WO2016167228A1 - Film conducteur photosensible, procédé de formation d'un motif conducteur, substrat ayant un motif conducteur, et capteur de panneau tactile - Google Patents

Film conducteur photosensible, procédé de formation d'un motif conducteur, substrat ayant un motif conducteur, et capteur de panneau tactile Download PDF

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Publication number
WO2016167228A1
WO2016167228A1 PCT/JP2016/061728 JP2016061728W WO2016167228A1 WO 2016167228 A1 WO2016167228 A1 WO 2016167228A1 JP 2016061728 W JP2016061728 W JP 2016061728W WO 2016167228 A1 WO2016167228 A1 WO 2016167228A1
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photosensitive
conductive
conductive film
film
conductive pattern
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PCT/JP2016/061728
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English (en)
Japanese (ja)
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雅彦 海老原
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日立化成株式会社
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Priority to JP2017512533A priority Critical patent/JPWO2016167228A1/ja
Publication of WO2016167228A1 publication Critical patent/WO2016167228A1/fr

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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
    • G06F3/044—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means
    • G06F3/0446—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means using a grid-like structure of electrodes in at least two directions, e.g. using row and column electrodes
    • 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
    • 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
    • G03F7/029—Inorganic compounds; Onium compounds; Organic compounds having hetero atoms other than oxygen, nitrogen or sulfur
    • 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
    • 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
    • G06F3/044—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means

Definitions

  • the present invention relates to a photosensitive conductive film, a method for forming a conductive pattern, a substrate with a conductive pattern, and a touch panel sensor.
  • Liquid crystal display elements or touch panel sensors are used in large electronic devices such as personal computers and televisions, small electronic devices such as car navigation, mobile phones, and electronic dictionaries, and display devices such as OA devices and FA devices. These liquid crystal display elements and touch panel sensors require a transparent electrode material.
  • capacitive touch panels In a capacitive touch panel, when a fingertip (conductor) contacts the touch input surface, the fingertip and the conductive film are capacitively coupled to form a capacitor. The capacitive touch panel detects the coordinates by capturing the change in charge at the contact position of the fingertip.
  • the projected capacitive touch panel has good operability because it can detect multiple points of the fingertip and can give complicated instructions. Due to its good operability, a projected capacitive touch panel is increasingly used as an input device on a display surface in a device having a small display device such as a mobile phone and a portable music player.
  • a plurality of X electrodes and a plurality of Y electrodes perpendicular to the X electrodes form a two-layer structure in order to express two-dimensional coordinates based on the X and Y axes. is doing.
  • a transparent electrode material is used for these electrodes.
  • Patent Document 1 proposes a method for forming a conductive pattern using a photosensitive conductive film having a photosensitive layer containing conductive fibers. If this technique is used, a conductive pattern can be easily formed directly on various substrates by a photolithography process.
  • An object of the present invention is to provide a photosensitive conductive film capable of forming a conductive pattern containing conductive fibers with sufficient resolution, a method for forming the conductive pattern, a substrate with a conductive pattern having a conductive pattern with excellent resolution, and An object is to provide a touch panel.
  • the present inventor has found that the resolution can be improved by blending a photosensitive layer containing conductive fibers with an ultraviolet absorber, and the present invention has been completed.
  • the present invention comprises a support film and a photosensitive layer provided on the support film, the photosensitive layer comprising conductive fibers, a binder polymer, a photopolymerizable compound, a photopolymerization initiator, and an ultraviolet absorber.
  • a photosensitive conductive film is provided.
  • a conductive pattern containing conductive fibers can be formed with sufficient resolution. This is presumably because the photosensitive layer has the above composition containing an ultraviolet absorber, so that the scattered light generated by the conductive fibers is absorbed during patterning, and the influence of halation can be reduced.
  • the ultraviolet absorber may have a maximum absorption wavelength in a wavelength range of 250 nm to 400 nm. Such an ultraviolet absorber can effectively absorb the scattered light from the conductive fiber, and can further suppress a reduction in resolution to a higher degree.
  • the photosensitive conductive film may have a minimum visible light transmittance of 85% or more at 400 to 700 nm. When the minimum value of the visible light transmittance is in the above range, it is possible to provide a conductive pattern which is not colored and has excellent transparency.
  • the ultraviolet absorber may have a thermally polymerizable group or a photopolymerizable group. When such an ultraviolet absorber is used, the bleeding of the ultraviolet absorber from the photosensitive layer or a cured product thereof can be further suppressed.
  • the ultraviolet absorber may be a polymer type ultraviolet absorber. When such an ultraviolet absorber is used, the bleeding of the ultraviolet absorber from the photosensitive layer or a cured product thereof can be further suppressed.
  • the conductive fiber may be a silver fiber.
  • a photosensitive conductive film having high visible light transmittance in the wavelength region of 400 nm to 700 nm and high conductivity can be provided.
  • the present invention also includes a step of transferring the photosensitive layer of the photosensitive conductive film of the present invention onto a substrate, an exposure step of irradiating the photosensitive layer transferred onto the substrate with actinic rays in a pattern, and the above And a development step of forming a conductive pattern by removing an unexposed portion of the photosensitive layer.
  • a conductive pattern can be formed with sufficient resolution even in the case of a photosensitive layer containing conductive fibers. According to the method for forming the conductive pattern, the conductive pattern can be easily formed on the substrate.
  • the present invention also provides a substrate with a conductive pattern, which has a substrate and a conductive pattern formed on the substrate by the method for forming a conductive pattern of the present invention.
  • the substrate with a conductive pattern of the present invention has a conductive pattern formed by the above-described method for forming a conductive pattern, a conductive pattern with excellent resolution, that is, a thinner conductive pattern and a thinner space portion (photosensitive layer removal) Part).
  • the present invention also provides a touch panel sensor comprising the substrate with a conductive pattern of the present invention.
  • the touch panel sensor of the present invention includes the above-described substrate with a conductive pattern, the pattern appearance of the conductive pattern can be reduced, and the visibility can be improved (the pattern is difficult to see).
  • a photosensitive conductive film capable of forming a conductive pattern containing conductive fibers with sufficient resolution, a method for forming a conductive pattern, a substrate with a conductive pattern having a conductive pattern with excellent resolution, and A touch panel can be provided.
  • (meth) acrylate in the present specification means “acrylate” or “methacrylate”.
  • (meth) acrylic acid means “acrylic acid” or “methacrylic acid”
  • (meth) acryloyl group means “acryloyl group” or “methacryloyl group”.
  • a numerical range indicated by using “to” indicates a range including the numerical values described before and after “to” as the minimum value and the maximum value, respectively.
  • “A or B” only needs to include one of A and B, or may include both.
  • the exemplary materials may be used alone or in combination of two or more unless otherwise specified.
  • the photosensitive conductive film according to the present embodiment includes a support film and a photosensitive layer provided on the support film, and the photosensitive layer includes conductive fibers, a binder polymer, a photopolymerizable compound, and a photopolymerization initiator. , And an ultraviolet absorber.
  • One embodiment of the photosensitive conductive film is shown in FIG.
  • the photosensitive conductive film 10 includes a support film 1, a photosensitive layer 4, and a protective film 5, and the photosensitive layer 4 includes a conductive film 2 and a photosensitive resin layer 3.
  • the conductive film 2 contains conductive fibers.
  • the photosensitive conductive film is used to transfer the photosensitive layer onto the base material and form the photosensitive layer on the base material, it can also be said to be a transfer type photosensitive conductive film.
  • the photosensitive conductive film 10 is illustrated so that the boundary between the conductive film 2 and the photosensitive resin layer 3 provided on the conductive film 2 is clear.
  • the boundary with the conductive resin layer 3 is not necessarily clear.
  • Any conductive film may be used as long as conductivity is obtained in the surface direction of the photosensitive layer, and the conductive resin may be mixed with the photosensitive resin layer.
  • the composition constituting the photosensitive resin layer may be impregnated in the conductive film, or the composition constituting the photosensitive resin layer may be present on the surface of the conductive film.
