WO2014207952A1 - 透明導電性積層フィルム、その製造方法及びタッチパネル - Google Patents
透明導電性積層フィルム、その製造方法及びタッチパネル Download PDFInfo
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- WO2014207952A1 WO2014207952A1 PCT/JP2013/078232 JP2013078232W WO2014207952A1 WO 2014207952 A1 WO2014207952 A1 WO 2014207952A1 JP 2013078232 W JP2013078232 W JP 2013078232W WO 2014207952 A1 WO2014207952 A1 WO 2014207952A1
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- transparent conductive
- laminated film
- transparent
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- conductive laminated
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- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/144—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers using layers with different mechanical or chemical conditions or properties, e.g. layers with different thermal shrinkage, layers under tension during bonding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/24—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer not being coherent before laminating, e.g. made up from granular material sprinkled onto a substrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/0008—Electrical discharge treatment, e.g. corona, plasma treatment; wave energy or particle radiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/0036—Heat treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/10—Removing layers, or parts of layers, mechanically or chemically
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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
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
- C08F220/283—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety and containing one or more carboxylic moiety in the chain, e.g. acetoacetoxyethyl(meth)acrylate
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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 active energy ray-curable adhesive composition is preferably used in combination with a photoacid generator (H) and a compound (I) containing either an alkoxy group or an epoxy group. .
- the method for forming the transparent conductive layer is not particularly limited, and a conventionally known method can be employed. Specifically, for example, a vacuum deposition method, a sputtering method, and an ion plating method can be exemplified. In addition, an appropriate method can be adopted depending on the required film thickness.
- the radically polymerizable compound (A) has a radically polymerizable group such as a (meth) acryloyl group and has an SP value of 29.0 (kJ / m 3 ) 1/2 or more and 32.0 or less (kJ / m 3 ) Any compound that is 1 ⁇ 2 can be used without limitation.
- Specific examples of the radical polymerizable compound (A) include hydroxyethyl acrylamide (SP value 29.6), N-methylol acrylamide (SP value 31.5) and the like.
- the radical polymerizable compound (C) has a radical polymerizable group such as a (meth) acryloyl group and has an SP value of 21.0 (kJ / m 3 ) 1/2 or more and 23.0 (kJ / m 3 ). Any compound that is 1 ⁇ 2 or less can be used without limitation.
- Specific examples of the radical polymerizable compound (C) include, for example, acryloylmorpholine (SP value 22.9), N-methoxymethylacrylamide (SP value 22.9), N-ethoxymethylacrylamide (SP value 22.3). Etc.
- the active energy ray curable adhesive composition has the radical polymerizable compounds (A) and (B) when the total amount of the radical polymerizable compound in the active energy ray curable adhesive composition is 100 parts by weight. And (C) in a total amount of 85 parts by weight or more, and further a radical polymerization having an SP value of more than 23.0 (kJ / m 3 ) 1/2 and less than 29.0 (kJ / m 3 ) 1/2
- the active compound (E) can be contained in an amount of 15 parts by weight or less.
- the acrylic oligomer (D) is preferably used in the range of 20% by weight or less.
- the acrylic oligomer (D) is preferably contained in an amount of 3% by weight or more, more preferably 5% by weight or more in the adhesive composition. preferable.
- the content of the acrylic oligomer (D) in the adhesive composition is preferably 20% by weight or less, and more preferably 15% by weight or less.
- the radically polymerizable compound (F) having an active methylene group examples include 2-acetoacetoxyethyl (meth) acrylate, 2-acetoacetoxypropyl (meth) acrylate, 2-acetoacetoxy-1-methylethyl (meta) ) Acetoacetoxyalkyl (meth) acrylate such as acrylate; 2-ethoxymalonyloxyethyl (meth) acrylate, 2-cyanoacetoxyethyl (meth) acrylate, N- (2-cyanoacetoxyethyl) acrylamide, N- (2-propionyl) Acetoxybutyl) acrylamide, N- (4-acetoacetoxymethylbenzyl) acrylamide, N- (2-acetoacetylaminoethyl) acrylamide and the like.
- the SP value of the radically polymerizable compound (F) having an active methylene group is not particularly limited, and a compound having an arbitrary value
- a radical is generated in the methylene group of the radical polymerizable compound (F) having an active methylene group in the presence of the radical polymerization initiator (G) having a hydrogen abstracting action, and the methylene group And a hydroxyl group of a polarizer such as PVA react to form a covalent bond. Therefore, in order to generate radicals in the methylene group of the radically polymerizable compound (F) having an active methylene group and to sufficiently form such a covalent bond, when the total amount of the composition is 100% by weight, it has an active methylene group.
- the active energy ray-curable resin composition contains a photoacid generator
- the water resistance and durability of the adhesive layer are dramatically improved as compared with the case where no photoacid generator is contained. be able to.
- the photoacid generator (H) can be represented by the following general formula (3).
- R 1 , R 2 and R 3 are each independently a hydrogen atom, a substituted or unsubstituted alkyl group, a substituted or unsubstituted alkenyl group, substituted or An unsubstituted aryl group, a substituted or unsubstituted heterocyclic group, a substituted or unsubstituted alkoxyl group, a substituted or unsubstituted aryloxy group, a substituted or unsubstituted heterocyclic oxy group, a substituted or unsubstituted acyl group, R 4 represents a group selected from a substituted or unsubstituted carbonyloxy group, a substituted or unsubstituted oxycarbonyl group, or a halogen atom, and R 4 represents a group similar to the groups described in R 1 , R 2 and R 3.
- .R 5 is a substituted or unsubstituted alkyl group
- R 6 and R 7 represents a substituted or unsubstituted alkylthio group, independently, be substituted
- Alkyl group substituted or unsubstituted alkenyl group, substituted or unsubstituted aryl group, substituted or unsubstituted heterocyclic group, substituted or unsubstituted alkoxyl group, substituted or unsubstituted aryloxy group, substituted or unsubstituted Heterocyclic oxy group, substituted or unsubstituted alkylthio group, substituted or unsubstituted arylthio group, substituted or unsubstituted heterocyclic thio group, substituted or unsubstituted acyl group, substituted or unsubstituted carbonyloxy group, substituted or .Ar 4 represent either a non-substituted oxycarbonyl group, Ar Is a substituted or unsubstituted aryl group, .X represent either a substituted or unsubstituted heterocyclic group, .j is .i representing an oxygen or sulfur atom represents
- Adjacent Rs, Ar 4 and Ar 5 , R 2 and R 3 , R 2 and R 4 , R 3 and R 4 , R 1 and R 2 , R 1 and R 3 , R 1 and R 4 , R 1 and R, or R 1 and R 5 may be a cyclic structure bonded to each other.
