/15.
- the obtained conductive pattern was observed with an optical microscope. A conductive pattern having a minimum L / S value with no residue between the patterns and no pattern peeling was confirmed.
- the L / S value was defined as a developable L / S value. A pattern that disappeared due to over-development was called a “pattern flow”.
- the exposure was performed using an exposure apparatus (PEM-6M; manufactured by Union Optical Co., Ltd.) with an exposure amount of 150 mJ / cm 2 (wavelength 365 nm conversion), and the development was performed with a 0.2 mass% Na 2 CO 3 solution.
- the substrate was immersed for 30 seconds, and then rinsed with ultrapure water.
- the conductive paste was applied on a PET film so that the film thickness after drying was 7 ⁇ m, and the obtained coating film was dried in a drying oven at 100 ° C. for 5 minutes.
- the coating film after drying was exposed and developed through a photomask having a translucent pattern A shown in FIG. 1 to obtain a pattern.
- the obtained pattern was cured in a drying oven at 140 ° C. for 30 minutes to obtain a conductive pattern for specific resistance measurement.
- the line width of the obtained conductive pattern was 0.400 mm, and the line length was 80 mm.
- the exposure and development conditions were the same as in the patterning evaluation method.
- the resistance values were measured by connecting the respective ends of the obtained conductive pattern for measuring specific resistance with a resistance meter, and the specific resistance was calculated based on the following formula (1). The thing with no continuity was defined as “insulation”.
- Specific resistance resistance value ⁇ film thickness ⁇ line width / line length (1).
- the conductive paste was applied on a transparent conductive film having a transparent electrode formed on the entire surface of the PET film so that the film thickness after drying was 7 ⁇ m, and the obtained coating film was dried in a drying oven at 100 ° C. for 5 minutes.
- the coating film after drying was exposed and developed through a photomask having a translucent pattern A shown in FIG. 2 to obtain a pattern.
- the obtained pattern was cured in a drying oven at 140 ° C. for 30 minutes to obtain a connection reliability evaluation sample with a transparent electrode.
- the line width of the conductive pattern in the obtained sample was 0.100 mm, the distance between the lines was 5 mm, and the terminal portion was a circle having a diameter of 2 mm.
- the sample was stored in a constant temperature and humidity chamber (LU-113; ESPEC Corporation) at 85 ° C. and 85% RH for 500 hours. did. Then, the terminal part of the electroconductive pattern in the taken out sample was connected with a tester, the resistance value after storage was measured, and the resistance change rate was calculated based on the following formula (2).
- a resistance change rate calculated as 1.30 or less was determined as A, a value greater than 1.30 and not greater than 1.50 as B, and a value greater than 1.50 as C.
- Resistance change rate resistance value after storage (after 500 hours) / initial resistance value (2).
- the measured initial resistance value and post-storage resistance value are obtained by adding the resistance value of the conductive pattern and the resistance value of the transparent electrode to the value of the contact resistance between the conductive pattern and the transparent electrode.
- the resistance value of the conductive pattern and the resistance value of the transparent electrode are extremely small compared to the value of the contact resistance, it is possible to evaluate the rate of change of the contact resistance with the initial resistance value and the resistance value after storage. .
- Metal particles (A) Au particles having a volume average particle diameter of 1.0 ⁇ m and Ag particle volume average particle diameter of 1.0 ⁇ m.
- Carbon particles (B) Carbon particles having a volume average particle diameter of primary particles of 0.05 ⁇ m (ratio of carbon in the entire particles: 99% by mass).
- IRGACURE registered trademark
- OXE-01 manufactured by Ciba Japan Co., Ltd.
- IRGACURE registered trademark 369 (hereinafter “IC-369”; manufactured by Ciba Japan Co., Ltd.).
- ITO film manufactured by Nitto Denko Corporation
- Silver nanowire film manufactured by Hitachi Chemical Co., Ltd.
- Example 1 In a 100 mL clean bottle, put 10.0 g of compound (C-1), 0.50 g of OXE-01, 5.0 g of DMEA and 2.0 g of BP-4EA. The mixture was mixed with “ARE-310 (registered trademark; manufactured by Shinky Corporation)” to obtain 17.5 g of a resin solution (solid content: 71.4% by mass).