  • the support film 1 includes a polymer film having heat resistance and solvent resistance.
  • a polymer film having heat resistance and solvent resistance.
  • examples of such a polymer film include a polyethylene terephthalate film, a polyethylene film, a polypropylene film, and a polycarbonate film.
  • a polyethylene terephthalate film is preferable from the viewpoint of transparency and heat resistance.
  • These polymer films may be surface-treated so as to be easily peeled off from the photosensitive layer 4, and are preferably materials that can be easily peeled off from the photosensitive layer 4.
  • the thickness of the support film 1 is preferably 5 to 300 ⁇ m, more preferably 10 to 200 ⁇ m, still more preferably 15 to 100 ⁇ m, and particularly preferably 30 to 70 ⁇ m.
  • a step of applying a photosensitive resin composition to form a conductive dispersion or a photosensitive resin layer 3 to form the conductive film 2, or a support film before developing the exposed photosensitive resin layer 3 In the step of peeling, from the viewpoint of preventing mechanical strength from being reduced and the support film from being broken, it is preferably 5 ⁇ m or more, more preferably 10 ⁇ m or more, further preferably 15 ⁇ m or more, and 30 ⁇ m. The above is particularly preferable.
  • the photosensitive resin layer is irradiated with actinic rays through the support film, it is preferably 300 ⁇ m or less, more preferably 200 ⁇ m or less, and 100 ⁇ m or less. More preferably, it is particularly preferably 70 ⁇ m or less.
  • the haze value of the support film 1 is preferably 0.01 to 5.0%, more preferably 0.01 to 3.0%, from the viewpoint of improving sensitivity and resolution. It is more preferably from 2.0% to 2.0%, particularly preferably from 0.01% to 1.0%.
  • the haze value can be measured according to JIS K 7375 (established in 2008). It can also be measured with a commercially available turbidimeter such as NDH-1001DP (trade name, manufactured by Nippon Denshoku Industries Co., Ltd.).
  • the conductive fiber examples include metal fibers such as gold, silver, copper, and platinum, or carbon fibers such as carbon nanotubes.
  • the conductive fiber is easy to prepare, is easy to control the shape of the conductive fiber, has high visible light transmittance in the wavelength range of 400 to 700 nm, and has high conductivity.
  • silver fiber is preferable, and silver nanowire is more preferable.
  • the nanowire is, for example, a small difference in size between two dimensions (X, Y) (specifically, the difference in size is 5 times or less), and both X and Y are 300 nm or less. This is a size, and indicates a shape in which the size of one remaining dimension (Z) is 10 times or more of X and Y.
  • FIG. 2 is a partially cutaway perspective view showing an embodiment of a photosensitive conductive film.
  • the conductive film 2 preferably has a network structure in which conductive fibers are in contact with each other like the photosensitive conductive film 12 shown in FIG.
  • the conductive film 2 having such a network structure may be formed on the surface of the photosensitive resin layer 3 on the support film 1 side, but on the surface of the photosensitive layer 4 exposed when the support film 1 is peeled off.
  • the conductive film 2 may be formed so that a part of the photosensitive resin layer 3 enters the conductive film 2, and the conductive film is formed on the surface layer of the photosensitive resin layer 3 on the support film 1 side. 2 may be included.
  • the conductive fibers including silver fibers or silver nanowires can be prepared by, for example, a method of reducing silver ions with a reducing agent such as NaBH 4 or a polyol method.
  • the fiber diameter of the conductive fiber is preferably 1 nm to 100 nm, more preferably 2 nm to 50 nm, and further preferably 3 nm to 30 nm.
  • the fiber length of the conductive fiber is preferably 1 ⁇ m to 100 ⁇ m, more preferably 2 ⁇ m to 50 ⁇ m, and even more preferably 3 ⁇ m to 10 ⁇ m.
  • the fiber diameter and fiber length can be measured with a scanning electron microscope.
  • an organic conductor may be used in combination with the conductive fiber.
  • the organic conductor can be used without particular limitation, but from the viewpoint of high transparency and conductivity, it is preferable to use an organic conductor such as a polymer of a thiophene derivative and an aniline derivative. Specifically, polyethylenedioxythiophene, polyhexylthiophene, polyaniline, polyvinylpyrrolidone, or the like can be used.
  • the thickness of the conductive film 2 varies depending on the use of the conductive pattern formed using the photosensitive conductive film of the present invention and the required conductivity, but is preferably 1 ⁇ m or less, and preferably 1 nm to 0.5 ⁇ m. More preferably, the thickness is 5 nm to 0.1 ⁇ m.
  • the thickness of the conductive film 2 is 1 ⁇ m or less, the light transmittance in the wavelength range of 400 to 700 nm is high, the pattern formation is excellent, and it is particularly suitable for the production of a transparent electrode.
  • the thickness of the conductive film 2 indicates a value measured by a scanning electron microscope.
  • the conductive film 2 is coated on the support film 1 with a conductive dispersion obtained by adding the above-described conductive fiber or organic conductor to water or an organic solvent, a dispersion stabilizer such as a surfactant, and the like, It can be formed by drying. After drying, the conductive film 2 formed on the support film 1 may be laminated as necessary.
  • Coating can be performed by a known method such as a roll coating method, a comma coating method, a gravure coating method, an air knife coating method, a die coating method, a bar coating method, or a spray coating method.
  • the drying can be performed at 30 to 150 ° C. for about 1 to 30 minutes with a hot air convection dryer or the like.
  • the conductive fiber and the organic conductor may coexist with a surfactant or a dispersion stabilizer.
  • the surface resistivity of the conductive film 2 and the photosensitive conductive film including the conductive film 2 can be adjusted by the amount of conductive fibers.
  • the photosensitive layer only needs to contain an ultraviolet absorber.
  • the conductive film is formed using a conductive dispersion containing the ultraviolet absorber, and the ultraviolet absorber is present in the conductive film.
  • an ultraviolet absorber may be present in the photosensitive resin layer.
  • an ultraviolet absorber can be contained.
  • the photosensitive resin layer 3 examples include those formed from a photosensitive resin composition containing (A) a binder polymer, (B) a photopolymerizable compound, and (C) a photopolymerization initiator.
  • the photosensitive resin composition may contain the (D) ultraviolet absorber.
  • (A) As binder polymer epoxy resin obtained by reaction of acrylic resin, styrene resin, epoxy resin, amide resin, amide epoxy resin, alkyd resin, phenol resin, ester resin, urethane resin, epoxy resin and (meth) acrylic acid Examples thereof include acid-modified epoxy acrylate resins obtained by reaction of acrylate resins and epoxy acrylate resins with acid anhydrides.
  • acrylic resin is derived from (meth) acrylic acid and a (meth) acrylic acid alkyl ester as a constituent unit. More preferably.
  • acrylic resin means a polymer mainly having a monomer unit derived from a polymerizable monomer having a (meth) acryloyl group.
  • acrylic resin one produced by radical polymerization of a polymerizable monomer having a (meth) acryloyl group can be used.
  • Examples of the polymerizable monomer having a (meth) acryloyl group include acrylamide such as diacetone acrylamide; (meth) acrylic acid alkyl ester, 2-hydroxyalkyl (meth) acrylate, (meth) acrylic acid tetrahydrofurfuryl ester, ( (Meth) acrylic acid dimethylaminoethyl ester, (meth) acrylic acid diethylaminoethyl ester, (meth) acrylic acid glycidyl ester, (meth) acrylic acid benzyl ester, 2,2,2-trifluoroethyl (meth) acrylate, 2, (Meth) acrylic acid esters such as 2,3,3-tetrafluoropropyl (meth) acrylate; (meth) acrylic acid, ⁇ -bromo (meth) acrylic acid, ⁇ -chloro (meth) acrylic acid, ⁇ -furyl ( (Meth) acrylic acid, ⁇ -styryl (meth)
  • the acrylic resin includes styrene derivatives; acrylonitrile; esters of vinyl alcohol such as vinyl-n-butyl ether; maleic acid; maleic anhydride; By copolymerizing monomeric monomers such as monomethyl maleate, monoethyl maleate and monoisopropyl maleate; fumaric acid; cinnamic acid; ⁇ -cyanocinnamic acid; itaconic acid; crotonic acid It may be manufactured.