- Onium cation (sulfonium cation) corresponding to general formula (4): Dimethylphenylsulfonium, dimethyl (o-fluorophenyl) sulfonium, dimethyl (m-chlorophenyl) sulfonium, dimethyl (p-bromophenyl) sulfonium, dimethyl (p-cyanophenyl) sulfonium, dimethyl (m-nitrophenyl) sulfonium, dimethyl ( 2,4,6-tribromophenyl) sulfonium, dimethyl (pentafluorophenyl) sulfonium, dimethyl (p- (trifluoromethyl) phenyl) sulfonium, dimethyl (p-hydroxyphenyl) sulfonium, dimethyl (p-mercaptophenyl) sulfonium , Dimethyl (p-methylsulfinylphenyl) sulfonium, dimethyl
- Onium cation corresponding to general formula (7) (pyridinium cation): Examples of pyridinium cations: N-phenylpyridinium, N- (o-chlorophenyl) pyridinium, N- (m-chlorophenyl) pyridinium, N- (p-cyanophenyl) pyridinium, N- (o-nitrophenyl) pyridinium, N- (p-acetylphenyl) ) Pyridinium, N- (p-isopropylphenyl) pyridinium, N- (p-octadecyloxyphenyl) pyridinium, N- (p-methoxycarbonylphenyl) pyridinium, N- (9-anthryl) pyridinium, 2-chloro-1- Phenylpyridinium, 2-cyano-1-phenylpyridinium, 2-methyl-1-phenylpyridinium, 2-viny
- Onium cation (quinolinium cation) corresponding to general formula (8): Examples of quinolinium cations: N-methylquinolinium, N-ethylquinolinium, N-phenylquinolinium, N-naphthylquinolinium, N- (o-chlorophenyl) quinolinium, N- (m-chlorophenyl) quinolinium, N- (p -Cyanophenyl) quinolinium, N- (o-nitrophenyl) quinolinium, N- (p-acetylphenyl) quinolinium, N- (p-isopropylphenyl) quinolinium, N- (p-octadecyloxyphenyl) quinolinium, N- ( p-methoxycarbonylphenyl) quinolinium, N- (9-anthryl) quinolinium, 2-chloro-1-phenylquinolinium, 2-cyano-1-phenylquino
- Onium cation (isoquinolinium cation) corresponding to the general formula (9):
- isoquinolinium cations N-phenylisoquinolinium, N-methylisoquinolinium, N-ethylisoquinolinium, N- (o-chlorophenyl) isoquinolinium, N- (m-chlorophenyl) isoquinolinium, N- (p-cyanophenyl) Isoquinolinium, N- (o-nitrophenyl) isoquinolinium, N- (p-acetylphenyl) isoquinolinium, N- (p-isopropylphenyl) isoquinolinium, N- (p-octadecyloxyphenyl) isoquinolinium, N- (p-methoxycarbonyl) Phenyl) isoquinolinium, N- (9-anthryl) isoquinolinium, 1,2-diphenylisoquinolinium, N- (2-fury
- Onium cation corresponding to general formula (10) (benzoxazolium cation, benzothiazolium cation): Examples of benzoxazolium cations: N-methylbenzoxazolium, N-ethylbenzoxazolium, N-naphthylbenzoxazolium, N-phenylbenzoxazolium, N- (p-fluorophenyl) benzoxazolium, N- (p- Chlorophenyl) benzoxazolium, N- (p-cyanophenyl) benzoxazolium, N- (o-methoxycarbonylphenyl) benzoxazolium, N- (2-furyl) benzoxazolium, N- (o -Fluorophenyl) benzoxazolium, N- (p-cyanophenyl) benzoxazolium, N- (m-nitrophenyl) benzoxazolium, N- (p-iso
- benzothiazolium cations N-methylbenzothiazolium, N-ethylbenzothiazolium, N-phenylbenzothiazolium, N- (1-naphthyl) benzothiazolium, N- (p-fluorophenyl) benzothiazolium, N -(P-chlorophenyl) benzothiazolium, N- (p-cyanophenyl) benzothiazolium, N- (o-methoxycarbonylphenyl) benzothiazolium, N- (p-tolyl) benzothiazolium, N- (o-fluorophenyl) benzothiazolium, N- (m-nitrophenyl) benzothiazolium, N- (p-isopropoxycarbonylphenyl) benzothiazolium, N- (2-furyl) benzothia Zorium, N- (4-methylthiophenyl) benzothiazolium, N-
- Onium cation corresponding to general formula (11) (furyl or thienyl iodonium cation): Difuryliodonium, dithienyliodonium, bis (4,5-dimethyl-2-furyl) iodonium, bis (5-chloro-2-thienyl) iodonium, bis (5-cyano-2-furyl) iodonium, bis (5- Nitro-2-thienyl) iodonium, bis (5-acetyl-2-furyl) iodonium, bis (5-carboxy-2-thienyl) iodonium, bis (5-methoxycarbonyl-2-furyl) iodonium, bis (5-phenyl) -2-furyl) iodonium, bis (5- (p-methoxyphenyl) -2-thienyl) iodonium, bis (5-vinyl-2-furyl) iodonium, bis (5-ethyn
- Onium cation corresponding to general formula (12) (diaryliodonium cation): Diphenyliodonium, bis (p-tolyl) iodonium, bis (p-octylphenyl) iodonium, bis (p-octadecylphenyl) iodonium, bis (p-octyloxyphenyl) iodonium, bis (p-octadecyloxyphenyl) iodonium, phenyl (P-octadecyloxyphenyl) iodonium, 4-isopropyl-4′-methyldiphenyliodonium, (4-isobutylphenyl) -p-tolyliodonium, bis (1-naphthyl) iodonium, bis (4-phenylsulfanylphenyl) iodonium, Phenyl (6-benzoyl-9-ethy
- counter anion X in - are but are not theoretically limited to, non-nucleophilic anion is preferred.
- the counter anion X ⁇ is a non-nucleophilic anion, a nucleophilic reaction is unlikely to occur in cations coexisting in the molecule and various materials used in combination, and as a result, the photoacid generator itself represented by the general formula (4) It is possible to improve the aging stability of a composition using the same.
- the non-nucleophilic anion here refers to an anion having a low ability to cause a nucleophilic reaction.
- Examples of such anions include PF 6 ⁇ , SbF 6 ⁇ , AsF 6 ⁇ , SbCl 6 ⁇ , BiCl 5 ⁇ , SnCl 6 ⁇ , ClO 4 ⁇ , dithiocarbamate anion, SCN ⁇ and the like.
- the counter anion X ⁇ in the general formula (3) particularly preferred as the counter anion X ⁇ in the general formula (3) include PF 6 ⁇ , SbF 6 ⁇ , and AsF 6 ⁇ , and particularly preferably PF 6 ⁇ , SbF 6 - and the like.
- preferable onium salts constituting the photoacid generator (H) of the present invention include specific examples of the structure of the onium cation represented by the above general formulas (4) to (12).
- the content of the photoacid generator (H) is preferably 0.01 to 10% by weight, and preferably 0.05 to 5% by weight, based on the total amount of the active energy ray-curable resin composition. Is more preferable, and 0.1 to 3% by weight is particularly preferable.
- Examples of the polymer having one or more epoxy groups in the molecule include epoxy resins, bisphenol A type epoxy resins derived from bisphenol A and epichlorohydrin, bisphenol F type epoxy derived from bisphenol F and epichlorohydrin.
- Resin bisphenol S type epoxy resin, phenol novolak type epoxy resin, cresol novolak type epoxy resin, bisphenol A novolak type epoxy resin, bisphenol F novolak type epoxy resin, alicyclic epoxy resin, diphenyl ether type epoxy resin, hydroquinone type epoxy resin, Multifunctional epoxy resin such as naphthalene type epoxy resin, biphenyl type epoxy resin, fluorene type epoxy resin, trifunctional type epoxy resin and tetrafunctional type epoxy resin There are glycidyl ester type epoxy resins, glycidyl amine type epoxy resins, hydantoin type epoxy resins, isocyanurate type epoxy resins, aliphatic chain epoxy resins, etc.