- ARE-310 registered trademark; manufactured by Shinky Corporation
- the patterning property of the conductive pattern, the specific resistance, and the connection reliability with ITO were evaluated.
- the developable L / S value which is an evaluation index of patterning property, was 15/15 ⁇ m, and it was confirmed that favorable pattern processing was performed.
- the specific resistance of the conductive pattern was 5.5 ⁇ 10 ⁇ 5 ⁇ cm.
- the rate of change in resistance in the connection reliability evaluation with ITO was 1.03, which was good.
- Example 2 A conductive paste having the composition shown in Table 1 was produced by the same method as in Example 1, and the results of the same evaluation as in Example 1 are shown in Table 2.
- the conductive paste of the present invention can be suitably used for manufacturing a conductive pattern such as a peripheral wiring for a touch panel.
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Abstract
Description
(1) 金属粒子(A)、カーボン粒子(B)、不飽和二重結合を有する化合物(C)、光重合開始剤(D)、及び、溶剤(E)を含有し、上記カーボン粒子(B)に対する上記金属粒子(A)の質量比が、20~1900である、導電ペースト。
(2) 上記光重合開始剤(D)として、オキシムエステル系化合物を含有する、上記(1)に記載の導電ペースト。
(3) 上記金属粒子(A)の体積平均粒子径が、0.1~10μmであり、かつ、上記カーボン粒子(B)の一次粒子の体積平均粒子径が、0.005~0.5μmである、上記(1)又は(2)に記載の導電ペースト。
(4) 不飽和二重結合を有する化合物(C)の酸価が、30~250mgKOH/gである、上記(1)~(3)のいずれかに記載の導電ペースト。
(5) 上記(1)~(4)のいずれかに記載の導電ペーストから形成された導電パターンと、ITOからなる透明電極と、を備え、上記透明電極と、上記導電パターンとが接続されている、タッチパネル。
(6) 上記(1)~(4)のいずれかに記載の導電ペーストを基板上に塗布し、乾燥し、露光し、現像した後に、100~300℃でキュアする、導電パターンの製造方法。
PETフィルム上に、導電ペーストを乾燥後の膜厚が7μmになるように塗布し、得られた塗布膜を100℃の乾燥オーブン内で5分間乾燥した。一定のラインアンドスペース(以下、「L/S」)で配列された直線群すなわち透光パターンを1つのユニットとし、L/Sの値が異なる9種類のユニットをそれぞれ有するフォトマスクを介して、乾燥後の塗布膜を露光及び現像して、L/Sの値が異なる9種類のパターンをそれぞれ得た。その後、得られた9つのパターンを30分間、140℃の乾燥オーブン内でいずれもキュアして、L/Sの値が異なる9種類の導電パターンをそれぞれ得た。フォトマスクが有する各ユニットのL/Sの値は、ライン幅(μm)/間隔(μm)が、500/500、250/250、100/100、50/50、40/40、30/30、25/25、20/20、15/15である。得られた導電パターンを光学顕微鏡で観察した。パターン間に残渣がなく、かつパターン剥がれのない、L/Sの値が最小の導電パターンを確認した。そのL/Sの値を、現像可能なL/Sの値とした。過現像となり、パターンが消失したものを「パターン流れ」とした。
