WO2016171083A1 - 導電パターン形成部材の製造方法 - Google Patents
導電パターン形成部材の製造方法 Download PDFInfo
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- WO2016171083A1 WO2016171083A1 PCT/JP2016/062150 JP2016062150W WO2016171083A1 WO 2016171083 A1 WO2016171083 A1 WO 2016171083A1 JP 2016062150 W JP2016062150 W JP 2016062150W WO 2016171083 A1 WO2016171083 A1 WO 2016171083A1
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- conductive pattern
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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
- G03F7/0047—Photosensitive materials characterised by additives for obtaining a metallic or ceramic pattern, e.g. by firing
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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
- G03F7/20—Exposure; Apparatus therefor
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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
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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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
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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
- C08F222/12—Esters of phenols or saturated alcohols
- C08F222/20—Esters containing oxygen in addition to the carboxy oxygen
- C08F222/205—Esters containing oxygen in addition to the carboxy oxygen the ester chains containing seven or more carbon atoms
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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
- C09D133/00—Coating compositions based on homopolymers or 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/08—Homopolymers or copolymers of acrylic acid esters
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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
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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
- G03F7/038—Macromolecular compounds which are rendered insoluble or differentially wettable
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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
- G03F7/038—Macromolecular compounds which are rendered insoluble or differentially wettable
- G03F7/0388—Macromolecular compounds which are rendered insoluble or differentially wettable with ethylenic or acetylenic bands in the side chains of the photopolymer
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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
- G03F7/09—Photosensitive materials characterised by structural details, e.g. supports, auxiliary layers
- G03F7/11—Photosensitive materials characterised by structural details, e.g. supports, auxiliary layers having cover layers or intermediate layers, e.g. subbing layers
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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
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/40—Treatment after imagewise removal, e.g. baking
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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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- 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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- 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
- G03F7/16—Coating processes; Apparatus therefor
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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
- G03F7/26—Processing photosensitive materials; Apparatus therefor
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F2203/00—Indexing scheme relating to G06F3/00 - G06F3/048
- G06F2203/041—Indexing scheme relating to G06F3/041 - G06F3/045
- G06F2203/04103—Manufacturing, i.e. details related to manufacturing processes specially suited for touch sensitive devices
Definitions
- the present invention relates to a method for manufacturing a conductive pattern forming member.
- the display electrode formed in the display area of the capacitive touch panel is a transparent electrode made of ITO (indium tin oxide) or the like.
- ITO indium tin oxide
- a metal thin film such as ITO is formed on the base material by sputtering or the like, and a photoresist, which is a photosensitive resin, is further applied to the surface and exposed through a photomask.
- etching and resist removal are performed.
- Patent Documents 1 and 2 disclose Technology has also been devised.
- peripheral wiring connected to the transparent electrode is formed around the display area.
- a method of forming this peripheral wiring a method of finely processing a conductive paste having photosensitivity by a photolithography method is known (Patent Documents 3 to 7).
- this conductive paste is used to form a peripheral wiring connected to a transparent electrode pattern formed from a base material on which the photosensitive resin layer and the transparent electrode layer are laminated, the photosensitivity formed on the base material It is necessary to apply the conductive paste to the surface of the resin layer and the transparent electrode layer before processing.
- the conductive paste coating film is not exposed in the development process after the conductive paste is exposed through the photomask. Residues are not only generated when the portions are dissolved and removed, but ion migration between the formed conductive pattern and the photosensitive resin layer is regarded as a problem.
- the present invention provides a method for producing a conductive pattern forming member that is excellent in ion migration resistance between a conductive pattern formed on a substrate and a photosensitive resin layer while suppressing generation of a residue in dissolution removal of an unexposed portion.
- the purpose is to provide.
- the present inventors have found that it is extremely effective in solving the above problems that the conductive particles used in the formation of the conductive pattern contain conductive particles that satisfy a certain condition. As a result, the present invention was completed.
- conductive particles, double bonds, and carboxyl groups are formed on the surface of the layer A made of a resin having a carboxyl group (a) and the transparent electrode layer B formed on the substrate.
- the composition C containing the resin (c) is applied to obtain a coating film C, a coating process, a drying process of drying the coating film C to obtain a dry film C, and the exposure of the dry film C.
- a method for producing a conductive pattern forming member wherein the proportion of particles having a particle size of 0.3 to 2.0 ⁇ m in the conductive particles is 80% or more.
- a conductive pattern forming member of the present invention it is possible to suppress the generation of residues in the dissolution and removal of unexposed portions, and to have an ion migration resistance with a layer made of a resin having a carboxyl group formed on a substrate. An excellent conductive pattern can be formed.
- the ion migration resistance can be further enhanced by laminating OCA having a benzotriazole-based compound or an isobornyl skeleton.
- conductive particles on the surface of the layer A formed of a resin (a) having a carboxyl group and a transparent electrode layer B formed on a base material and two A coating step of applying a composition C containing a resin (c) having a heavy bond and a carboxyl group to obtain a coating film C; and a drying step of drying the coating film C to obtain a dry film C.
- a ratio of particles having a particle size of 0.3 to 2.0 ⁇ m in the conductive particles is 80% or more.
- the coating step provided in the method for producing a conductive pattern forming member of the present invention is a step of obtaining a coating film C by coating the composition C on the surface of the resin layer A and the transparent electrode layer B.
- the transparent electrode layer B is laminated on a layer A (hereinafter “resin layer A”) made of a resin (a) having a carboxyl group (hereinafter “resin (a)”). And the resin layer A is formed on the base material.
- resin layer A made of a resin (a) having a carboxyl group (hereinafter “resin (a)”).
- the base material on which the resin layer A is formed refers to a support for forming a transparent electrode layer, a conductive pattern or the like on the surface.