- epoxy resins may be halogenated and hydrogenated. May be.
- resin products for example, JER Coat 828, 1001, 801N, 806, 807, 152, 604, 630, 871, YX8000, YX8034, YX4000 manufactured by Japan Epoxy Resin Co., Ltd., Epicron manufactured by DIC Corporation 830, EXA835LV, HP4032D, HP820, EP4100 series, EP4000 series, EPU series, manufactured by ADEKA Co., Ltd., Celoxide series (2021, 2021P, 2083, 2085, 3000, etc.) manufactured by Daicel Chemical Industries, Ltd., Eporide series, EHPE Series, YD series, YDF series, YDCN series, YDB series, phenoxy resin (polyethylene synthesized from bisphenols and epichlorohydrin) B carboxymethyl having an epoxy group at both ends with polyether; YP series, etc.), Nagase Chemt
- the compound having an alkoxyl group in the molecule is not particularly limited as long as it has one or more alkoxyl groups in the molecule, and known compounds can be used. Representative examples of such compounds include melamine compounds, amino resins, and silane coupling agents. In calculating the glass transition temperature Tg of the adhesive layer, the compound having an alkoxyl group and the polymer (H) are not included in the calculation.
- silane coupling agent (J) having an amino group examples include ⁇ -aminopropyltrimethoxysilane, ⁇ -aminopropyltriethoxysilane, ⁇ -aminopropyltriisopropoxysilane, ⁇ -aminopropylmethyldimethoxysilane, ⁇ -aminopropylmethyldiethoxysilane, ⁇ - (2-aminoethyl) aminopropyltrimethoxysilane, ⁇ - (2-aminoethyl) aminopropylmethyldimethoxysilane, ⁇ - (2-aminoethyl) aminopropyltriethoxysilane ⁇ - (2-aminoethyl) aminopropylmethyldiethoxysilane, ⁇ - (2-aminoethyl) aminopropyltriisopropoxysilane, ⁇ - (2- (2-aminoethyl) aminoethyl) aminopropyltrime
- the silane coupling agent (J) having an amino group may be used alone or in combination of two or more.
- the compounding amount of the amino group-containing silane coupling agent (J) is preferably in the range of 0.01 to 20% by weight and preferably 0.05 to 15% by weight when the total amount of the composition is 100% by weight.
- the content is 0.1 to 10% by weight. This is because when the blending amount exceeds 20% by weight, the storage stability of the adhesive deteriorates, and when the blending amount is less than 0.1% by weight, the water-resistant adhesive effect is not sufficiently exhibited.
- the silane coupling agent (J) having an amino group is not included in the calculation.
- the active energy ray curable adhesive composition When used in an electron beam curable type, it is not particularly necessary to include a photopolymerization initiator in the composition, but when used in a visible light curable type or an ultraviolet curable type.
- a photopolymerization initiator Is preferably a photopolymerization initiator, and particularly preferably a photopolymerization initiator that is highly sensitive to light of 380 nm or more.
- a photopolymerization initiator that is highly sensitive to light of 380 nm or more will be described later.
- a photopolymerization initiator a compound represented by the following general formula (1); (Wherein R 1 and R 2 represent —H, —CH 2 CH 3 , —iPr or Cl, and R 1 and R 2 may be the same or different), respectively, or a general formula ( It is preferable to use together the compound represented by 1) and a photopolymerization initiator that is highly sensitive to light of 380 nm or more, which will be described later. When the compound represented by the general formula (1) is used, the adhesiveness is excellent as compared with a case where a photopolymerization initiator having high sensitivity to light of 380 nm or more is used alone.
- the composition ratio of the compound represented by the general formula (1) in the composition is preferably 0.1 to 5.0% by weight when the total amount of the composition is 100% by weight, and preferably 0.5 to 4%. It is more preferably 0.0% by weight, and even more preferably 0.9 to 3.0% by weight.
- polymerization initiators include triethylamine, diethylamine, N-methyldiethanolamine, ethanolamine, 4-dimethylaminobenzoic acid, methyl 4-dimethylaminobenzoate, ethyl 4-dimethylaminobenzoate, isoamyl 4-dimethylaminobenzoate, etc. Among them, ethyl 4-dimethylaminobenzoate is particularly preferable.
- a polymerization initiation assistant its addition amount is usually 0 to 5% by weight, preferably 0 to 4% by weight, most preferably 0 to 3% by weight, when the total amount of the composition is 100% by weight. .
- the photopolymerization initiator is a photopolymerization initiator that is highly sensitive to light of 380 nm or more. Is preferably used.
- 2-methyl-1- (4-methylthiophenyl) -2-morpholinopropan-1-one 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) -butanone-1 2- (dimethylamino) -2-[(4-methylphenyl) methyl] -1- [4- (4-morpholinyl) phenyl] -1-butanone, 2,4,6-trimethylbenzoyl-diphenyl-phosphine Oxide, bis (2,4,6-trimethylbenzoyl) -phenylphosphine oxide, bis ( ⁇ 5-2,4-cyclopentadien-1-yl) -bis (2,6-difluoro-3- (1H-pyrrole) 1-yl) -phenyl) titanium and the like.
- a photopolymerization initiator in addition to the photopolymerization initiator of the general formula (1), a compound represented by the following general formula (2); Wherein R 3 , R 4 and R 5 represent —H, —CH 3 , —CH 2 CH 3 , —iPr or Cl, and R 3 , R 4 and R 5 may be the same or different. It is preferable to use it.
- the compound represented by the general formula (2) 2-methyl-1- (4-methylthiophenyl) -2-morpholinopropan-1-one (trade name: IRGACURE907 manufacturer: BASF) which is also a commercially available product is suitable. Can be used.
- 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) -butanone-1 (trade name: IRGACURE369 manufacturer: BASF)
- 2- (dimethylamino) -2-[(4-methylphenyl) Methyl] -1- [4- (4-morpholinyl) phenyl] -1-butanone (trade name: IRGACURE379 manufacturer: BASF) is preferred because of its high sensitivity.
- additives can be blended as other optional components as long as the objects and effects of the present invention are not impaired.
- additives include epoxy resin, polyamide, polyamideimide, polyurethane, polybutadiene, polychloroprene, polyether, polyester, styrene-butadiene block copolymer, petroleum resin, xylene resin, ketone resin, cellulose resin, fluorine-based oligomer, Polymers or oligomers such as silicone oligomers and polysulfide oligomers; polymerization inhibitors such as phenothiazine and 2,6-di-t-butyl-4-methylphenol; polymerization initiators; leveling agents; wettability improvers; Plasticizer; UV absorber; Silane coupling agent; Inorganic filler; Pigment;
- the silane coupling agent can act on the surface of a film substrate such as the first or second film substrate, and can impart an improvement in adhesion.
- a silane coupling agent When a silane coupling agent is used, its addition amount is usually 0 to 10% by weight, preferably 0 to 5% by weight, most preferably 0 to 3% by weight, when the total amount of the composition is 100% by weight. .