  • (meth) acrylic acid alkyl ester (meth) acrylic acid methyl ester, (meth) acrylic acid ethyl ester, (meth) acrylic acid propyl ester, (meth) acrylic acid butyl ester, (meth) acrylic acid hexyl ester,
  • acrylic acid heptyl ester (meth) acrylic acid octyl ester, (meth) acrylic acid 2-ethylhexyl ester, (meth) acrylic acid nonyl ester, and the like.
  • the binder polymer preferably has a carboxyl group from the viewpoint of improving alkali developability.
  • Examples of the polymerizable monomer having a carboxyl group include (meth) acrylic acid as described above.
  • the ratio of the carboxyl group of the binder polymer is preferably 10 to 50% by mass, and preferably 12 to 40% by mass as the ratio of the polymerizable monomer having a carboxyl group to the total polymerizable monomer to be used. Is more preferable, 12 to 30% by mass is further preferable, and 12 to 25% by mass is particularly preferable. In terms of excellent alkali developability, the content is preferably 10% by mass or more, and in terms of excellent alkali resistance, it is preferably 50% by mass or less.
  • the binder polymer is preferably a binder polymer having a structural unit based on (meth) acrylic acid and a structural unit based on (meth) acrylic acid methyl ester or a structural unit based on (meth) acrylic acid ethyl ester. Binder polymers having a structural unit based on (meth) acrylic acid, a structural unit based on (meth) acrylic acid methyl ester, and a structural unit based on (meth) acrylic acid ethyl ester are more preferred.
  • the weight average molecular weight of the binder polymer is preferably 5000 to 300000, more preferably 20000 to 150,000, and more preferably 30000 to 100,000 from the viewpoint of balancing the mechanical strength and alkali developability. Further preferred. In terms of excellent developer resistance, the weight average molecular weight is preferably 5000 or more. Further, from the viewpoint of development time, it is preferably 300000 or less. In this specification, the weight average molecular weight is a value measured by a gel permeation chromatography method (GPC) and converted by a calibration curve created using standard polystyrene.
  • GPC gel permeation chromatography
  • the acid value of the binder polymer is preferably 75 to 200 mgKOH / g, more preferably 75 to 150 mgKOH / g, and more preferably 75 to 120 mgKOH / g from the viewpoint of excellent pattern formability. More preferred is 78 to 120 mg KOH / g.
  • the acid value of a binder polymer can be measured as follows. First, 1 g of the binder polymer that is the object of acid value measurement is precisely weighed. 30 g of acetone is added to the precisely weighed binder polymer and dissolved uniformly. Next, an appropriate amount of phenolphthalein as an indicator is added to the solution, and titration is performed using a 0.1N aqueous KOH solution. And an acid value is computed by following Formula.
  • Acid value 0.1 ⁇ Vf ⁇ 56.1 / (Wp ⁇ I / 100)
  • Vf represents the titration amount (mL) of the KOH aqueous solution
  • Wp represents the weight (g) of the solution containing the measured binder polymer
  • I represents the ratio of the nonvolatile content in the solution containing the measured binder polymer ( Mass%).
  • the photopolymerizable compound (B) The photopolymerizable compound will be described.
  • the photopolymerizable compound preferably has an ethylenically unsaturated bond.
  • Examples of the photopolymerizable compound having an ethylenically unsaturated bond include 2,2-bis (4-((meth) acryloxypolyethoxy) phenyl) propane, 2,2-bis (4-((meth) acryloxypoly).
  • Bisphenol A di (meth) acrylate compounds such as propoxy) phenyl) propane, 2,2-bis (4-((meth) acryloxypolyethoxypolypropoxy) phenyl) propane; polyethylene glycol di (meth) acrylate, polypropylene glycol di Polyalkylene glycol di (meth) acrylates such as (meth) acrylate and polyethylene polypropylene glycol di (meth) acrylate; trimethylolpropane di (meth) acrylate, trimethylolpropane tri (meth) acrylate, trimethylolpropane etoxy Trimethylolpropane (meth) acrylates such as tri (meth) acrylate and trimethylolpropane triethoxytri (meth) acrylate; tetramethylolmethane (meta) such as tetramethylolmethane tri (meth) acrylate and tetramethylolmethanetetra (meth
  • trimethylolpropane (meth) acrylate or dipentaerythritol (meth) acrylate is preferably used, and trimethylolpropane (meth) acrylate is more preferably used.
  • the content ratio of the photopolymerizable compound is preferably 30 to 80% by mass, and more preferably 40 to 70% by mass with respect to 100% by mass of the total of the binder polymer and the photopolymerizable compound. . It is preferably 30% by mass or more in terms of excellent coating properties of the photocurable and photosensitive resin composition, and 80% by mass or less in terms of excellent storage stability when wound as a film. Is preferred.
  • the photopolymerization initiator will be described.
  • the photopolymerization initiator is not particularly limited as long as the photopolymerization initiator is selected so that the light wavelength of the exposure machine to be used matches the wavelength necessary for function expression.
  • Examples of the photopolymerization initiator include benzophenone, N, N, N ′, N′-tetramethyl-4,4′-diaminobenzophenone (Michler ketone), N, N, N ′, N′-tetraethyl-4,4 '-Diaminobenzophenone, 4-methoxy-4'-dimethylaminobenzophenone, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) -butanone-1,2-methyl-1- [4- (methylthio) Aromatic ketones such as phenyl] -2-morpholino-propanone-1; benzoin ether compounds such as benzoin methyl ether, benzoin ethyl
  • an oxime ester compound or a phosphine oxide compound is preferable because of transparency and pattern forming ability when the photosensitive layer is a thin film (for example, 10 ⁇ m or less).
  • Examples of the oxime ester compound include compounds represented by the following general formula (C-1) and general formula (C-2). From the viewpoint of fast curability and transparency, a compound represented by the following general formula (C-1) is preferred.
  • R 1 represents an alkyl group having 1 to 12 carbon atoms or a cycloalkyl group having 3 to 20 carbon atoms.
  • R 1 is preferably an alkyl group having 3 to 9 carbon atoms.
  • the aromatic ring in the general formula (C-1) may have a substituent. Examples of the substituent include a hydrogen atom or an alkyl group having 1 to 12 carbon atoms.
  • R 2 represents a hydrogen atom or an alkyl group having 1 to 12 carbon atoms
  • R 3 represents an alkyl group having 1 to 12 carbon atoms or a cycloalkyl group having 3 to 20 carbon atoms
  • R 4 represents an alkyl group having 1 to 12 carbon atoms
  • R 5 represents an alkyl group or aryl group having 1 to 20 carbon atoms
  • p1 represents an integer of 0 to 3. When p1 is 2 or more, the plurality of R 4 may be the same or different.
  • the carbazole structure may have a substituent as long as the effects of the present invention are not impaired. Examples of the substituent include a hydrogen atom or an alkyl group having 1 to 12 carbon atoms.
  • R 2 or R 4 is preferably an alkyl group having 1 to 12 carbon atoms, more preferably an alkyl group having 1 to 8 carbon atoms, and 1 to 4 carbon atoms. More preferably, it is an alkyl group.
  • R 3 is preferably an alkyl group having 1 to 8 carbon atoms, or a cycloalkyl group having 4 to 15 carbon atoms, and an alkyl group having 1 to 4 carbon atoms or a carbon number A 4 to 10 cycloalkyl group is more preferable, and a methyl group and an ethyl group are particularly preferable.
  • R 5 is preferably an alkyl group having 1 to 12 carbon atoms or an aryl group having 6 to 16 carbon atoms, and an alkyl group having 1 to 8 carbon atoms or 6 to 14 carbon atoms. Are more preferable, and an alkyl group having 1 to 4 carbon atoms or an aryl group having 6 to 12 carbon atoms is more preferable.