- Examples of the base material include a rigid substrate such as glass, a glass epoxy substrate or a ceramic substrate, or a flexible substrate such as a polyester film or a polyimide film.
- the resin layer A formed on the base material is a so-called photosensitive resin layer and functions as a photoresist for pattern formation of the transparent electrode layer B.
- the resin (a) constituting the resin layer A has a carboxyl group in its molecular chain and is alkali-soluble.
- Examples of the resin (a) include an acrylic copolymer, an epoxycarboxylate compound, a polyamic acid, or a siloxane polymer.
- An acrylic copolymer or an epoxy carboxylate compound having a high visible light transmittance is preferable.
- An acrylic copolymer having a carboxyl group can be obtained by copolymerizing an acrylic monomer and an unsaturated acid such as an unsaturated carboxylic acid as a copolymerization component.
- acrylic monomer examples include acrylic acid (hereinafter “AA”), methyl acrylate, ethyl acrylate (hereinafter “EA”), 2-ethylhexyl acrylate, n-butyl acrylate (hereinafter “BA”), iso- Butyl acrylate, iso-propane acrylate, glycidyl acrylate, butoxytriethylene glycol acrylate, dicyclopentanyl acrylate, dicyclopentenyl acrylate, 2-hydroxyethyl acrylate, isobornyl acrylate, 2-hydroxypropyl acrylate, isodexyl acrylate, Isooctyl acrylate, lauryl acrylate, 2-methoxyethyl acrylate, methoxyethylene glycol acrylate, methoxydiethylene glycol acrylate , Octafluoropentyl acrylate, phenoxyethyl acrylate, stearyl acrylate, triflu
- the unsaturated acid examples include acrylic acid, methacrylic acid, itaconic acid, crotonic acid, maleic acid, fumaric acid, vinyl acetate, and acid anhydrides thereof.
- the acid value of the resulting acrylic copolymer can be adjusted by the amount of the unsaturated acid used as the copolymer component.
- 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, and epoxy resins. More specifically, for example, methyl glycidyl ether, ethyl glycidyl ether, butyl glycidyl ether, ethylene glycol diglycidyl ether, diethylene glycol diglycidyl ether, propylene glycol diglycidyl ether, tripropylene glycol diglycidyl ether, neopentyl glycol diglycidyl ether Bisphenol A diglycidyl ether, hydrogenated bisphenol A diglycidyl ether, bisphenol F diglycidyl ether, bisphenol S diglycidyl ether, bisphenol fluorenediglycidyl ether, biphenol diglycidyl ether, tetramethylbiphenol glycidyl ether, trimethyl
- Examples of the carboxyl compound having an unsaturated double bond that can be used as a starting material include (meth) acrylic acid, crotonic acid, cinnamic acid, and ⁇ -cyanocinnamic acid.
- 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 is obtained by reacting a carboxyl group of an epoxy carboxylate compound whose acid value is adjusted with the above polybasic acid anhydride and a compound having an unsaturated double bond such as glycidyl (meth) acrylate. You may adjust the quantity of the reactive unsaturated double bond which has.
- 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 resin (a) is preferably 50 to 250 mgKOH / g since the resin layer A functions as an alkali-soluble photoresist, and 60 to 150 mgKOH / g in order to further improve pattern processability. Is more preferable.
- the acid value of the resin (a) can be measured according to JIS K 0070 (1992).
- the visible light transmittance of the resin layer A is preferably 80% or more when the conductive pattern forming member manufactured by the manufacturing method of the present invention is a constituent element of the touch panel.
- the transparent electrode layer B laminated on the resin layer A is not an entirely flat layer, but is an arbitrarily shaped pattern that is patterned using the function of the resin layer A as a photoresist. . That is, the transparent electrode layer does not completely cover the resin layer A, but the resin layer A is exposed at a portion where the pattern of the transparent electrode layer B is not formed.
- the transparent electrode layer B consists only of a conductive component or contains a conductive component.
- the conductive component constituting the transparent electrode layer B include indium, tin, zinc, gallium, antimony, titanium, zirconium, magnesium, aluminum, gold, silver, copper, palladium, tungsten, oxides of these metals, or carbon nanotubes. Is mentioned. More specifically, for example, indium tin oxide (hereinafter “ITO”), indium zinc oxide, indium oxide-zinc oxide composite oxide, aluminum zinc oxide, gallium zinc oxide, fluorine zinc oxide, fluorine Indium oxide, antimony tin oxide, or fluorine tin oxide may be used.
- ITO indium tin oxide
- ITO or fibrous silver (hereinafter referred to as “silver fiber”), which has high conductivity and visible light transmittance and is advantageous in terms of price, is preferable, and has high connection reliability with the conductive pattern C described later. Fiber is more preferred.
- Examples of the method for forming the transparent electrode layer before pattern processing include a vacuum deposition method, a sputtering method, an ion plating method, and a coating method.
- the thickness of the transparent electrode layer B is preferably 0.01 to 1.5 ⁇ m in order to achieve both good conductivity and visible light transmittance. Further, the visible light transmittance of the transparent electrode layer B is preferably 80% or more for the same reason as the resin layer A.
- composition C applied to the surface of the resin layer A and the transparent electrode layer B contains conductive particles and a resin (c) having a double bond and a carboxyl group (hereinafter “resin (c)”). To do.
- Examples of the conductive particles contained in the composition C include silver, gold, copper, platinum, lead, tin, nickel, aluminum, tungsten, molybdenum, chromium, titanium, indium, and alloys of these metals. Silver, gold or copper is preferred, and silver is more preferred because of its high stability and advantageous price.
- the aspect ratio which is a value obtained by dividing the major axis length by the minor axis length, is preferably 1.0 to 3.0, more preferably 1.0 to 2.0. preferable.