- an active energy ray-curable compound is preferably used, but the same water resistance can be imparted even if it is not active energy ray-curable.
- silane coupling agents include vinyltrichlorosilane, vinyltrimethoxysilane, vinyltriethoxysilane, 2- (3,4 epoxycyclohexyl) ethyltrimethoxysilane, and 3-glycid as active energy ray-curable compounds.
- Xylpropyltrimethoxysilane 3-glycidoxypropylmethyldiethoxysilane, 3-glycidoxypropyltriethoxysilane, p-styryltrimethoxysilane, 3-methacryloxypropylmethyldimethoxysilane, 3-methacryloxypropyltrimethoxy Examples thereof include silane, 3-methacryloxypropylmethyldiethoxysilane, 3-methacryloxypropyltriethoxysilane, and 3-acryloxypropyltrimethoxysilane.
- the active energy ray-curable adhesive composition used in the present invention is cured by irradiating active energy rays to form an adhesive layer.
- an electron beam one containing visible light having a wavelength range of 380 nm to 450 nm can be used.
- the long wavelength limit of visible light is about 780 nm, but visible light exceeding 450 nm does not contribute to the absorption of the polymerization initiator, but may cause heat generation of the transparent protective film and the polarizer. For this reason, in the present invention, it is preferable to block visible light on the long wavelength side exceeding 450 nm using a band-pass filter.
- the acceleration voltage is preferably 5 kV to 300 kV, and more preferably 10 kV to 250 kV. If the acceleration voltage is less than 5 kV, the electron beam may not reach the adhesive and may be insufficiently cured. If the acceleration voltage exceeds 300 kV, the penetration force through the sample is too strong and damages the transparent protective film and the polarizer. There is a risk of giving.
- the irradiation dose is 5 to 100 kGy, more preferably 10 to 75 kGy.
- the adhesive becomes insufficiently cured, and when it exceeds 100 kGy, the transparent protective film and the polarizer are damaged, resulting in a decrease in mechanical strength and yellowing, thereby obtaining predetermined optical characteristics. I can't.
- the electron beam irradiation is usually performed in an inert gas, but if necessary, it may be performed in the atmosphere or under a condition where a little oxygen is introduced. Depending on the material of the transparent protective film, by appropriately introducing oxygen, the transparent protective film surface where the electron beam first hits can be obstructed to prevent oxygen damage and prevent damage to the transparent protective film. An electron beam can be irradiated efficiently.
- the wavelength range is used as an active energy ray. It is preferable to use an active energy ray that contains visible light having a wavelength of 380 nm to 450 nm, in particular, an active energy ray having the largest irradiation amount of visible light having a wavelength range of 380 nm to 450 nm.
- a transparent protective film (ultraviolet non-transparent transparent protective film) imparted with ultraviolet absorbing ability
- light having a wavelength shorter than 380 nm is absorbed, so that light having a wavelength shorter than 380 nm is an active energy ray-curable adhesive composition. Since it does not reach the product, it does not contribute to the polymerization reaction. Furthermore, light having a wavelength shorter than 380 nm absorbed by the transparent protective film is converted into heat, and the transparent protective film itself generates heat, which causes defects such as curling and wrinkling of the polarizing film.
- an apparatus that does not emit light having a wavelength shorter than 380 nm as the active energy ray generator, and more specifically, an integrated illuminance in the wavelength range of 380 to 440 nm and a wavelength range of 250 to 370 nm. Is preferably from 100: 0 to 100: 50, and more preferably from 100: 0 to 100: 40.
- the active energy ray satisfying such a relationship of integrated illuminance a gallium-filled metal halide lamp and an LED light source that emits light in the wavelength range of 380 to 440 nm are preferable.
- low pressure mercury lamp, medium pressure mercury lamp, high pressure mercury lamp, ultra high pressure mercury lamp, incandescent lamp, xenon lamp, halogen lamp, carbon arc lamp, metal halide lamp, fluorescent lamp, tungsten lamp, gallium lamp, excimer laser or sunlight as the light source
- a light having a wavelength shorter than 380 nm by using a band pass filter.
- a bandpass filter capable of blocking light having a wavelength shorter than 400 nm.
- an active energy ray having a wavelength of 405 nm obtained by using an active energy ray or an LED light source.
- the active energy ray-curable adhesive composition before irradiation with visible light (pre-irradiation warming), in which case it is preferable to heat to 40 ° C. or higher. It is more preferable to heat to more than ° C. It is also preferable to warm the active energy ray-curable adhesive composition after irradiation with visible light (heating after irradiation), in which case it is preferable to warm to 40 ° C. or higher, and warm to 50 ° C. or higher. It is more preferable.
- the active energy ray curable adhesive composition forms a transparent curable adhesive layer for adhering film substrates such as first and second film substrates having a light transmittance of less than 5%, particularly at a wavelength of 365 nm.
- the said active energy ray hardening-type adhesive composition contains film bases, such as a 1st, 2nd film base material etc. which have UV absorption ability by containing the photoinitiator of General formula (1) mentioned above.
- the transparent cured adhesive layer can be cured and formed by irradiating visible light or ultraviolet rays through the material.
- the transparent cured adhesive layer can be cured even in film substrates such as the first and second film substrates that do not have UV absorbing ability.
- film base materials such as the 1st and 2nd film base materials which have UV absorption ability
- Examples of a method for imparting UV absorbing ability to a film substrate such as the first and second film substrates include a method of containing an ultraviolet absorber in a film substrate such as the first and second film substrates, The method of laminating
- ultraviolet absorber examples include conventionally known oxybenzophenone compounds, benzotriazole compounds, salicylic acid ester compounds, benzophenone compounds, cyanoacrylate compounds, nickel complex compounds, triazine compounds, and the like.
- the thickness of the transparent cured adhesive layer it is preferable to control the thickness of the transparent cured adhesive layer to be 0.01 ⁇ m or more and 10 ⁇ m or less.
- the thickness of the transparent cured adhesive layer is preferably 0.01 to 8 ⁇ m, more preferably 0.01 to 5 ⁇ m, still more preferably 0.01 to 2 ⁇ m, and most preferably 0.01 to 1 ⁇ m.
- the thickness of the transparent cured adhesive layer is thinner than 0.01 ⁇ m, the cohesive force of the adhesive force itself cannot be obtained, and the adhesive strength may not be obtained.
- the thickness of the transparent cured adhesive layer it is preferable that the thickness of the transparent cured adhesive layer be 10 ⁇ m or less because the curing time of the adhesive composition can be easily controlled.
- the transparent conductive laminated film A is transparent on one side of the first, second, and third film bases 11, 12, and 13 via an undercoat layer.
- Conductive layers 21 and 22 can be provided.
- the undercoat layer may have a multilayer structure of two or more layers.
- the transparent conductive laminated film A is transparently cured through an oligomer layer on one side of the first, second, and third film bases 11, 12, and 13. It can have an adhesive layer 3.
- the refractive index of the transparent conductive layer is usually about 1.95 to 2.05.
- the difference in refractive index from the transparent conductive layer is preferably 0.1 or more.
- the undercoat layer can be formed of an inorganic material, an organic material, or a mixture of an inorganic material and an organic material.