  • Examples of the compound represented by the general formula (C-1) include 1,2-octanedione-1- [4- (phenylthio) phenyl] -2- (O-benzoyloxime). IRGACURE OXE It is commercially available as 01 (BASF Corporation, trade name).
  • Examples of the compound represented by the general formula (C-2) include ethanone, 1- [9-ethyl-6- (2-methylbenzoyl) -9H-carbazol-3-yl]-, 1- (O-acetyl). Oxime) and the like, and is commercially available as IRGACURE OXE 02 (trade name, manufactured by BASF Corporation).
  • Examples of the phosphine oxide compound include compounds represented by the following general formula (C-3) and general formula (C-4). From the viewpoint of fast curability and transparency, a compound represented by the following general formula (C-3) is preferred.
  • R 6 , R 7 and R 8 each independently represents an alkyl group or aryl group having 1 to 20 carbon atoms.
  • R 9 , R 10 and R 11 each independently represents an alkyl group or aryl group having 1 to 20 carbon atoms.
  • R 6 , R 7 or R 8 in the general formula (C-3) is an alkyl group having 1 to 20 carbon atoms
  • R 9 , R 10 or R 11 in the general formula (C-4) are In the case of an alkyl group having 1 to 20 carbon atoms, the alkyl group may be linear, branched, or cyclic, and the alkyl group preferably has 5 to 10 carbon atoms. .
  • R 6 , R 7 or R 8 in the general formula (C-3) is an aryl group
  • R 9 , R 10 or R 11 in the general formula (C-4) is an aryl group
  • the aryl The group may have a substituent.
  • the substituent include an alkyl group having 1 to 6 carbon atoms and an alkoxy group having 1 to 4 carbon atoms.
  • R 6 , R 7 , and R 8 are preferably aryl groups.
  • R 9 , R 10 and R 11 are preferably aryl groups.
  • 2,4,6-trimethyl is used because of the transparency of the formed conductive pattern and the pattern forming ability when the film thickness is reduced (for example, 10 ⁇ m or less).
  • Benzoyl-diphenyl-phosphine oxide is preferred.
  • 2,4,6-Trimethylbenzoyl-diphenyl-phosphine oxide is commercially available, for example, as LUCIRIN TPO (trade name, manufactured by BASF Corporation).
  • bis (2, 4, 6) can be obtained from the transparency of the conductive pattern to be formed and the pattern forming ability when the film thickness is reduced (for example, 10 ⁇ m or less).
  • -Trimethylbenzoyl) -phenyl-phosphine oxide is preferred.
  • Bis (2,4,6-trimethylbenzoyl) -phenyl-phosphine oxide is commercially available, for example, as Irgacure 819 (trade name, manufactured by BASF Corporation).
  • 2,2-dimethoxy-1,2-diphenylethane-1-one may be used as a compound having good transparency and pattern forming ability when the photosensitive layer is thinned. Is preferred. 2,2-dimethoxy-1,2-diphenylethane-1-one is commercially available, for example, as Irgacure 651 (trade name, manufactured by BASF Corporation).
  • Photopolymerization initiators are 1,2-octanedione-1- [4- (phenylthio) phenyl] -2- (O-benzoyloxime), ethanone, 1- [9-ethyl-6- (2- Methylbenzoyl) -9H-carbazol-3-yl]-, 1- (O-acetyloxime), 2,4,6-trimethylbenzoyl-diphenyl-phosphine oxide, bis (2,4,6-trimethylbenzoyl) -phenyl It is particularly preferable to use either -phosphine oxide or 2,2-dimethoxy-1,2-diphenylethane-1-one.
  • the content ratio of the photopolymerization initiator is preferably 0.1 to 20 parts by mass, more preferably 1 to 10 parts by mass with respect to 100 parts by mass in total of the binder polymer and the photopolymerizable compound. More preferably, it is 1 to 5 parts by mass. In terms of excellent photosensitivity, it is preferably 0.1 parts by mass or more, and in terms of excellent photocurability, it is preferably 20 parts by mass or less.
  • the ultraviolet absorber will be described.
  • the ultraviolet absorber is excellent in the ability to absorb ultraviolet light having a wavelength of 400 nm or less from the viewpoint of scattered light absorption by the conductive fiber, and has little absorption of visible light having a wavelength of 400 nm or more from the viewpoint of improving transparency. Those are preferred. Specifically, a material having a maximum absorption wavelength in a wavelength range of 250 nm to 400 nm corresponds to this.
  • Examples of the ultraviolet absorber include oxybenzophenone compounds, triazole compounds, benzotriazole compounds, salicylic acid ester compounds, benzophenone compounds, diphenyl acrylate compounds, cyanoacrylate compounds, diphenyl cyanoacrylate compounds, nickel complex salts, and the like. Among these, a diphenyl cyanoacrylate compound, a cyanoacrylate compound, or a diphenyl acrylate compound is preferable.
  • the ultraviolet absorber is preferably a compound having a reactive group, and more preferably a compound having a thermally polymerizable group or a photopolymerizable group. Increasing the content of the ultraviolet absorber can be expected to improve the effect of the present invention. However, when the content of the ultraviolet absorber is increased, the ultraviolet absorber oozes from the cured resin after patterning. (Bleed out). Bleed-out of the ultraviolet absorber is not preferable because it may cause a decrease in transparency of the cured resin and deterioration of optical properties such as turbidity.
  • curing material may adsorb
  • the ultraviolet absorber has a reactive group, the ultraviolet absorber is fixed to the cured resin during patterning (for example, it is firmly connected and incorporated into the network of the cured resin by a covalent bond). Therefore, the ultraviolet absorber bleeds out (bleed out) or the movement of the ultraviolet absorber in the cured resin is suppressed. Therefore, even if the content of the ultraviolet absorber is increased, an increase in the resistance value due to the adsorption of the ultraviolet absorber to the conductive fiber surface can be suppressed.
  • thermally polymerizable group examples include an epoxy group, a glycidyl group, an isocyanate group, an acetylene group, a maleimide group, and an oxetanyl group.
  • photopolymerizable group examples include a (meth) acryloyl group, an allyl group, and a maleimide group.
  • the thermopolymerizable group and the photopolymerizable group are not limited to the above examples.
  • any ultraviolet absorber having a reactive group that can be polymerized by an active radical, an acid, or a base generated by heat or light can be used without particular limitation. Bleed out or adsorption to the surface of conductive fibers can be suppressed.
  • the compounds having a thermally polymerizable group or a photopolymerizable group it has a (meth) acryloyl group which is a photopolymerizable group from the viewpoint of availability and stability in the photosensitive conductive film before curing.
  • Compounds are particularly preferred.
  • Examples of such an ultraviolet absorber include 2- [2-hydroxy-5- [2- (methacryloyloxy) ethyl] phenyl] -2H-benzotriazole, which is a benzotriazole compound having a (meth) acryloyl group. .
  • 2- [2-hydroxy-5- [2- (methacryloyloxy) ethyl] phenyl] -2H-benzotriazole is, for example, RUVA-93 (trade name, manufactured by Otsuka Chemical Co., Ltd.) or DAINSORB T-31 (Yamato (Trade name, manufactured by Kasei Co., Ltd.).
  • the ultraviolet absorber is preferably a polymer type ultraviolet absorber.
  • the polymer type ultraviolet absorber is an ultraviolet absorber obtained by polymerizing the compound having the above-mentioned heat-reactive group or photopolymerizable group.
  • a polymer type ultraviolet absorber is a material having one or more ultraviolet absorption sites in a molecule and a large molecular weight. In the present specification, an ultraviolet absorber having a weight average molecular weight of 3000 or more is referred to as a polymer-type ultraviolet absorber.
  • the polymer type ultraviolet absorber is one in which bleeding out is suppressed as compared with a low molecular weight ultraviolet absorber.
  • the polymer-type ultraviolet absorber is hardly suppressed from being adsorbed on the surface of the conductive fiber.