- the aspect ratio of the conductive particles is 1.0 or more, the contact probability between the conductive particles is further increased.
- the aspect ratio of the conductive particles is 2.0 or less, the exposure light is not easily shielded in the exposure process described later, and the development margin is widened.
- the aspect ratio of the conductive particles is determined by observing the conductive particles with a scanning electron microscope (SEM) or a transmission electron microscope (TEM), and randomly selecting primary particles of 100 conductive particles. It can be determined by measuring the major axis length and minor axis length and determining the aspect ratio from the average value of both.
- the particle size of the conductive particles is preferably 0.3 to 2.0 ⁇ m, more preferably 0.5 to 1.5 ⁇ m.
- the resin layer A swells due to the components contained in the composition C, and the conductive particles are taken into the resin layer A, and a residue is easily generated.
- the particle diameter of the conductive particles is 0.3 ⁇ m or more, the conductive particles taken into the resin layer A are easily exposed in the development process described later, and can be washed away. As a result, ion migration is performed. Resistance is improved.
- the particle size of the conductive particles is 2.0 ⁇ m or less, the straightness of the obtained conductive pattern C is increased.
- the proportion of particles having a particle size of 0.3 to 2.0 ⁇ m in the conductive particles contained in the composition C is: It is necessary to be 80% or more, and preferably 90% or more.
- the particle size of the conductive particles is obtained by observing the conductive particles with an electron microscope, randomly selecting the primary particles of 20 conductive particles, measuring the maximum width of each, and obtaining the average value thereof. Can be calculated.
- the proportion of the particles having a particle size of 0.3 to 2.0 ⁇ m in the conductive particles contained in the composition C is determined by observing the conductive particles with an electron microscope, and randomly 100 primary particles of the conductive particles. And the maximum width of each is measured, and the maximum width can be determined from the proportion of primary particles in the range of 0.3 to 2.0 ⁇ m.
- the particle size of the conductive particles contained in the conductive pattern C is such that the collected conductive pattern C is dissolved in tetrahydrofuran (hereinafter referred to as “THF”), the precipitated conductive particles are recovered, and 70 ° C. using a box oven. It can calculate similarly to the above about what dried for 10 minutes.
- THF tetrahydrofuran
- the proportion of the conductive particles in the solid content of the composition C is preferably 60 to 95% by mass.
- the proportion of the conductive particles is 60% by mass or more, the contact probability between the conductive particles is increased, and the resistance value of the obtained conductive pattern C can be stabilized.
- the ratio of the conductive particles is 95% by mass or less, the exposure light is not easily shielded in the exposure process described later, and the development margin is widened.
- solid content means all the components of the composition C except a solvent.
- Examples of the resin (c) contained in the composition C include an acrylic copolymer or an epoxycarboxylate compound. In order to improve the adhesiveness of the obtained conductive pattern C, an epoxy carboxylate compound is preferable.
- An acrylic copolymer having a double bond and a carboxyl group can be obtained by copolymerizing an acrylic monomer and an unsaturated acid having a carboxyl group and an unsaturated double bond as a copolymerization component.
- the unsaturated acid include AA, methacrylic acid, itaconic acid, crotonic acid, maleic acid, fumaric acid, vinyl acetate, and acid anhydrides thereof.
- the acid value of the resulting acrylic copolymer can be adjusted by the amount of the unsaturated acid used as the copolymer component.
- the acid value of the resin (c) is preferably the same as that of the resin (a). Moreover, the acid value of resin (c) can be measured similarly to resin (a).
- Composition C may contain a photopolymerization initiator.
- the photopolymerization initiator 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′-methyldiphenyl Ketone, dibenzyl ketone, fluorenone, 2,2'
- the addition amount of the photopolymerization initiator is preferably 0.05 to 30 parts by mass with respect to 100 parts by mass of the resin (c).
- the addition amount of the photopolymerization initiator is 0.05 parts by mass or more, the cured density of the exposed part increases, and the remaining film ratio after development can be increased.
- the addition amount of the photopolymerization initiator is 30 parts by mass or less, excessive light absorption by the photopolymerization initiator at the top of the coating film C obtained by applying the composition C is suppressed. .
- a decrease in adhesion with the resin layer A due to the resulting conductive pattern C having an inversely tapered shape is suppressed.
- Composition C may contain a sensitizer together with the photopolymerization initiator.
- 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 resin (c). Photosensitivity improves that the addition amount of a sensitizer is 0.05 mass part or more. On the other hand, when the addition amount of the sensitizer is 10 parts by mass or less, excessive light absorption at the upper part of the coating film C obtained by applying the conductive paste is suppressed. As a result, a decrease in adhesion with the resin layer A due to the manufactured conductive pattern C having an inversely tapered shape is suppressed.
- Composition C may contain a solvent.
- a solvent an alcohol solvent having a boiling point of 200 ° C. or higher, which has high solubility of the resin (c) and hardly causes uneven coating due to volatilization of the solvent, is preferable. Examples of the alcohol solvent having a boiling point of 200 ° C.
- diethylene glycol triethylene glycol, 1,3-butanediol, glycerin, benzyl alcohol, dipropylene glycol, 1,4-butanediol, octanediol, 2,2,4 Trimethyl 1,3-pentanediol monoisobutyrate, ethylene glycol mono-2-ethylhexyl ether, 2,4-diethyl-1,5-pentanediol, 2-butyl-2-ethyl-1,3-propanediol, 3,5,5-trimethyl-1-hexanol, isodecanol, isotridecanol or ethylene glycol monohexyl ether.
- the amount of the solvent added is preferably 10 to 200 parts by mass with respect to 100 parts by mass of the resin (c). It is easy to control the film thickness of the coating film of the composition C uniformly as the addition amount of a solvent is 10 mass parts or more. On the other hand, when the amount of the solvent added is 200 parts by mass or less, it is possible to suppress sedimentation of the conductive particles that occurs during storage of the composition C.