- NaF 1.3
- Na 3 AlF 6 (1.35)
- LiF (1.36 LiF (1.36)
- MgF 2 (1.38)
- CaF 2 1.4
- BaF 2 (1. 3)
- inorganic substances such as SiO 2 (1.46), LaF 3 (1.55), CeF 3 (1.63), Al 2 O 3 (1.63) It is a rate].
- SiO 2 , MgF 2 , A1 2 O 3 and the like are preferably used.
- SiO 2 is suitable.
- a composite oxide containing about 10 to 40 parts by weight of cerium oxide and about 0 to 20 parts by weight of tin oxide with respect to indium oxide can be used.
- the undercoat layer formed of an inorganic material can be formed as a dry process such as a vacuum deposition method, a sputtering method, or an ion plating method, or by a wet method (coating method).
- a wet method coating method
- SiO 2 is preferable as described above.
- a SiO 2 film can be formed by applying silica sol or the like.
- examples of the organic material include acrylic resin, urethane resin, melamine resin, alkyd resin, siloxane polymer, and organic silane condensate. At least one of these organic substances is used.
- a thermosetting resin made of a mixture of a melamine resin, an alkyd resin, and an organosilane condensate.
- An undercoat layer can be provided between a 1st, 2nd film base material and a transparent conductive layer, and does not have a function as a conductor layer. That is, the undercoat layer is provided as a dielectric layer that insulates between the patterned transparent conductive layers. Therefore, the undercoat layer usually has a surface resistance of 1 ⁇ 10 6 ⁇ / ⁇ or more, preferably 1 ⁇ 10 7 ⁇ / ⁇ or more, and more preferably 1 ⁇ 10 8 ⁇ / ⁇ or more.
- the upper limit of the surface resistance of the undercoat layer is not particularly limited. In general, the upper limit of the surface resistance of the undercoat layer is about 1 ⁇ 10 13 ⁇ / ⁇ , which is the measurement limit, but may exceed 1 ⁇ 10 13 ⁇ / ⁇ .
- the refractive index of the undercoat layer is preferably such that the difference between the refractive index of the transparent conductive layer and the refractive index of the undercoat layer is 0.1 or more.
- the difference between the refractive index of the transparent conductive layer and the refractive index of the undercoat layer is preferably from 0.1 to 0.9, and more preferably from 0.1 to 0.6.
- the refractive index of the undercoat layer is usually 1.3 to 2.5, more preferably 1.38 to 2.3, and further preferably 1.4 to 2.3.
- the thickness of the undercoat layer is not particularly limited, but is usually about 1 to 300 nm, preferably 5 from the viewpoint of the optical design and the effect of preventing oligomer generation from the first and second film substrates. ⁇ 300 nm.
- the thickness of each layer is about 5 to 250 nm, preferably 10 to 250 nm.
- the surface on the opposite side to the 1st transparent conductive layer 21 of laminated film A '(The 2nd film base material 12 in FIG. 1, 3rd film in FIG. A functional layer can be provided on one side of the substrate 13: the opposite side of the transparent cured adhesive layer 3.
- an antiglare treatment layer, an antireflection layer, and a hard coat layer can be provided.
- the constituent material of the antiglare layer is not particularly limited, and for example, an ionizing radiation curable resin, a thermosetting resin, a thermoplastic resin, or the like can be used.
- the thickness of the antiglare treatment layer is preferably from 0.1 to 30 ⁇ m.
- the antireflection layer titanium oxide, zirconium oxide, silicon oxide, magnesium fluoride or the like is used. In order to express the antireflection function more greatly, it is preferable to use a laminate of a titanium oxide layer and a silicon oxide layer.
- the method for producing a transparent conductive laminated film of the present invention is not particularly limited as long as the method having the above structure is obtained.
- An example of the manufacturing method is shown below.
- a transparent conductive film provided with a first transparent conductive layer on one surface of a first film substrate is prepared (step a).
- a first transparent conductive layer (which may include an undercoat layer) is formed on one surface of the first film substrate.
- a transparent conductive laminated film as shown in FIG. 2, FIG. 4, ie, when a 2nd film base material or a 3rd film base material also has a transparent conductive layer, it is the 2nd film base material.
- a transparent conductive film in which a second transparent conductive layer is provided on one surface of the third film substrate can be prepared.
- the other surface of the first film substrate that does not have the first transparent conductive layer and the second film substrate are pasted with a transparent uncured adhesive layer.
- the transparent uncured adhesive layer can be formed by applying a curable adhesive to at least one of the first film substrate and the second film substrate.
- the second film base and the third film base were pasted together with a transparent uncured adhesive layer in advance. Can be used with things.
- the coating method of the curable adhesive is appropriately selected depending on the viscosity of the adhesive and the target thickness.
- coating methods include reverse coaters, gravure coaters (direct, reverse and offset), bar reverse coaters, roll coaters, die coaters, bar coaters, rod coaters, and the like.
- a method such as a dipping method can be appropriately used for coating.
- the first film substrate and the second film substrate are bonded together through the transparent uncured adhesive layer.
- the first film base material and the second film base material can be bonded together using a roll laminator or the like.
- the transparent uncured adhesive layer used for laminating the first film substrate and the second film substrate is cured (step c) to produce a transparent conductive laminated film.
- the curing is appropriately determined depending on the type of adhesive, but when an active energy ray-curable adhesive is used, the cured adhesive layer is irradiated with active energy rays (electron beams, ultraviolet rays, etc.). Form.
- the irradiation direction of the active energy ray (electron beam, ultraviolet ray, etc.) can be irradiated from any appropriate direction, but irradiation from the second film base material increases the transmittance of the active energy ray. preferable.
- the oligomer prevention layer or the easy adhesion is applied to the surfaces of the first and second film bases to which the curable adhesive is applied.
- a layer can be provided.
- the material for forming the oligomer prevention layer or the easy adhesion layer an appropriate material capable of forming a transparent film is used, and an inorganic material, an organic material, or a composite material thereof may be used.
- the film thickness is preferably 0.01 to 20 ⁇ m.
- the oligomer prevention layer or the easy adhesion layer are often used to form the oligomer prevention layer or the easy adhesion layer, but a vacuum deposition method, a sputtering method, an ion plating method, etc. A technique such as spray pyrolysis, chemical plating, or electroplating may be used.
- a resin component such as polyvinyl alcohol resin, acrylic resin, urethane resin, melamine resin, UV curable resin, epoxy resin or a mixture of these inorganic particles such as alumina, silica, mica is used. May be.
- the base material component may have a function of a prevention layer by coextrusion of two or more layers of the polymer substrate.
- a metal made of cobalt or tin or an alloy thereof, or a metal oxide made of indium oxide, tin oxide, titanium oxide, cadmium oxide or a mixture thereof, or another metal compound made of steel iodide etc. can be used. .
- the polyvinyl alcohol-based resin is excellent in the oligomer prevention function and is particularly suitable for the use of the present invention.
- the polyvinyl alcohol-based resin is mainly composed of polyvinyl alcohol, and usually the content of polyvinyl alcohol is preferably in the range of 30 to 100% by weight. When the content of polyvinyl alcohol is 30% by weight or more, the effect of preventing oligomer precipitation is good.
- the resin that can be mixed with polyvinyl alcohol include addition of water-based resins such as polyester and polyurethane in order to impart easy adhesion.