PETフィルム上に、導電ペーストを乾燥後の膜厚が7μmになるように塗布し、得られた塗布膜を100℃の乾燥オーブン内で5分間乾燥した。図1に示す透光パターンAを有するフォトマスクを介して、乾燥後の塗布膜を露光及び現像して、パターンを得た。その後、得られたパターンを30分間、140℃の乾燥オーブン内でキュアして、比抵抗測定用の導電性パターンを得た。得られた導電性パターンのライン幅は0.400mmであり、ライン長さは80mmであった。
比抵抗 = 抵抗値×膜厚×線幅/ライン長 ・・・ (1)。
PETフィルムに透明電極が全面形成された透明導電フィルム上に、導電ペーストを乾燥後の膜厚が7μmになるように塗布し、得られた塗布膜を100℃の乾燥オーブンで5分間乾燥した。図2に示す透光パターンAを有するフォトマスクを介して、乾燥後の塗布膜を露光及び現像して、パターンを得た。その後、得られたパターンを30分間、140℃の乾燥オーブン内でキュアして、透明電極との接続信頼性評価サンプルを得た。得られたサンプルにおける導電性パターンのライン幅は0.100mmであり、ライン間は5mmであり、端子部は直径2mmの円形であった。
抵抗変化率=保管後抵抗値(500時間後)/初期抵抗値 ・・・ (2)。
体積平均粒子径が1.0μmのAg粒子
体積平均粒子径が1.0μmのAu粒子。
一次粒子の体積平均粒子径が0.05μmのカーボン粒子(粒子全体に占める炭素の割合:99質量%)。
(モノマー)
ライトアクリレートBP-4EA(以下、「BP-4EA」;共栄社化学(株)製)
(合成例1:化合物(C-1))
共重合比率(質量基準):エチルアクリレート(以下、「EA」)/メタクリル酸2-エチルヘキシル(以下、「2-EHMA」)/スチレン(以下、「St」)/グリシジルメタクリレート(以下、「GMA」)/アクリル酸(以下、「AA」)=20/40/20/5/15
窒素雰囲気の反応容器中に、150gのDMEAを仕込み、オイルバスを用いて80℃まで昇温した。これに、20gのEA、40gの2-EHMA、20gのSt、15gのAA、0.8gの2,2’-アゾビスイソブチロニトリル及び10gのDMEAからなる混合物を、1時間かけて滴下した。滴下終了後、さらに6時間重合反応を行った。その後、1gのハイドロキノンモノメチルエーテルを添加して、重合反応を停止した。引き続き、5gのGMA、1gのトリエチルベンジルアンモニウムクロライド及び10gのDMEAからなる混合物を、0.5時間かけて滴下した。滴下終了後、さらに2時間付加反応を行った。得られた反応溶液をメタノールで精製することで未反応不純物を除去し、さらに24時間真空乾燥することで、化合物(C-1)を得た。得られた化合物(C-1)の酸価は103mgKOH/gであった。
共重合比率(質量基準):エチレンオキサイド変性ビスフェノールAジアクリレート(FA-324A;日立化成工業(株)製)/EA/GMA/AA=60/25/10/5
窒素雰囲気の反応容器中に、150gのDMEAを仕込み、オイルバスを用いて80℃まで昇温した。これに、60gのエチレンオキサイド変性ビスフェノールAジアクリレート、25gのEA、5gのAA、0.8gの2,2’-アゾビスイソブチロニトリル及び10gのDMEAからなる混合物を、1時間かけて滴下した。滴下終了後、さらに6時間重合反応を行った。その後、1gのハイドロキノンモノメチルエーテルを添加して、重合反応を停止した。引き続き、10gのGMA、1gのトリエチルベンジルアンモニウムクロライド及び10gのDMEAからなる混合物を、0.5時間かけて滴下した。滴下終了後、さらに2時間付加反応を行った。得られた反応溶液をメタノールで精製することで未反応不純物を除去し、さらに24時間真空乾燥することで、カルボキシル基及び不飽和二重結合を有する化合物(C-2)を得た。得られた化合物(C-2)の酸価は1.4mgKOH/gであった。
窒素雰囲気の反応溶液中に、123gのRE-310S(日本化薬(株)製)、47gのAA、0.3gのハイドロキノンモノメチルエーテル及び0.5gのトリフェニルホスフィンを仕込み、98℃の温度で反応液の酸価が0.5mgKOH/g以下になるまで反応させ、化合物(C-3)を得た。得られた化合物(C-3)の酸価は0.4mgKOH/gであった。