- Composition C may contain an epoxy resin.
- the epoxy resin include ethylene glycol-modified epoxy resin, bisphenol A type epoxy resin, hydrogenated bisphenol A type epoxy resin, brominated epoxy resin, bisphenol F type epoxy resin, novolac type epoxy resin, alicyclic epoxy resin, glycidyl.
- examples include amine type epoxy resins, glycidyl ether type epoxy resins, and heterocyclic epoxy resins.
- a bisphenol A type epoxy resin or a hydrogenated bisphenol A type epoxy resin is preferable, and a hydrogenated bisphenol A type epoxy resin having a high exposure light transmittance is more preferable. preferable.
- the addition amount of the epoxy resin is 0.05 to 20 parts by mass of the epoxy resin with respect to 100 parts by mass of the resin (c). Adhesion can be improved. On the other hand, when the addition amount of the epoxy resin is 20 parts by mass or less, the solubility of the exposure film C in the developer is improved.
- Examples of the method of applying the composition C 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.
- the drying step included in the method for producing a conductive pattern forming member of the present invention is a step of drying the coating film C to obtain the dry film C.
- the film thickness of the obtained dry film C is preferably 1 to 20 ⁇ m.
- the film thickness of the dry film C can be measured using a stylus type step meter (for example, Surfcom (registered trademark) 1400; manufactured by Tokyo Seimitsu Co., Ltd.). More specifically, the film thicknesses at three randomly selected positions were measured with a stylus-type step gauge (measurement length: 1 mm, scanning speed: 0.3 mm / sec), and the average value thereof was determined as a dry film.
- the film thickness can be C.
- Examples of the method for drying the coating film C include heat drying or vacuum drying using a box oven, a hot plate, infrared rays, or the like.
- the heating temperature is preferably 50 to 80 ° C, more preferably 60 to 80 ° C.
- the heating temperature is 50 ° C. or higher, the amount of solvent or the like contained in the dry film C is sufficiently reduced, and the development margin is widened.
- the heating temperature is 80 ° C. or lower, the resin layer A is difficult to swell and the conductive particles taken into the resin layer A are reduced, so that a residue in the development process is hardly generated.
- the heating time is preferably 1 minute to several hours.
- the heating temperature refers to the temperature at which the substrate surface is measured with a K thermocouple.
- the exposure step included in the method for producing a conductive pattern forming member of the present invention is a step of exposing the coating film C to obtain a dry film C.
- Examples of the light source for exposure include a high pressure mercury lamp, an ultrahigh pressure mercury lamp, or an LED that emits i-line (365 nm), h-line (405 nm), or g-line (436 nm).
- Examples of the exposure method include vacuum suction exposure, proxy exposure, projection exposure, and direct drawing exposure.
- the developing step included in the method for producing a conductive pattern forming member of the present invention is a step of developing the exposed film C and dissolving and removing the unexposed portion to obtain a desired pattern C.
- Examples of 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.
- An aqueous solution of aminoethyl, dimethylaminoethanol, dimethylaminoethyl methacrylate, cyclohexylamine, ethylenediamine or hexamethylenediamine may be mentioned.
- polar solvents such as N-methyl-2-pyrrolidone, N, N-dimethylformamide, N, N-dimethylacetamide, dimethyl sulfoxide or ⁇ -butyrolactone, alcohols such as methanol, ethanol or isopropanol, ethyl lactate
- esters such as propylene glycol monomethyl ether acetate, ketones such as cyclopentanone, cyclohexanone, isobutyl ketone or methyl isobutyl ketone, or a surfactant may be added.
- 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 developing method for example, a method of spraying a developing solution onto the surface of the exposure film C while the substrate is allowed to stand or rotate, a developing vessel in which a number of nozzles for discharging the developing solution are arranged, Examples thereof include a method of passing through a conveyor, a method of immersing in a developer, and a method of applying ultrasonic waves while immersing a substrate in the developer. From the viewpoint of uniformly developing a large area, development in which the substrate is passed through a conveyor through the developing tank is preferable. In that case, the pressure of the developer discharged from the nozzle is preferably 0.02 to 0.2 MPa.
- the pattern C obtained in the development process may be rinsed with a rinse solution.
- the rinsing liquid 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 curing step provided in the method for producing a conductive pattern forming member of the present invention is a step of obtaining the conductive pattern C by curing the pattern C.
- the curing temperature is preferably 100 to 300 ° C, more preferably 120 to 180 ° C.
- the curing temperature is less than 100 ° C.
- the volume shrinkage of the resin (c) does not increase, and the specific resistance of the conductive pattern C obtained does not become sufficiently low.
- the curing temperature exceeds 300 ° C., a conductive pattern cannot be formed on a substrate having low heat resistance.
- Examples of the curing method include heat drying using an oven, inert oven or hot plate, electromagnetic wave such as an ultraviolet lamp, infrared heater, halogen heater or xenon flash lamp, heat drying using microwaves, or vacuum drying. .
- electromagnetic wave such as an ultraviolet lamp, infrared heater, halogen heater or xenon flash lamp
- heat drying using microwaves or vacuum drying.
- the difference (SA-SC value) between the acid value SA of the resin layer A and the organic component acid value SC of the conductive pattern C is preferably 20 to 150 mgKOH / g. It is more preferably 30 to 100 mg KOH / g, and further preferably 40 to 90 mg KOH / g.
- the obtained conductive pattern C is highly hygroscopic due to the resin (c) having a carboxyl group, and an ion migration phenomenon starting from the conductive particles easily occurs due to the influence.