- the degree of polymerization of polyvinyl alcohol is not particularly limited, but usually 300 to 4000 is suitable for use.
- the degree of saponification of polyvinyl alcohol is not particularly limited, but usually 70 mol% or more and 99.9 mol% or more are suitable.
- a crosslinking agent can be used in combination with the polyvinyl alcohol resin.
- Specific examples of the crosslinking agent include methylolated or alkylolized urea-based, melamine-based, guanamine-based, acrylamide-based, polyamide-based compounds, epoxy compounds, aziridine compounds, blocked isocyanates, silane coupling agents, titanium cups. Examples thereof include a ring agent and a zirco-aluminate coupling agent.
- crosslinking components may be bonded in advance to the binder polymer.
- inorganic particles may be contained for the purpose of improving adhesion and slipperiness, and specific examples include silica, alumina, kaolin, calcium carbonate, titanium oxide, barium salt and the like.
- an antifoaming agent, a coating property improving agent, a thickener, an organic lubricant, organic polymer particles, an antioxidant, an ultraviolet absorber, a foaming agent, a dye, and the like may be contained as necessary.
- the transparent conductive layer of the transparent conductive laminated film obtained as described above can be subjected to a heat treatment crystallization step (step d).
- the laminated film in the transparent conductive laminated film of the present invention is formed by laminating a plurality of transparent film substrates having a first film substrate and a second film substrate by the transparent cured adhesive layer having the predetermined storage elastic modulus. Therefore, even when the heat treatment is performed, the swell can be suppressed small.
- the heating temperature for crystallization is usually about 60 to 200 ° C., preferably 100 to 150 ° C.
- the heat treatment time is 5 to 250 minutes.
- the film bases such as the first and second film bases are preferably subjected to the heat treatment, and thus have a heat resistance of 100 ° C. or higher, more preferably 140 ° C. or higher.
- the crystallization step d is preferably performed before the patterning step e. Further, when etching the undercoat layer, it is preferable to perform the crystallization step d after the etching of the undercoat layer.
- the transparent conductive layer of the transparent conductive laminated film obtained as described above can be patterned (step e).
- patterning can be performed by etching the transparent conductive layer.
- the transparent conductive layer is covered with a mask for forming a pattern, and the transparent conductive layer is etched with an etching solution. After the etching, the film is dried by heating.
- the laminated film in the transparent conductive laminated film of the present invention has the first film substrate and the first film by the transparent cured adhesive layer having the predetermined storage elastic modulus. Since a plurality of transparent film base materials having two film base materials are laminated, undulation can be suppressed even when heat drying is performed.
- the above-exemplified compounds are preferably used, so that an acid is preferably used as the etching solution.
- the acid include inorganic acids such as hydrogen chloride, hydrogen bromide, sulfuric acid, nitric acid and phosphoric acid, organic acids such as acetic acid, and mixtures thereof, and aqueous solutions thereof.
- the transparent conductive layer alone can be etched and patterned, and after the transparent conductive layer is etched and patterned with acid, at least from the film substrate.
- the separated undercoat layer can be etched and patterned in the same manner as the transparent conductive layer.
- the transparent conductive layer other than the first undercoat layer from the film substrate can be etched and patterned in the same manner as the transparent conductive layer.
- the undercoat layer is covered with a mask for forming a pattern similar to that obtained when the transparent conductive layer is etched, and the undercoat layer is etched with an etching solution.
- an inorganic material such as SiO 2 is preferably used for the undercoat layer above the second layer, and therefore alkali is preferably used as the etching solution.
- the alkali include aqueous solutions of sodium hydroxide, potassium hydroxide, ammonia, tetramethylammonium hydroxide, and mixtures thereof.
- the first transparent conductive layer is preferably formed of an organic material that is not etched by acid or alkali.
- the transparent conductive laminated film of the present invention can be used for an electrode substrate of an input device of a capacitive touch panel, for example.
- the capacitive touch panel can adopt a multi-touch method, and the transparent conductive laminated film of the present invention can be used as a part of the electrode substrate.
- an ultraviolet ray (gallium encapsulated metal halide lamp) Irradiation device Fusion UV Systems, Inc.
- Light HAMMER10 bulb V bulb Peak illuminance: 1600 mW / cm 2 , integrated irradiation amount 1000 / mJ / cm 2 (wavelength 380 to 440 nm) )It was used.
- the illuminance of ultraviolet rays was measured using a Sola-Check system manufactured by Solatell.
- ⁇ Thickness of each layer> The film thickness of the film base material and the adhesive layer was measured using a film thickness meter (Digital Dial Gauge DG-205 manufactured by Peacock). In addition, in the case of a layer for which it is difficult to directly measure the thickness, the total thickness of the base material provided with each layer was measured, and the thickness of each layer was calculated by subtracting the thickness of the base material.
- a film thickness meter Digital Dial Gauge DG-205 manufactured by Peacock
- Radical polymerizable compound having active methylene group (F) AAEM (2-acetoacetoxyethyl methacrylate), SP value 20.23 (KJ / M 3 ) 1/2 , homopolymer Tg 9 ° C., manufactured by Nippon Synthetic Chemical Co., Ltd.
- Radical polymerization initiator with hydrogen abstraction action G) KAYACURE DETX-S (DETX-S) (diethylthioxanthone), manufactured by Nippon Kayaku Co., Ltd.
- Photopolymerization initiator (compound represented by general formula (2))) IRGACURE907 (IRG907) (2-methyl-1- (4-methylthiophenyl) -2-morpholinopropan-1-one), manufactured by BASF (10) Photoacid generator (H) CPI-100P (Propylene carbonate solution containing 50% active ingredient based on triarylsulfonium hexafluorophosphate), San Apro (11) Compound containing either alkoxy group or epoxy group (I) Denacol EX-611 (sorbitol polyglycidyl ether), Nicalesin S-260 (methylolated melamine) manufactured by Nagase ChemteX Corporation, KBM-5103 (3-acryloxypropyltrimethoxysilane) manufactured by Nippon Carbide Industries, Shin-Etsu Chemical Co., Ltd.
- Silane coupling agent having an amino group J) KBM-603 ( ⁇ - (2-aminoethyl) aminopropyltrimethoxysilane), Shin-Etsu Chemical Co., Ltd. KBM-602 ( ⁇ - (2-aminoethyl) aminopropylmethyldimethoxysilane), Shin-Etsu Chemical Co., Ltd. KBE- 9103 3-Triethoxysilyl-N- (1,3-dimethyl-butylidene) propylamine, manufactured by Shin-Etsu Chemical Co., Ltd.
- Example 1 Formation of first transparent conductive layer
- a sputtering apparatus equipped with a sintered compact target of indium tin oxide of 97% by weight of indium oxide and 3% by weight of tin oxide on one side of a 25- ⁇ m-thick polyene terephthalate film (first film substrate)
- ITO indium tin oxide
- irradiation device Fusion UV Systems, Inc.
- Light HAMMER10 manufactured by Inc. Valve: V bulb Peak illuminance: 1600 mW / cm 2 , integrated irradiation amount 1000 / mJ / cm 2 (wavelength 380 to 440 nm)
- irradiation amount 1000 / mJ / cm 2 (wavelength 380 to 440 nm)
- Example 2-16 Comparative Examples 1-2
- the thickness of the first film base material, the second film base material, the blending ratio of the active energy ray-curable adhesive composition, and the thickness of the adhesive layer were changed as shown in Tables 2 and 3.