  • a polymer type ultraviolet absorber photopolymerizability from the point of availability of a compound having a polymerizable reactive group as a raw material, easy adjustment of molecular weight, and wide selection of copolymerization components of the polymer A polymer polymerized using a compound having a (meth) acryloyl group as a raw material is preferred.
  • polymer-type ultraviolet absorbers examples include solvent-based RSA series (for example, RSA-0124, RSA-0151, and RSA-0191H; all manufactured by Shannan Synthetic Chemical Co., Ltd.), solvent-based PUVA series (for example, PUVA-30M- 50BA, PUVA-30M-30T, and PUVA-50M-50K; all manufactured by Daiwa Kasei Co., Ltd.), solvent-based RSU series (for example, RSU-0017 and SG-864; all manufactured by Daiwa Kasei Co., Ltd.) Water-based RWU series (for example, MW-022, RWU-0001, and RWU-0109; all manufactured by Daiwa Kasei Co., Ltd.) are commercially available.
  • solvent-based RSA series for example, RSA-0124, RSA-0151, and RSA-0191H; all manufactured by Shannan Synthetic Chemical Co., Ltd.
  • solvent-based PUVA series for example, PUVA-30M- 50BA,
  • water-based New Coat UVA series for example, New Coat UVA-101, New Coat UVA-102, New Coat UVA-103, and New Coat UVA-104
  • Solvent-based Vana Resin UVA series for example, Vana Resin UVA-5080, hydroxyl group Introducing vanaresin UVA-5080 (OHV20), vanaresin UVA-55T, high hydroxyl value type vanaresin UVA-55MHB, vanaresin UVA-7075, hydroxylintroducing vanaresin UVA-7075 (OHV20), vanaresin UVA-73T), etc.
  • Solvent-based UVA series for example, UVA-935LH and UVA-1935LH
  • aqueous-based UVA series for example, UVA-700 and UVA-1700 are commercially available from BASF Corporation.
  • the weight average molecular weight of the polymer type ultraviolet absorber is preferably 300,000 or less, more preferably 150,000 or less, and more preferably 100,000 or less from the viewpoint of solubility in a solvent and compatibility with a photosensitive resin composition. More preferably it is. Further, from the viewpoint of preventing bleeding out from the photosensitive conductive film and its cured film, it is preferably 3000 or more, more preferably 5000 or more, and further preferably 10,000 or more. From the viewpoint of balancing the solubility in a solvent, the compatibility with the photosensitive resin composition, and the bleed-out prevention property, it is preferably 3000 to 300000, more preferably 5000 to 150,000, and more preferably 10,000 to 100,000. More preferably.
  • the weight average molecular weight is a value measured by a gel permeation chromatography method (GPC) and converted by a calibration curve prepared using standard polystyrene.
  • the content ratio of the (D) ultraviolet absorber is preferably 0.1 to 30 parts by mass, and preferably 1 to 20 parts by mass with respect to 100 parts by mass of the total amount of the components (A) and (B). More preferred is 2 to 10 parts by mass.
  • the content of the ultraviolet absorber is preferably 0.1 parts by mass or more in terms of effectively suppressing light scattering by the conductive fiber and being excellent in resolution.
  • suction to the surface of a conductive fiber, or absorption on the surface of a photosensitive layer in the case of actinic ray irradiation Is preferably 30 parts by mass or less from the viewpoint of suppressing an increase in the amount of photocuring and insufficient internal photocuring.
  • a method for incorporating the ultraviolet absorber into the photosensitive layer a method of internally adding in advance into the photosensitive resin composition is common, but the present invention is not limited to the internal addition.
  • Other methods for incorporating an ultraviolet absorber in the photosensitive layer include, for example, a method of internally adding an ultraviolet absorber in a conductive fiber dispersion, and a film containing conductive fibers formed on a support film that absorbs ultraviolet rays.
  • internal addition to the photosensitive resin composition in advance The method is most preferred.
  • an adhesion imparting agent such as a silane coupling agent, a leveling agent, a plasticizer, a filler, an antifoaming agent, a flame retardant, a stabilizer, and an antioxidant.
  • a perfume, a thermal crosslinking agent, a polymerization inhibitor and the like can be contained in an amount of about 0.01 to 20 parts by mass with respect to 100 parts by mass of the total amount of the component (A) and the component (B).
  • the photosensitive resin layer 3 is a photosensitive resin composition dissolved in a solvent such as methanol, ethanol, acetone, methyl ethyl ketone, methyl cellosolve, ethyl cellosolve, toluene, N, N-dimethylformamide, propylene glycol monomethyl ether, or a mixed solvent thereof.
  • a solvent such as methanol, ethanol, acetone, methyl ethyl ketone, methyl cellosolve, ethyl cellosolve, toluene, N, N-dimethylformamide, propylene glycol monomethyl ether, or a mixed solvent thereof.
  • This solution can be formed by coating and drying on the support film 1 on which the conductive film 2 is formed.
  • the amount of the remaining organic solvent in the photosensitive resin layer after drying is preferably 2% by mass or less in order to prevent the organic solvent from diffusing in the subsequent step.
  • the photosensitive resin layer 3 can be applied by a known method such as a roll coating method, a comma coating method, a gravure coating method, an air knife coating method, a die coating method, a bar coating method, or a spray coating method. After coating, drying to remove the organic solvent and the like can be performed at 70 to 150 ° C. for about 5 to 30 minutes with a hot air convection dryer or the like.
  • the thickness of the photosensitive resin layer 3 varies depending on the use, but the thickness after drying is preferably 1 to 50 ⁇ m, more preferably 1 to 15 ⁇ m, and further preferably 1 to 10 ⁇ m. If the thickness is less than 1 ⁇ m, coating tends to be difficult, and if it exceeds 50 ⁇ m, the sensitivity due to the decrease in light transmission is insufficient, and the photocuring property of the photosensitive resin layer to be transferred tends to decrease.
  • the thickness of the layer (cured film) after curing the photosensitive resin layer 3 is also preferably within these ranges.
  • the laminate of the conductive film 2 and the photosensitive resin layer 3 is visible in a wavelength range of 400 nm to 700 nm when the total film thickness of both layers is 1 to 10 ⁇ m.
  • the minimum value of light transmittance is preferably 85% or more, and more preferably 90% or more.
  • the surface resistivity of the conductive film or the conductive pattern is preferably 1000 ⁇ / ⁇ or less, more preferably 500 ⁇ / ⁇ or less, from the viewpoint of effective utilization as a transparent electrode. Preferably, it is 300 ⁇ / ⁇ or less.
  • the surface resistivity can be adjusted by, for example, the concentration of the conductive fiber or the dispersion of the organic conductor or the coating amount.
  • the protective film 5 may be laminated so as to be in contact with the surface of the photosensitive resin layer 3 opposite to the support film 1 side.
  • a polymer film having heat resistance and solvent resistance such as a polyethylene terephthalate film, a polypropylene film, and a polyethylene film can be used. Further, as the protective film 5, a polymer film similar to the above-described support film may be used.
  • the adhesive force between the protective film 5 and the photosensitive layer 4 is such that when the protective film is peeled off and laminated on the substrate from the photosensitive resin layer 3 side, the photosensitive layer is formed in order to make the protective film easy to peel off from the photosensitive layer. It is preferable that it is smaller than the adhesive force between 4 and the support film 1.
  • the adhesive force between the protective film 5 and the photosensitive layer 4 is such that when the support film 1 is peeled off and laminated to the base material from the conductive film 2 side, It is preferable that it is larger than the adhesive force between the layer 4 and the support film 1.
  • the number of fish eyes with a diameter of 80 micrometers or more contained in a protective film is 5 pieces / m ⁇ 2 > or less.
  • “Fisheye” means that materials are melted, kneaded, extruded, biaxially stretched, casting materials, etc., and foreign materials, undissolved materials, oxidized degradation products, etc. are taken into the film. It is a thing.
  • the thickness of the protective film 5 is preferably 1 to 100 ⁇ m, more preferably 5 to 50 ⁇ m, still more preferably 5 to 30 ⁇ m, and particularly preferably 15 to 30 ⁇ m.