- the resin layer A preferentially absorbs moisture, so that the moisture absorption of the conductive pattern C is suppressed, and as a result, the ion migration resistance of the conductive pattern forming member is improved. Can be made.
- the SA-SC value is 150 mgKOH / g or less, the amount of hydrogen bonds between the carboxyl groups of the resin (a) and the resin (c) contained in the resin layer A and the conductive pattern C is increased. The adhesion between the resin layer A and the conductive pattern C can be improved.
- the value of SA is calculated by dissolving 1 part by mass of the collected resin layer A in 100 parts by mass of THF and titrating the solution with a 0.1 mol / L potassium hydroxide solution using a phenolphthalein solution as an indicator. can do.
- the SC value was determined by first dissolving 1 part by mass of the collected conductive pattern C in 10 parts by mass of THF, removing the conductive particles with a filter or the like, and then adding 0.1 mol / l of the solution using a phenolphthalein solution as an indicator.
- the acid value of the conductive pattern C can be calculated by titration with an L potassium hydroxide solution.
- the epoxy resin when contained in the composition C, it can react with a carboxyl group in a curing process, and the organic component acid value of the conductive pattern C can be lowered.
- the conductive pattern forming member of the present invention can be covered with an OCA (Optical Clear Adhesive) layer D having a benzotriazole compound or an isobornyl skeleton for the purpose of suppressing migration.
- OCA Optical Clear Adhesive
- benzotriazole compounds include 1H-benzotriazole (1,2,3-benzotriazole), 4-methylbenzotriazole, 5-methylbenzotriazole, benzotriazole-1-methylamine, 4-methylbenzotriazole-1-methyl Amine, 5-methylbenzotriazole-1-methylamine, N-methylbenzotriazole-1-methylamine, N-ethylbenzotriazole-1-methylamine, N, N-dimethylbenzotriazole-1-methylamine, N, N-diethylbenzotriazole-1-methylamine, N, N-dipropylbenzotriazole-1-methylamine, N, N-dibutylbenzotriazole-1-methylamine, N, N-dihexylbenzotriazole-1-methylamine , N, N Dioctylbenzotriazole-1-methylamine, N, N-dimethyl-4-benzotriazole-1-methylamine, N, N-dimethyl-5-benzotriazole-1
- Examples of the compound having an isobornyl skeleton include isobornyl acetate, isobornyl acrylate, isobornyl methacrylate, isobornyl cyclohexanol, etc., and these compounds may be contained as one of the components of the acrylic copolymer. Good.
- the OCA material for forming the OCA layer D is obtained by applying a pressure-sensitive adhesive containing the above compound onto a release-treated substrate and drying it.
- the OCA layer D can be formed by thermocompression bonding of the obtained OCA material with a thermal laminator or the like.
- the touch panel of the present invention includes a conductive pattern forming member manufactured by the manufacturing method of the present invention. More specifically, the conductive pattern forming member manufactured by the manufacturing method of the present invention is suitably used as a member for a touch panel. Examples of the touch panel system include a resistive film type, an optical type, an electromagnetic induction type, and a capacitance type. Since the capacitance type touch panel requires particularly fine wiring, the conductive pattern formation of the present invention is performed. A member is used more suitably. In the touch panel provided with the conductive pattern C 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 reduced. Can be wide.
- St 2-EHMA / styrene
- GMA glycidyl methacrylate
- the acrylic copolymer solution was diluted with ethyl acetate to a resin solid content of 30%, and 1.2 g of Duranate P301-75E (Asahi Kasei Co., Ltd .; solid content 75%) was added thereto.
- the product was coated on a 50 ⁇ m PET film having one surface released from the mold so that the thickness after drying was 25 ⁇ m, and dried at 75 ° C. for 5 minutes to obtain OCA (d-2).
- Example 1 A biaxially stretched polyethylene terephthalate film having a thickness of 30 ⁇ m was prepared as a substrate. A composition A1 in which resin (a-1), MPD-A, and OXE-01 are mixed at a ratio of 100: 50: 1 is applied to one side of the substrate, and heat treatment and drying are performed. A 4 ⁇ m resin layer A1 was formed. ⁇ Formation of transparent electrode layer B> An ITO thin film made of ITO and having a thickness of 22 nm was formed on the surface of the resin layer A using a sputtering apparatus equipped with an ITO sintered body target.
- a photomask is brought into close contact with the ITO thin film, the resin layer A1 and the ITO thin film are exposed with an exposure amount of 200 mJ / cm 2 with an exposure machine having an ultra-high pressure mercury lamp, and further 200 mJ / cm 2 without passing through the photomask.
- the resin layer A1 and the ITO thin film were exposed on the entire surface with an exposure amount, and then subjected to spray development with a 1% by mass aqueous sodium carbonate solution at 30 ° C. for 30 seconds to form a patterned transparent electrode layer B1 on the resin layer A1.
- composition C ⁇ Preparation of composition C>
- a resin solution C1 solid content: 70.1% by mass
- 17.0 g of the obtained resin solution C1 and 68.0 g of silver particles were mixed and kneaded using a three roller mill (EXAKT M-50; manufactured by EXAKT) to obtain 85.0 g of composition C1. It was.
- the composition C1 is applied to the surface of the resin layer A1 and the patterned transparent electrode layer B1 with a screen printer so that the dry film C1 has a thickness of 5 ⁇ m, dried at 70 ° C. for 10 minutes, and then given photo
- a 0.2 mass% aqueous sodium carbonate solution is spray-developed at a pressure of 0.1 MPa for 30 seconds, and then at 140 ° C. for 60 seconds.
- the conductive pattern forming member 1 was manufactured by curing for a minute.
- the acid value SA of the resin layer A1 of the conductive pattern forming member 1 was 98 mgKOH / g
- the organic component acid value SC of the conductive pattern C1 was 55 mgKOH / g
- the value of SA-SC was 43 mgKOH / g.