窒素雰囲気の反応溶液中に、164gのカルビトールアセテート、287gのEOCN-103S(日本化薬(株)製)、96gのAA、2gの2,6-ジ-tert-ブチル-p-クレゾール及び2gのトリフェニルホスフィンを仕込み、98℃の温度で反応液の酸価が0.5mgKOH/g以下になるまで反応させ、エポキシカルボキシレート化合物を得た。引き続き、この反応液に57gのカルビトールアセテート及び67gのテトラヒドロ無水フタル酸を仕込み、95℃で4時間反応させ、化合物(C-4)を得た。得られた化合物(C-4)の酸価は104mgKOH/gであった。
窒素雰囲気の反応容器中に、123gのRE-310S(日本化薬(株)製)、47gのAA、0.3gのハイドロキノンモノメチルエーテル及び0.5gのトリフェニルホスフィンを仕込み、98℃の温度で反応液の酸価が0.5mgKOH/g以下になるまで反応させ、エポキシカルボキシレート化合物を得た。その後、この反応溶液に252gのカルビトールアセテート、89gの2,2-ビス(ジメチロール)-プロピオン酸、0.4gの2-メチルハイドロキノン及び47gのスピログリコールを加え、45℃に昇温した。この溶液に162gのトリメチルヘキサメチレンジイソシアネートを、反応温度が65℃を超えないように徐々に滴下した。滴下終了後、反応温度を80℃に上昇させ、赤外吸収スペクトル測定法により、2250cm-1付近の吸収がなくなるまで6時間反応させ、化合物(C-5)を得た。得られた化合物(C-5)の酸価は80.0mgKOH/gであった。
窒素雰囲気の反応容器に、300gのデナコールEX-203(ナガセケムテックス(株)製)のアクリル酸付加物(分子量:368)、500gのDMEA、0.5gの2-メチルハイドロキノン及び200gの2,2-ビス(ヒドロキシメチル)プロピオン酸を仕込み、45℃に昇温した。この溶液に201.3gのトルエンジイソシアネートを、反応温度が50℃を超えないように徐々に滴下した。滴下終了後、反応温度を80℃に上昇させ、赤外吸収スペクトル測定法により、2250cm-1付近の吸収がなくなるまで6時間反応させた。この溶液に120gのグリシジルメタクリレートを加え、95℃に昇温して6時間反応させ、化合物(C-6)を得た。得られた化合物(C-6)の酸価は83mgKOH/gであった。
IRGACURE(登録商標)OXE-01(以下、「OXE-01」;チバジャパン(株)製)
IRGACURE(登録商標)369(以下、「IC-369」;チバジャパン(株)製)。
DMEA(東京化成工業(株)製)。
ITOフィルム(日東電工(株)製)
銀ナノワイヤーフィルム(日立化成(株)製)。
100mLクリーンボトルに、10.0gの化合物(C-1)、0.50gのOXE-01、5.0gのDMEA及び2.0gのBP-4EAを入れ、自転-公転真空ミキサー“あわとり錬太郎”ARE-310(登録商標;(株)シンキー製)で混合して、17.5gの樹脂溶液(固形分71.4質量%)を得た。
表1に示す組成の導電ペーストを実施例1と同様の方法で製造し、実施例1と同様の評価を行った結果を表2に示す。
表1に示す組成の導電ペーストを実施例1と同様の方法で製造し、実施例1と同様の評価を行った結果を表2に示す。
Claims (6)
- 金属粒子(A)、
カーボン粒子(B)、
不飽和二重結合を有する化合物(C)、
光重合開始剤(D)、及び、
溶剤(E)を含有し、
前記カーボン粒子(B)に対する前記金属粒子(A)の質量比が、20~1900である、導電ペースト。 - 前記光重合開始剤(D)として、オキシムエステル系化合物を含有する、請求項1記載の導電ペースト。
- 前記金属粒子(A)の体積平均粒子径が、0.1~10μmであり、かつ、
前記カーボン粒子(B)の一次粒子の体積平均粒子径が、0.005~0.5μmである、請求項1又は2記載の導電ペースト。 - 前記不飽和二重結合を有する化合物(C)の酸価が、30~250mgKOH/gである、請求項1~3のいずれか一項記載の導電ペースト。
- 請求項1~4のいずれか一項記載の導電ペーストから形成された導電パターンと、ITOからなる透明電極と、を備え、前記透明電極と、前記導電パターンとが接続されている、タッチパネル。
- 請求項1~4のいずれか一項記載の導電ペーストを、基板上に塗布し、乾燥し、露光し、現像した後に、100~300℃でキュアする、導電パターンの製造方法。
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JPWO2015174348A1 (ja) | 2017-04-20 |
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