  • the thickness of the protective film is less than 1 ⁇ m, the protective film tends to be broken during lamination, and when it exceeds 100 ⁇ m, the winding property of the photosensitive conductive film tends to be lowered.
  • the method for forming a conductive pattern of the present invention comprises a step of transferring the photosensitive layer of the photosensitive conductive film of the present invention onto a substrate (also referred to as a laminating step), and a pattern active on the photosensitive layer transferred onto the substrate.
  • FIG. 3 is a schematic cross-sectional view for explaining one embodiment of a conductive pattern forming method using a photosensitive conductive film.
  • a method for forming a conductive pattern according to the present embodiment includes a laminating process in which the above-described photosensitive conductive film 10 is laminated so that the support film 1 is peeled off and the conductive layer 2 is in close contact with the base material 20 (FIG. 3A And a patterning step of forming a conductive pattern by exposing and developing the photosensitive layer 4 on the substrate (FIGS. 3B and 3C).
  • the patterning step includes an exposure step (FIG.
  • FIG. 4 is a schematic cross-sectional view for explaining another embodiment of a conductive pattern forming method using a photosensitive conductive film.
  • the conductive pattern forming method according to the present embodiment is different from the conductive pattern forming method described above in that the photosensitive resin layer 3 is laminated so as to be in close contact with the substrate 20 when the photosensitive layer is laminated. That is, a photosensitive conductive film 10 having a support film 1, a conductive film 2, and a photosensitive resin layer 3 is prepared, and the photosensitive resin layer 3 of the photosensitive conductive film 10 is in close contact with the base material 20. A photosensitive layer is laminated on 20 (FIG. 4A).
  • the photosensitive resin layer 3 is irradiated with an actinic ray L in a pattern via the mask pattern 6 (FIG. 4B), the support film 1 is peeled off, and an uncured portion (unexposed portion) is developed by development. ) Is removed to form a conductive pattern 2a (FIG. 4C).
  • the conductive pattern forming method includes the steps of laminating the photosensitive conductive film of the present invention so that the photosensitive resin layer is in close contact with the substrate, and the photosensitive resin layer on the substrate with the support film attached. An exposure step of irradiating the predetermined portion with actinic rays, a step of peeling off the support film, and a development step of forming a conductive pattern by developing the exposed photosensitive resin layer. By passing through these processes, the base material 41 with a conductive pattern provided with the conductive pattern patterned on the base material is obtained. The conductive pattern thus obtained has the thickness of the resin cured pattern 3b in addition to the thickness of the conductive pattern 2a.
  • FIG. 5 is a schematic cross-sectional view for explaining another embodiment of a method for forming a conductive pattern using a photosensitive conductive film.
  • the first exposure step (FIG. 5B) for irradiating a predetermined portion of the photosensitive layer 4 having the support film 1 with an actinic ray
  • the first exposure step is performed in the presence of oxygen after the support film 1 is peeled off.
  • a second exposure step (FIG. 5C) for irradiating a part or all of the exposed portion and the unexposed portion with actinic rays.
  • the second exposure step is preferably performed in the presence of oxygen, for example, in air. Moreover, the conditions which increased oxygen concentration may be sufficient.
  • the surface portion of the photosensitive resin layer 3 exposed in the second exposure step that has not been sufficiently cured is removed. Specifically, the surface portion of the photosensitive resin layer 3 that is not sufficiently cured, that is, the surface layer including the conductive film 2 is removed by the wet phenomenon. Thereby, the resin cured layer which does not have a conductive film with a conductive pattern is provided on the base material 20, the base material 42 with a conductive pattern is obtained, and it is conductive compared with the case where only a conductive pattern is provided on the base material. The level difference Ha of the pattern can be reduced.
  • the conductive pattern forming method includes a step of laminating the photosensitive conductive film of the present invention so that the photosensitive resin composition is in close contact with the substrate, a photosensitive resin layer provided on the substrate, A first exposure step of irradiating a photosensitive layer including a conductive film provided on a surface of the photosensitive resin layer opposite to the substrate with an actinic ray in a pattern; and in the presence of oxygen, the photosensitive layer A second exposure step of irradiating a part or all of the unexposed portion in at least the first exposure step with actinic rays, and developing the photosensitive layer after the second exposure step, thereby forming a conductive pattern. A developing step to be formed.
  • the conductive pattern 2a formed on the cured resin layer 3a can have a small step Ha.
  • the base material examples include glass substrates and plastic substrates such as polycarbonate.
  • the substrate preferably has a minimum light transmittance of 85% or more in a wavelength region of 400 to 700 nm.
  • the laminating step is performed by, for example, removing the protective conductive film or the supporting film from the photosensitive conductive film, if present, and then pressing the photosensitive resin layer or conductive film side to the substrate while heating. This operation is preferably performed under reduced pressure from the viewpoint of adhesion and followability.
  • the photosensitive layer or the substrate is preferably heated to 70 to 130 ° C., and the pressure bonding pressure is about 0.1 to 1.0 MPa (about 1 to 10 kgf / cm 2 ). Although preferred, these conditions are not particularly limited.
  • the photosensitive layer is heated to 70 to 130 ° C. as described above, it is not necessary to pre-heat the base material in advance, but the base material can be pre-heated in order to further improve the lamination property. .
  • a known light source is used as the active light source.
  • Exposure at the exposure step may vary depending on the composition of the device and the photosensitive resin composition used, it is preferably 5mJ / cm 2 ⁇ 1000mJ / cm 2, is 10mJ / cm 2 ⁇ 200mJ / cm 2 More preferred. In terms of excellent photocurability, it is preferably 10 mJ / cm 2 or more, and in terms of resolution, it is preferably 1000 mJ / cm 2 or less.
  • the exposure process may be performed in two steps, and the first step may be performed at the exposure amount described above, and then the second step may be performed at 100 to 10,000 mJ / cm 2 .
  • the wet development is performed by a known method such as spraying, rocking dipping, brushing, or scrubbing using a developer corresponding to the photosensitive resin to be used, such as an alkaline aqueous solution, an aqueous developer, an organic solvent developer, or the like.
  • a safe and stable aqueous solution such as an alkaline aqueous solution
  • alkali hydroxides such as lithium, sodium or potassium hydroxide
  • alkali carbonates such as lithium, sodium, potassium or ammonium carbonate or bicarbonate
  • potassium phosphate sodium phosphate and the like
  • alkali metal pyrophosphates such as sodium pyrophosphate and potassium pyrophosphate.
  • the alkaline aqueous solution used for development a sodium carbonate aqueous solution, a potassium carbonate aqueous solution, a sodium hydroxide aqueous solution, a sodium tetraborate aqueous solution and the like are preferable.
  • the concentration of the alkaline aqueous solution is usually 0.1 to 5% by mass.
  • the pH of the alkaline aqueous solution is preferably in the range of 9 to 11, and the temperature is adjusted according to the developability of the photosensitive resin layer.
  • a surfactant, an antifoaming agent, a small amount of an organic solvent for accelerating development, and the like may be mixed.
  • aqueous developer composed of water or an aqueous alkali solution and one or more organic solvents
  • a base contained in the alkaline aqueous solution in addition to the above-mentioned bases, borax, sodium metasilicate, tetramethylammonium hydroxide, ethanolamine, ethylenediamine, diethylenetriamine, 2-amino-2-hydroxymethyl-1,3 -Propanediol, 1,3-diamino-2-propanol, morpholine and the like may be used.
  • organic solvent examples include acetone, ethyl acetate, alkoxyethanol having an alkoxy group having 1 to 4 carbon atoms, ethyl alcohol, isopropyl alcohol, butyl alcohol, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, and the like.
  • the aqueous developer preferably has an organic solvent concentration of 2 to 90% by mass, and the temperature can be adjusted according to the developability. Furthermore, the pH of the aqueous developer is preferably as low as possible within a range where the resist can be sufficiently developed, preferably pH 8-12, and more preferably pH 9-10. In addition, a small amount of a surfactant, an antifoaming agent, or the like can be added to the aqueous developer.