- the total light transmittance T 0 (of the resin layer A alone) of the portion where the composition C is not applied is measured in the same manner, and the decrease rate of T with respect to T 0 is calculated. Based on good / bad judgment.
- the results are shown in Table 2.
- Reduction rate is 10% or less: Good reduction rate is over 10%:
- Defect ⁇ Evaluation of ion migration resistance> The conductive pattern forming member 1 on which the conductive pattern C1 shown in FIG. 2 is formed is put into a high-temperature and high-humidity tank at 85 ° C. and 85% RH, and a voltage of DC5V is applied from the terminal portion, and the resistance value suddenly increases by 3 digits. The decreasing short circuit time was confirmed. The same evaluation was repeated with a total of ten conductive pattern forming members 1, and the average value thereof was taken as the value of ion migration resistance. The results are shown in Table 2.
- Example 2 In the case where the transparent electrode layer B is silver fiber, a conductive pattern forming member having the conditions shown in Table 1 was produced by the same method as in Example 1 except that the transparent electrode layer B was formed by the following method, and the same evaluation as in Example 1 was performed. . The results are shown in Table 2.
- a photomask is adhered to the silver fiber thin film, the resin layer A2 and the silver fiber thin film are exposed at an exposure amount of 200 mJ / cm 2 with an exposure machine having an ultrahigh pressure mercury lamp, and further 200 mJ / cm without passing through the photomask.
- spray development is performed with a 1% by mass aqueous sodium carbonate solution at 30 ° C. for 30 seconds to form a patterned transparent electrode layer B2 on the resin layer A2. did.
- Example 15 A conductive pattern forming member was manufactured in the same manner as in Example 1.
- the laminated layer 6 shown in FIG. 5 is obtained by laminating the resin layer A1, the patterned transparent electrode layer B1, and the conductive pattern C1 on the surface of OCA (d-1) under the conditions of 80 ° C. and pressing pressure of 0.5 MPa.
- Laminated members 7 shown in FIG. The laminated members 6 and 7 were evaluated in the same manner as in Example 1. The results are shown in Table 2. (Examples 16 to 17) Conductive pattern forming members shown in Table 1 were produced in the same manner as in Example 15 and evaluated in the same manner as in Example 1. The results are shown in Table 2.
- the conductive pattern forming member manufactured by the manufacturing method of the present invention can be suitably used as a constituent element of a touch panel.
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Abstract
Description
なお組成物Cにエポキシ樹脂が含有されている場合、キュア工程でカルボキシル基と反応し、導電パターンCの有機成分酸価を下げることができる。
(合成例1)
共重合比率(質量基準):EA/メタクリル酸2-エチルヘキシル(以下、「2-EHMA」)/BA/N-メチロールアクリルアミド(以下、「MAA」)/AA=20/40/20/5/15
窒素雰囲気の反応容器中に、150gのジエチレングリコールモノエチルエーテルアセテート(以下、「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BA、5gのMAA、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。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、樹脂(a-1)を得た。得られた樹脂(a-1)の酸価は103mgKOH/gであった。
共重合比率(質量基準):EA/2-EHMA/BA/MAA/AA=20/20/20/15/25
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、20gの2-EHMA、20gのBA、5gのMAA、25g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。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、樹脂(a-2)を得た。得られた樹脂(a-2)の酸価は153mgKOH/gであった。
共重合比率(質量基準):EA/2-EHMA/BA/MAA/AA=30/20/10/25/15