- the second film base material having the second transparent conductive layer having a thickness of 22 nm was used in the same manner as the first film base material.
- the transparent conductive laminated film the second film substrate was bonded to the uncured adhesive layer on the opposite side on which the second transparent conductive layer was formed.
- ⁇ Storage modulus The storage elastic modulus was measured using TA Instruments dynamic viscoelasticity measuring device RSAIII under the following measurement conditions. Sample size: width 10mm, length 30mm, Clamp distance 20mm, Measurement mode: Tensile, Frequency: 1 Hz, Rate of temperature increase: 5 ° C./min Dynamic viscoelasticity was measured, and the storage elastic modulus was measured at 140 ° C.
- the transparent conductive laminated film was cut into a size of 200 mm parallel to the stretching direction of the first film substrate and 20 mm in the orthogonal direction. Next, a cut was made with a cutter knife between the first film substrate and the second film substrate of the cut transparent conductive film. Using Tensilon, the first film and the second film were peeled T-shaped at a peeling speed of 300 mm / min, and the peel strength was measured. Moreover, the infrared absorption spectrum of the peeling surface after peeling was measured by ATR method, and the peeling interface was evaluated based on the following reference
- A Cohesive fracture of film
- B Interfacial peeling between film / adhesive layer
- A means that the adhesive force is very excellent because the adhesive force is greater than the cohesive force of the film.
- B means that the adhesive force at the interface of the film / adhesive layer is insufficient (adhesive force is inferior).
- the adhesive strength in the case of A is ⁇
- the adhesive strength in the case of A ⁇ B (“film cohesive failure” and “interfacial peeling between film / adhesive layer” simultaneously) is ⁇
- the adhesive force in the case of only B is set as x.
- ⁇ Swell> The transparent conductive laminated film was heat-treated at 140 ° C. for 90 minutes to crystallize the transparent conductive layer (indium tin oxide layer). Thereafter, a desired pattern photoresist was formed on the surface of the first transparent conductive layer (first film substrate side). Next, the first transparent conductor layer was immersed in a 10% hydrochloric acid aqueous solution at 50 ° C. for 10 minutes to remove the unnecessary first transparent conductor layer. Subsequently, it was dried at 140 ° C. for 30 minutes to form a striped transparent electrode pattern (etching step). In the obtained transparent conductive laminated film, the swell (the height difference: ⁇ m) between the portion with and without the transparent electrode pattern was evaluated. The waviness (height difference: ⁇ m) was measured using an optical profilometer (Optical Profilometer NT3000 manufactured by Veeco Instruments).
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Abstract
Description
前記第1フィルム基材の、前記透明硬化接着剤層とは反対の面に積層された第1透明導電層とを有することを特徴とする透明導電性積層フィルム、に関する。
前記ラジカル重合性化合物(A)は、SP値が29.0(kJ/m3)1/2以上32.0以下(kJ/m3)1/2であり、
前記ラジカル重合性化合物(B)は、SP値が18.0(kJ/m3)1/2以上21.0(kJ/m3)1/2未満であり、
前記ラジカル重合性化合物(C)は、SP値が21.0(kJ/m3)1/2以上23.0(kJ/m3)1/2以下であり、
組成物全量を100重量%としたとき、前記ラジカル重合性化合物(B)を25~80重量%含有することが好ましい。
第1フィルム基材の一方の面に第1透明導電層が設けられた透明導電性フィルムを準備する工程aと、
前記透明導電性フィルムにおける、前記第1透明導電層を有しない前記第1フィルム基材の他方の面と、第2フィルム基材を、硬化によって、140℃における貯蔵弾性率が1×107Pa以上である透明硬化接着剤層を形成することができる、透明未硬化接着剤層により貼り合わせる工程b、および、
前記透明未硬化接着剤層を硬化させる工程cを有することを特徴とする透明導電性積層フィルムの製造方法、に関する。
本発明において、ラジカル重合性化合物などの溶解度パラメーター(SP値)は、Fedorsの算出法[「ポリマー・エンジニアリング・アンド・サイエンス(Polymer Eng.& Sci.)」,第14巻,第2号(1974),第148~154ページ参照]すなわち、
(ただし、L+は、任意のオニウムカチオンを表す。また、X-は、PF6 -、SbF6 -、AsF6 -、SbCl6 -、BiCl5 -、SnCl6 -、ClO4 -、ジチオカルバメートアニオン、SCN-よりからなる群より選択されるカウンターアニオンを表す。)