  • organic solvent developer examples include 1,1,1-trichloroethane, N-methylpyrrolidone, N, N-dimethylformamide, cyclohexanone, methyl isobutyl ketone, and ⁇ -butyrolactone. These organic solvents are preferably added with water in the range of 1 to 20% by mass in order to prevent ignition.
  • Examples of the developing method include a dip method, a paddle method, a high-pressure spray method, brushing, and slapping. Among these, it is preferable to use a high-pressure spray system from the viewpoint of improving resolution.
  • the conductive pattern may be further cured by performing heating at about 60 to 250 ° C. or exposure at about 0.2 to 10 J / cm 2 as necessary after development. .
  • the method for forming a conductive pattern of the present invention it is possible to easily form a transparent conductive pattern on a substrate such as glass or plastic without forming an etching resist like an inorganic film such as ITO. is there.
  • the surface resistivity of the conductive film or the conductive pattern may be 1000 ⁇ / ⁇ or less from the viewpoint that it can be effectively used as a transparent electrode. Preferably, it is 500 ⁇ / ⁇ or less, more preferably 300 ⁇ / ⁇ or less.
  • the surface resistivity can be adjusted by, for example, the concentration of the conductive fiber or the dispersion of the organic conductor or the coating amount.
  • the minimum value of visible light transmittance in the wavelength region of 400 nm to 700 nm is preferably 80% or more, more preferably 85% or more, and 90% or more. More preferably.
  • the light transmittance can be adjusted by the concentration of the conductive fiber or the dispersion of the organic conductor and the coating amount.
  • the transmittance can also be adjusted by the shape (fiber diameter and fiber length) of the conductive fiber. The thinner the fiber diameter, the higher the transmittance.
  • the method for forming a conductive pattern and the substrate with a conductive pattern of the present invention can be preferably used, for example, as a transparent electrode of a capacitive touch panel and a capacitive touch panel sensor, respectively.
  • FIG. 6 is a schematic top view showing an example of a capacitive touch panel sensor.
  • FIG. 6 shows an example of a capacitive touch panel sensor that includes a transparent substrate 101, a transparent electrode (X position coordinate) 103, and a transparent electrode (Y position coordinate) 104 in the touch screen 102.
  • the transparent electrode 103 and the transparent electrode 104 may exist on the same plane, may be laminated on the transparent substrate 101, and may be disposed so as to sandwich the transparent substrate 101 therebetween.
  • the transparent electrodes 103 and 104 have lead-out wires (not shown) for connection to a control circuit of a driver element circuit that controls an electric signal.
  • the touch panel sensor In the touch panel sensor according to the present embodiment, at least one of the transparent electrodes is formed using the photosensitive conductive film of the present invention.
  • the other transparent electrode may be formed in advance on a transparent substrate by a known method using a transparent conductive material.
  • Carbon nanotubes Hipco single-walled carbon nanotube high-purity product, manufactured by Unidym
  • Dodecyl-pentaethylene glycol manufactured by Wako Pure Chemical Industries, Ltd.
  • Octamethylcyclotetrasiloxane manufactured by Toray Dow Corning Co., Ltd., trade name “SH-30”
  • leveling agent Methyl ethyl ketone
  • solution 2 a solution in which 5 g of AgNO 3 was dissolved in 300 mL of ethylene glycol
  • 5 g of solution 3 polyvinylpyrrolidone (manufactured by Wako Pure Chemical Industries, Ltd., weight average molecular weight: 58000)) were added to 150 mL of ethylene glycol.
  • the dissolved solution was dropped from each dropping funnel over 1 minute, and the reaction solution was stirred at 160 ° C. for 60 minutes.
  • the reaction solution was allowed to stand at 30 ° C. or lower and then diluted 10 times with acetone.
  • the diluted solution of the reaction solution was centrifuged at 2000 rpm for 20 minutes using a centrifuge, and the supernatant was decanted.
  • Acetone was added to the precipitate, and after stirring, the mixture was centrifuged under the same conditions as described above, and acetone was decanted. Then, it centrifuged twice similarly using distilled water, and obtained the silver fiber.
  • the fiber diameter (diameter) was 30 nm, and the fiber length was 3 ⁇ m.
  • the properties of the prepared polymer solution were measured by the following method.
  • Weight average molecular weight The weight average molecular weight (Mw) was measured by gel permeation chromatography (GPC), and was derived by conversion using a standard polystyrene calibration curve. The GPC conditions are shown below.
  • Hitachi L-6000 type (trade name, manufactured by Hitachi, Ltd.) Column: Gelpack GL-R420, Gelpack GL-R430, Gelpack GL-R440 (above, manufactured by Hitachi Chemical Co., Ltd., trade name) Eluent: Tetrahydrofuran Measurement temperature: 40 ° C Flow rate: 2.05 mL / min Detector: Hitachi L-3300 RI (trade name, manufactured by Hitachi, Ltd.)
  • the acid value was measured as follows. First, the binder polymer solution was heated at 130 ° C. for 1 hour to remove volatile components, thereby obtaining a solid polymer. Then, after precisely weighing 1 g of the solid polymer, the precisely weighed polymer was put into an Erlenmeyer flask, and 30 g of acetone was added and dissolved uniformly. Next, an appropriate amount of an indicator, phenolphthalein, was added to the solution, and titration was performed using a 0.1N aqueous KOH solution. And the acid value was computed by following Formula.
  • Acid value 0.1 ⁇ Vf ⁇ 56.1 / (Wp ⁇ I / 100)
  • Vf represents the titration amount (mL) of the KOH aqueous solution
  • Wp represents the mass (g) of the measured resin solution
  • I represents the proportion (mass%) of the non-volatile content in the measured resin solution.
  • the acid value of the polymer type ultraviolet absorber (D1) was also calculated by the same operation.
  • Example 1 ⁇ Preparation of photosensitive conductive film V1> [Preparation of conductive film (conductive film of photosensitive conductive film) W1]
  • the silver fiber dispersion obtained in Production Example 1 was uniformly applied at 25 g / m 2 on a 50 ⁇ m thick polyethylene terephthalate film (PET film, manufactured by Teijin Ltd., trade name “G2-50”), The film was dried with a hot air convection dryer at 100 ° C. for 3 minutes to form a conductive film W1.
  • the thickness of the conductive film after drying was 0.1 ⁇ m.
  • photosensitive conductive film V1 Preparation of photosensitive conductive film V1
  • the solution X1 of the photosensitive resin composition was uniformly applied on the conductive film W1, and dried for 10 minutes with a hot air convection dryer at 100 ° C. to form a photosensitive resin layer. Thereafter, the photosensitive resin layer was covered with a polyethylene film (trade name “NF-13” manufactured by Tamapoly Co., Ltd.) to obtain a photosensitive conductive film V1.
  • the film thickness after drying of the photosensitive resin layer was 5 ⁇ m.
  • the support film is removed, and further irradiated with ultraviolet rays at an exposure amount of 1 ⁇ 10 4 J / m 2 (measured value at i-line (wavelength 365 nm)) from the conductive film side with a parallel light exposure machine, and a photosensitive resin layer And a sample for measuring transmittance of the conductive film (photosensitive layer) (film thickness: 5.0 ⁇ m).
  • the ultraviolet light transmittance of the obtained sample was measured using a UV-visible spectrophotometer (trade name “U-3310” manufactured by Hitachi Instrument Service Co., Ltd.) in the measurement wavelength range of 300 to 380 nm, and the measurement wavelength.
  • the visible light transmittance was measured in the region of 400 to 700 nm.
  • permeability in the photosensitive conductive film independent was measured for the glass substrate as the background.
  • the visible light transmittance of the obtained photosensitive conductive film was 99% at a wavelength of 700 nm, 99% at a wavelength of 550 nm, and 87% at a wavelength of 400 nm.
  • the minimum value of the visible light transmittance in the wavelength region of 400 nm or more and 700 nm or less was 87%, and good transmittance was secured.
  • the ultraviolet light transmittance was 71% at 380 nm and 15% at 300 nm.