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、30gのEA、20gの2-EHMA、10gのBA、25gのMAA、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。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、樹脂(a-3)を得た。得られた樹脂(a-3)の酸価は101mgKOH/gであった。
共重合比率(質量基準):EA/2-EHMA/BA/グリシジルメタクリレート(以下、「GMA」)/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BA、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、樹脂(a-4)を得た。得られた樹脂(a-4)の酸価は107mgKOH/gであった
[樹脂(c)]
(合成例5)
共重合比率(質量基準):EA/2-EHMA/スチレン(以下、「St」)/グリシジルメタクリレート(以下、「GMA」)/AA=20/40/25/5/10
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、25gのSt、10g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、樹脂(c-1)を得た。得られた樹脂(c-1)の酸価は73mgKOH/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=60/20/5/15
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、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、20gのEA、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、樹脂(c-2)を得た。得られた樹脂(c-2)の酸価は104mgKOH/gであった。
窒素雰囲気の反応溶液中に、492.1gのカルビトールアセテート、860.0gのEOCN-103S(日本化薬(株)製;クレゾールノボラック型エポキシ樹脂;エポキシ当量:215.0g/当量)、288.3gのAA、4.92gの2,6-ジ-tert-ブチル-p-クレゾール及び4.92g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0.5mg・KOH/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169.8gのカルビトールアセテート及び201.6g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、樹脂(c-3)を得た。得られた樹脂(c-3)の酸価は104mgKOH/gであった。
窒素雰囲気の反応容器中に、368.0gのRE-310S(日本化薬(株)製;エポキシ当量:184.0g/当量)、141.2gのAA、1.02gのハイドロキノンモノメチルエーテル及び1.53g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755.5gのカルビトールアセテート、268.3gの2,2-ビス(ジメチロール)-プロピオン酸、1.08gの2-メチルハイドロキノン及び140.3gのスピログリコールを加え、45℃に昇温した。この溶液に485.2g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、樹脂(c-4)を得た。得られた樹脂(c-4)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GMAを加え、95℃に昇温して6時間反応させ、樹脂(c-5)を得た。得られた化合物(c-5)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)
[モノマー]
・ライトアクリレートMPD-A(以下、「MPD-A」;共栄社化学(株)製)
[アルコール系溶剤]
・ジエチレングリコール(以下、「DEG」)
[エポキシ樹脂]
・jER(登録商標)828(以下、「828」;三菱化学(株)製)
・jER(登録商標)YX-8000(以下、「YX-8000」;三菱化学(株)製)
[透明電極材料]
・ITO(酸化インジウム97質量%、酸化スズ3質量%)
・銀繊維(線径5nm、線長5μm)
[OCA(d)]
(合成例10)
窒素雰囲気の反応容器中に、150gの酢酸エチルを仕込み、オイルバスを用いて80℃まで昇温した。これに、50.0gのEA、10.0gの2-ヒドロキシエチルアクリレート、0.8gの2,2’-アゾビスイソブチロニトリル及び10gの酢酸エチルからなる混合物を、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。
次に上記アクリル共重合体溶液に1gの1,2,3-ベンゾトリアゾールを添加し、樹脂固形分が30%になるように酢酸エチルで希釈し、そこへ1.2gのデュラネートP301-75E(旭化成(株)製;固形分75%)を添加したものを片面を離型処理された50μmのPETフィルム上に乾燥後の厚さが25μmになるように塗工して、75℃で5分間乾燥することでOCA(d-1)を得た。
窒素雰囲気の反応容器中に、150gの酢酸エチルを仕込み、オイルバスを用いて80℃まで昇温した。これに、50.0gのイソボルニルメタクリレート、10.0gの2-ヒドロキシエチルアクリレート、0.8gの2,2’-アゾビスイソブチロニトリル及び10gの酢酸エチルからなる混合物を、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。
次に上記アクリル共重合体溶液を酢酸エチルで樹脂固形分が30%になるように希釈し、そこへ1.2gのデュラネートP301-75E(旭化成(株)製;固形分75%)を添加したものを片面を離型処理された50μmのPETフィルム上に乾燥後の厚さが25μmになるように塗工して、75℃で5分間乾燥することでOCA(d-2)を得た。
窒素雰囲気の反応容器中に、150gの酢酸エチルを仕込み、オイルバスを用いて80℃まで昇温した。これに、50.0gのイソボルニルメタクリレート、10.0gの2-ヒドロキシエチルアクリレート、0.8gの2,2’-アゾビスイソブチロニトリル及び10gの酢酸エチルからなる混合物を、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。
次に上記アクリル共重合体溶液に1gの1,2,3-ベンゾトリアゾールを添加し、樹脂固形分が30%になるように酢酸エチルで希釈し、そこへ1.2gのデュラネートP301-75E(旭化成(株)製;固形分75%)を添加したものを片面を離型処理された50μmのPETフィルム上に乾燥後の厚さが25μmになるように塗工して、75℃で5分間乾燥することでOCA(d-3)を得た。
<樹脂層Aの形成>
基材として、厚さ30μmの二軸延伸ポリエチレンテレフタレートフィルムを用意した。基材の片面に、樹脂(a-1)、MPD-A及びOXE-01がそれぞれ100:50:1の割合で混合された組成物A1を塗布し、熱処理及び乾燥をして、厚さが4μmの樹脂層A1を形成した。
<透明電極層Bの形成>
樹脂層Aの表面に、ITOの焼結体ターゲットを備えたスパッタ装置を用いて、ITOからなる厚さ22nmのITO薄膜を形成した。
<ITO薄膜のパターン加工>
ITO薄膜にフォトマスクを密着させ、超高圧水銀ランプを有する露光機で200mJ/cm2の露光量で樹脂層A1及びITO薄膜を露光し、さらにフォトマスクを介すことなく、200mJ/cm2の露光量で樹脂層A1及びITO薄膜を全面露光した露光後、30℃の1質量%炭酸ナトリウム水溶液で30秒間スプレー現像し、樹脂層A1上にパターン加工された透明電極層B1を形成した。
<組成物Cの調製>