  • the maximum ultraviolet light transmittance at 300 to 380 nm was 71%.
  • a 41-step tablet (manufactured by Hitachi Chemical Co., Ltd.) is brought into close contact with the support film 1 of the photosensitive conductive film on the film substrate as a photomask, and a parallel light exposure machine (manufactured by Oak Manufacturing Co., Ltd., trade name “EXM1201”). )) From the support film 1 side and exposed through a photomask.
  • the exposure amount was 4 ⁇ 10 2 J / m 2 (measured value at i-line (wavelength 365 nm)). After the exposure, the substrate was allowed to stand at room temperature (23 ° C.
  • the sensitivity was evaluated based on the number of remaining steps after development. When the sensitivity of the photosensitive conductive film V1 was evaluated, it was 8 steps. The higher the number of steps of the remaining step tablet (the higher the numerical value), the higher the sensitivity.
  • a PET photomask having a wiring pattern with a line width / space width of 6/6 to 47/47 (unit: ⁇ m) is brought into intimate contact with the support film 1 of the photosensitive conductive film on the film substrate, and parallel rays Using an exposure machine (trade name “EXM1201” manufactured by Oak Seisakusho Co., Ltd.), exposure was performed from the support film 1 side through a photomask.
  • the exposure amount was an exposure amount at which the sensitivity of a 41-step tablet (manufactured by Hitachi Chemical Co., Ltd.) was 8 steps.
  • the substrate was allowed to stand at room temperature (23 ° C. to 25 ° C.) for 15 minutes, and then the support film 1 was removed.
  • the conductive layer in the unexposed area could be removed cleanly by the development process, and the conductive pattern could be formed without the exposed area being missing.
  • the resolution was evaluated by the smallest value of the line width / space width. It was 25 micrometers when the resolution of the photosensitive conductive film V1 was evaluated. The evaluation of resolution means that the smaller the numerical value, the better.
  • a laminator (Hitachi Chemical Co., Ltd.) is made so that the photosensitive resin layer is in contact with the easy-adhesion surface of a PET film substrate (thickness 50 ⁇ m, manufactured by Toyobo, trade name “A4100”) while peeling the polyethylene film of the photosensitive conductive film V1.
  • HMM-3000 type Manufactured under the trade name “HLM-3000 type” and laminated on a PET film substrate under conditions of a roll temperature of 110 ° C., a substrate feed rate of 1 m / min, and a pressure (cylinder pressure) of 4 ⁇ 10 5 Pa.
  • a film substrate on which a photosensitive conductive film V1 including a support film was laminated was produced.
  • a PET photomask having a wiring pattern with a line width / space width of 6/6 to 47/47 (unit: ⁇ m) is brought into intimate contact with the support film 1 of the photosensitive conductive film on the film substrate, and parallel rays Using an exposure machine (Oak Seisakusho Co., Ltd., trade name “EXM1201”), exposure was performed from the support film 1 side through a photomask (first stage exposure).
  • the exposure amount was an exposure amount at which the sensitivity of a 41-step tablet (manufactured by Hitachi Chemical Co., Ltd.) was 8 steps.
  • the exposure amount was set to be three times the exposure amount of the first stage exposure.
  • the film was allowed to stand at room temperature (23 ° C. to 25 ° C.) for 15 minutes, and then developed by spraying a 1% by mass aqueous sodium carbonate solution at 30 ° C. for 30 seconds.
  • the resolution was evaluated by the smallest value of the line width / space width in which the conductive fiber pattern could be formed without missing in the exposed portion at times.
  • the resolution of the photosensitive conductive film V1 was evaluated, it was 20 ⁇ m. The evaluation of resolution means that the smaller the numerical value, the better.
  • Examples 7 and 8 Except having used the conductive film W2 or W3 instead of the conductive film W1, the photosensitive conductive film was produced similarly to Example 1 and various characteristics were evaluated. The results are shown in Table 4.
  • the production methods of the conductive films W2 and W3 are as follows.
  • conductive film (conductive film of photosensitive conductive film) W2]
  • the silver fiber dispersion obtained in Production Example 1 above was uniformly applied at 20 g / m 2 onto a 50 ⁇ m-thick polyethylene terephthalate film (PET film, manufactured by Teijin Ltd., trade name “G2-50”), The film was dried with a hot air convection dryer at 100 ° C. for 3 minutes to form a conductive film W2.
  • the film thickness after drying of the conductive film was 0.08 ⁇ m.
  • conductive film (conductive film of photosensitive conductive film) W3]
  • the carbon nanotube dispersion obtained in Production Example 1 above was uniformly applied at 30 g / m 2 on a polyethylene terephthalate film (PET film, manufactured by Teijin Ltd., trade name “G2-50”) having a thickness of 50 ⁇ m, The film was dried with a hot air convection dryer at 100 ° C. for 3 minutes to form a conductive film W3.
  • the thickness of the conductive film after drying was 0.05 ⁇ m.
  • Comparative Example 4 A photosensitive conductive film was prepared in the same manner as in Example 1 except that the conductive film W3 was used instead of the conductive film W1 and the photosensitive resin composition solution (X) shown in Table 5 was used. Characteristics were evaluated. The results are shown in Table 5.
  • a conductive pattern can be formed with sufficient resolution even when the photosensitive layer contains conductive fibers. Moreover, it can use for manufacture of the touchscreen containing preparation of the base material with a conductive pattern which has sufficient resolution, and a base material with a conductive pattern.
  • SYMBOLS 1 Support film, 2 ... Conductive film, 2a ... Conductive pattern, 3 ... Photosensitive resin layer, 3a ... Resin hardened layer, 3b ... Resin hardened pattern, 4 ... Photosensitive layer, 5 ... Protective film, 6 ... Mask pattern, 10 , 12 ... photosensitive conductive film, 20 ... base material, 40, 41, 42 ... base material with conductive pattern, 101 ... transparent base material, 102 ... touch screen, 103 ... transparent electrode (X position coordinate), 104 ... transparent electrode (Y position coordinate).

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • General Engineering & Computer Science (AREA)
  • Theoretical Computer Science (AREA)
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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Materials For Photolithography (AREA)

Abstract

La présente invention a trait à un film conducteur photosensible qui est muni d'un film de support et d'une couche photosensible située sur le film de support, la couche photosensible contenant des fibres conductrices, un polymère liant, un composé photopolymérisable, un initiateur de photopolymérisation, ainsi qu'un absorbant d'ultraviolet.
PCT/JP2016/061728 2015-04-15 2016-04-11 Film conducteur photosensible, procédé de formation d'un motif conducteur, substrat ayant un motif conducteur, et capteur de panneau tactile WO2016167228A1 (fr)

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WO2020060057A1 (fr) * 2018-09-19 2020-03-26 삼성디스플레이 주식회사 Dispositif d'affichage
JP2022032022A (ja) * 2020-08-10 2022-02-24 カンブリオス フィルム ソリューションズ（シアメン） コーポレーション 透明導電膜及びその製造方法
WO2022138630A1 (fr) * 2020-12-25 2022-06-30 富士フイルム株式会社 Film de transfert, procédé de production de stratifié et procédé de production de câblage de circuit
WO2022181016A1 (fr) * 2021-02-26 2022-09-01 富士フイルム株式会社 Méthode de production d'un motif conducteur et méthode de production de dispositif électronique
WO2023090253A1 (fr) * 2021-11-22 2023-05-25 富士フイルム株式会社 Stratifié, son procédé de production et dispositif électronique

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WO2022138630A1 (fr) * 2020-12-25 2022-06-30 富士フイルム株式会社 Film de transfert, procédé de production de stratifié et procédé de production de câblage de circuit
WO2022181016A1 (fr) * 2021-02-26 2022-09-01 富士フイルム株式会社 Méthode de production d'un motif conducteur et méthode de production de dispositif électronique
WO2023090253A1 (fr) * 2021-11-22 2023-05-25 富士フイルム株式会社 Stratifié, son procédé de production et dispositif électronique

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