100mLクリーンボトルに、10.0gの化合物(C-1)、2.0gのIC-369及び5.0gのジエチエングリコールを入れ、自転-公転真空ミキサー“あわとり錬太郎”(登録商標)ARE-310((株)シンキー製)で混合して、17.0gの樹脂溶液C1(固形分70.1質量%)を得た。
得られた17.0gの樹脂溶液C1、68.0gの銀粒子を混ぜ合わせ、3本ローラーミル(EXAKT M-50;EXAKT社製)を用いて混練し、85.0gの組成物C1を得た。
<導電パターン形成部材の製造>
樹脂層A1及びパターン加工された透明電極層B1の表面に、組成物C1をスクリーン印刷機で乾燥膜C1の膜厚が5μmになるように塗布し、70℃で10分間乾燥後、所定のフォトマスクを介して超高圧水銀ランプを有する露光機で300mJ/cm2の露光量で露光し、0.2質量%炭酸ナトリウム水溶液を0.1MPaの圧力で30秒間スプレー現像した後、140℃で60分間キュアを行い、導電パターン形成部材1を製造した。
<残渣の評価>
図3に示す導電パターンC1を形成した導電パターン形成部材1について、未露光部分の全光線透過率Tを、NDH-7000SP(日本電色工業(株)製)を用いて、JIS K7361-1に準じて測定した。一方で、組成物Cを塗布していない部位の(樹脂層A単独の)全光線透過率T0を、同様に測定し、T0に対するTの低下率を算出して、以下の判断基準に基づき良/不良の別を判断した。結果を表2に示す。
低下率が10%以下 : 良
低下率が10%超 : 不良
<イオンマイグレーション耐性の評価>
図2に示す導電パターンC1を形成した導電パターン形成部材1を、85℃、85%RHの高温高湿槽に投入し、端子部からDC5Vの電圧を印加して、急激に抵抗値が3桁低下する短絡時間を確認した。計10個の導電パターン形成部材1で同評価を繰り返し、それらの平均値を、イオンマイグレーション耐性の値とした。結果を表2に示す。
透明電極層Bが銀繊維の場合は下記方法により形成した以外は、表1に示す条件の導電パターン形成部材を実施例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。
<透明電極層Bの形成>
銀繊維の水分散液(固形分0.2質量%)を樹脂層A2上に塗布し、100℃で5分間乾燥し、厚さ1.0μmからなる銀繊維薄膜を形成した。
<銀繊維薄膜のパターン加工>
銀繊維薄膜にフォトマスクを密着させ、超高圧水銀ランプを有する露光機で200mJ/cm2の露光量で樹脂層A2及び銀繊維薄膜を露光し、さらにフォトマスクを介すことなく、200mJ/cm2の露光量で樹脂層A2及び銀繊維薄膜を全面露光した露光後、30℃の1質量%炭酸ナトリウム水溶液で30秒間スプレー現像し、樹脂層A2上にパターン加工された透明電極層B2を形成した。
(実施例15)
実施例1と同様の方法で、導電パターン形成部材を製造した。
<OCA層Dの形成>
樹脂層A1及びパターン加工した透明電極層B1、導電パターンC1の表面にOCA(d-1)を80℃、圧着圧力0.5MPaの条件でラミネートして、図5に示す積層部材6、及び図6に示す積層部材7をそれぞれ製造した。
積層部材6及び7について、実施例1と同様の評価を行った。結果を表2に示す。
(実施例16~17)
表1に示す導電パターン形成部材を実施例15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に示す条件の導電パターン形成部材を実施例1もしくは実施例2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。
2 導電パターンC
3 層A
4 支持体
5 端子部
6 乾燥膜Cの露光エリア
7 乾燥膜Cの未露光部エリア
8 塗布膜Cの印刷エリア
9 OCA層D
Claims (15)
- 基材上に形成された、カルボキシル基を有する樹脂(a)からなる層A、及び、透明電極層Bの表面に、導電性粒子、及び、二重結合とカルボキシル基とを有する樹脂(c)を含有する組成物Cを塗布して、塗布膜Cを得る、塗布工程と、
前記塗布膜Cを乾燥して乾燥膜Cを得る、乾燥工程と、
前記乾燥膜Cを露光して露光膜Cを得る、露光工程と、
前記露光膜Cを現像してパターンCを得る、現像工程と、
前記パターンCをキュアして導電パターンCを得る、キュア工程と、を備え、
前記導電性粒子に占める粒径0.3~2.0μmの粒子の割合が、80%以上である、導電パターン形成部材の製造方法。 - 前記導電性粒子に占める粒径0.5~1.5μmの粒子の割合が、80%以上である、請求項1記載の導電パターン形成部材の製造方法。
- 前記組成物Cが、さらに光重合開始剤を含有する、請求項1又は2記載の導電パターン形成部材の製造方法。
- 前記二重結合とカルボキシル基を有する樹脂(c)が、酸価が50~250mgKOH/gのアクリル樹脂である、請求項1~3のいずれか一項記載の導電パターン形成部材の製造方法。
- 前記透明電極層Bが銀を含有し、かつ、前記組成物Cが前記導電性粒子として銀粒子を含む、請求項1~4のいずれか一項記載の導電パターン形成部材の製造方法。
- 前記透明電極層Bが含有する銀が、繊維状である、請求項5記載の導電パターン形成部材の製造方法。
- 前記組成物Cが、沸点200℃以上のアルコール系溶剤を含有する、請求項1~6のいずれか一項記載の導電パターン形成部材の製造方法。
- 前記乾燥工程の温度が、50~80℃である、請求項1~7のいずれか一項記載の導電パターン形成部材の製造方法。
- 前記現像工程の現像圧力が、0.02~0.2MPaである、請求項1~8のいずれか一項記載の導電パターン形成部材の製造方法。
- 前記組成物Cが、エポキシ樹脂を含有する、請求項1~9のいずれか一項記載の導電パターン形成部材の製造方法。
- 前記カルボキシル基を有する樹脂(a)からなる層Aの酸価SAと、前記導電パターンCの有機成分酸価SCとの差が、20~150mgKOH/gである、請求項1~10のいずれか一項記載の導電パターン形成部材の製造方法。
- 請求項1~11のいずれか一項記載の導電パターン形成部材の製造方法によって得られた導電パターン形成部材であって、前記導電パターンCが、ウレタン結合を有する化合物を含有する導電パターン形成部材。
- 請求項1~11のいずれか一項記載の導電パターン形成部材の製造方法によって得られた導電パターン形成部材または請求項12に記載の導電パターン形成部材であって、前記導電パターンCが、シクロヘキサン骨格を有する化合物を含有する導電パターン形成部材。
- 請求項1~11のいずれか一項記載の導電パターン形成部材の製造方法によって得られた導電パターン形成部材または請求項12もしくは13に記載の導電パターン形成部材であって、前記層Aと、前記透明電極層Bと、導電パターンC上に積層されたOptical Clear Adhesive層Dがイソボルニル骨格を含有する導電パターン形成部材。
- 請求項1~11のいずれか一項記載の導電パターン形成部材の製造方法によって得られた導電パターン形成部材または請求項12、13もしくは14に記載の導電パターン形成部材であって、前記層Dがベンゾトリアゾール系化合物を含有する導電パターン形成部材。
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JP6150021B2 (ja) | 2017-06-21 |
TW201706711A (zh) | 2017-02-16 |
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US10048583B2 (en) | 2018-08-14 |
CN107430336B (zh) | 2019-06-11 |
KR20170140166A (ko) | 2017-12-20 |
KR101898955B1 (ko) | 2018-09-14 |
TWI620983B (zh) | 2018-04-11 |
US20170363956A1 (en) | 2017-12-21 |
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