(上記一般式(4)-(12)中、ただし、R1、R2およびR3は、それぞれ独立に、水素原子、置換もしくは未置換のアルキル基、置換もしくは未置換のアルケニル基、置換もしくは未置換のアリール基、置換もしくは未置換の複素環基、置換もしくは未置換のアルコキシル基、置換もしくは未置換のアリールオキシ基、置換もしくは未置換の複素環オキシ基、置換もしくは未置換のアシル基、置換もしくは未置換のカルボニルオキシ基、置換もしくは未置換のオキシカルボニル基、またはハロゲン原子より選ばれる基を表す。R4は、R1、R2およびR3に記載した基と同様の基を表す。R5は、置換もしくは未置換のアルキル基、置換もしくは未置換のアルキルチオ基を表す。R6およびR7は、それぞれ独立に、置換もしくは未置換のアルキル基、置換もしくは未置換のアルコキシル基を表す。Rは、ハロゲン原子、水酸基、カルボキシル基、メルカプト基、シアノ基、ニトロ基、置換もしくは未置換のカルバモイル基、置換もしくは未置換のアルキル基、置換もしくは未置換のアルケニル基、置換もしくは未置換のアリール基、置換もしくは未置換の複素環基、置換もしくは未置換のアルコキシル基、置換もしくは未置換のアリールオキシ基、置換もしくは未置換の複素環オキシ基、置換もしくは未置換のアルキルチオ基、置換もしくは未置換のアリールチオ基、置換もしくは未置換の複素環チオ基、置換もしくは未置換のアシル基、置換もしくは未置換のカルボニルオキシ基、置換もしくは未置換のオキシカルボニル基のいずれかを表す。Ar4、Ar5は、置換もしくは未置換のアリール基、置換もしくは未置換の複素環基のいずれかを表す。Xは、酸素もしくは硫黄原子を表す。iは0~5の整数を表す。jは0~4の整数を表す。kは0~3の整数を表す。また、隣接したR同士、Ar4とAr5、R2とR3、R2とR4、R3とR4、R1とR2、R1とR3、R1とR4、R1とR、もしくはR1とR5は、相互に結合した環状構造であってもよい。)
ジメチルフェニルスルホニウム、ジメチル(o-フルオロフェニル)スルホニウム、ジメチル(m-クロロフェニル)スルホニウム、ジメチル(p-ブロモフェニル)スルホニウム、ジメチル(p-シアノフェニル)スルホニウム、ジメチル(m-ニトロフェニル)スルホニウム、ジメチル(2,4,6-トリブロモフェニル)スルホニウム、ジメチル(ペンタフルオロフェニル)スルホニウム、ジメチル(p-(トリフルオロメチル)フェニル)スルホニウム、ジメチル(p-ヒドロキシフェニル)スルホニウム、ジメチル(p-メルカプトフェニル)スルホニウム、ジメチル(p-メチルスルフィニルフェニル)スルホニウム、ジメチル(p-メチルスルホニルフェニル)スルホニウム、ジメチル(o-アセチルフェニル)スルホニウム、ジメチル(o-ベンゾイルフェニル)スルホニウム、ジメチル(p-メチルフェニル)スルホニウム、ジメチル(p-イソプロピルフェニル)スルホニウム、ジメチル(p-オクタデシルフェニル)スルホニウム、ジメチル(p-シクロヘキシルフェニル)スルホニウム、ジメチル(p-メトキシフェニル)スルホニウム、ジメチル(o-メトキシカルボニルフェニル)スルホニウム、ジメチル(p-フェニルスルファニルフェニル)スルホニウム、(7-メトキシ-2-オキソ-2H-クロメン-4-イル)ジメチルスルホニウム、(4-メトキシナフタレン-1-イル)ジメチルスルホニウム、ジメチル(p-イソプロポキシカルボニルフェニル)スルホニウム、ジメチル(2-ナフチル)スルホニウム、ジメチル(9-アンスリル)スルホニウム、ジエチルフェニルスルホニウム、メチルエチルフェニルスルホニウム、メチルジフェニルスルホニウム、トリフェニルスルホニウム、ジイソプロピルフェニルスルホニウム、ジフェニル(4-フェニルスルファニル-フェニル)-スルホニウム、4,4’-ビス(ジフェニルスルホニウム)ジフェニルスルフィド、4,4’-ビス[ジ[(4-(2-ヒドロキシ-エトキシ)-フェニル)]スルホニウム]]ジフェニルスルフィド、4,4’-ビス(ジフェニルスルホニウム)ビフェニレン、ジフェニル(o-フルオロフェニル)スルホニウム、ジフェニル(m-クロロフェニル)スルホニウム、ジフェニル(p-ブロモフェニル)スルホニウム、ジフェニル(p-シアノフェニル)スルホニウム、ジフェニル(m-ニトロフェニル)スルホニウム、ジフェニル(2,4,6-トリブロモフェニル)スルホニウム、ジフェニル(ペンタフルオロフェニル)スルホニウム、ジフェニル(p-(トリフルオロメチル)フェニル)スルホニウム、ジフェニル(p-ヒドロキシフェニル)スルホニウム、ジフェニル(p-メルカプトフェニル)スルホニウム、ジフェニル(p-メチルスルフィニルフェニル)スルホニウム、ジフェニル(p-メチルスルホニルフェニル)スルホニウム、ジフェニル(o-アセチルフェニル)スルホニウム、ジフェニル(o-ベンゾイルフェニル)スルホニウム、ジフェニル(p-メチルフェニル)スルホニウム、ジフェニル(p-イソプロピルフェニル)スルホニウム、ジフェニル(p-オクタデシルフェニル)スルホニウム、ジフェニル(p-シクロヘキシルフェニル)スルホニウム、ジフェニル(p-メトキシフェニル)スルホニウム、ジフェニル(o-メトキシカルボニルフェニル)スルホニウム、ジフェニル(p-フェニルスルファニルフェニル)スルホニウム、(7-メトキシ-2-オキソ-2H-クロメン-4-イル)ジフェニルスルホニウム、(4-メトキシナフタレン-1-イル)ジフェニルスルホニウム、ジフェニル(p-イソプロポキシカルボニルフェニル)スルホニウム、ジフェニル(2-ナフチル)スルホニウム、ジフェニル(9-アンスリル)スルホニウム、エチルジフェニルスルホニウム、メチルエチル(o-トリル)スルホニウム、メチルジ(p-トリル)スルホニウム、トリ(p-トリル)スルホニウム、ジイソプロピル(4-フェニルスルファニルフェニル)スルホニウム、ジフェニル(2-チエニル)スルホニウム、ジフェニル(2-フリル)スルホニウム、ジフェニル(9-エチル-9Hカルバゾール-3-イル)スルホニウム等を挙げることができるが、これらに限定されるものではない。
ジメチルフェニルスルホキソニウム、ジメチル(o-フルオロフェニル)スルホキソニウム、ジメチル(m-クロロフェニル)スルホキソニウム、ジメチル(p-ブロモフェニル)スルホキソニウム、ジメチル(p-シアノフェニル)スルホキソニウム、ジメチル(m-ニトロフェニル)スルホキソニウム、ジメチル(2,4,6-トリブロモフェニル)スルホキソニウム、ジメチル(ペンタフルオロフェニル)スルホキソニウム、ジメチル(p-(トリフルオロメチル)フェニル)スルホキソニウム、ジメチル(p-ヒドロキシフェニル)スルホキソニウム、ジメチル(p-メルカプトフェニル)スルホキソニウム、ジメチル(p-メチルスルフィニルフェニル)スルホキソニウム、ジメチル(p-メチルスルホニルフェニル)スルホキソニウム、ジメチル(o-アセチルフェニル)スルホキソニウム、ジメチル(o-ベンゾイルフェニル)スルホキソニウム、ジメチル(p-メチルフェニル)スルホキソニウム、ジメチル(p-イソプロピルフェニル)スルホキソニウム、ジメチル(p-オクタデシルフェニル)スルホキソニウム、ジメチル(p-シクロヘキシルフェニル)スルホキソニウム、ジメチル(p-メトキシフェニル)スルホキソニウム、ジメチル(o-メトキシカルボニルフェニル)スルホキソニウム、ジメチル(p-フェニルスルファニルフェニル)スルホキソニウム、(7-メトキシ-2-オキソ-2H-クロメン-4-イル)ジメチルスルホキソニウム、(4-メトキシナフタレン-1-イル)ジメチルスルホキソニウム、ジメチル(p-イソプロポキシカルボニルフェニル)スルホキソニウム、ジメチル(2-ナフチル)スルホキソニウム、ジメチル(9-アンスリル)スルホキソニウム、ジエチルフェニルスルホキソニウム、メチルエチルフェニルスルホキソニウム、メチルジフェニルスルホキソニウム、トリフェニルスルホキソニウム、ジイソプロピルフェニルスルホキソニウム、ジフェニル(4-フェニルスルファニル-フェニル)-スルホキソニウム、4,4’-ビス(ジフェニルスルホキソニウム)ジフェニルスルフィド、4,4’-ビス[ジ[(4-(2-ヒドロキシ-エトキシ)-フェニル)] スルホキソニウム]ジフェニルスルフィド、4,4’-ビス(ジフェニルスルホキソニウム)ビフェニレン、ジフェニル(o-フルオロフェニル)スルホキソニウム、ジフェニル(m-クロロフェニル)スルホキソニウム、ジフェニル(p-ブロモフェニル)スルホキソニウム、ジフェニル(p-シアノフェニル)スルホキソニウム、ジフェニル(m-ニトロフェニル)スルホキソニウム、ジフェニル(2,4,6-トリブロモフェニル)スルホキソニウム、ジフェニル(ペンタフルオロフェニル)スルホキソニウム、ジフェニル(p-(トリフルオロメチル)フェニル)スルホキソニウム、ジフェニル(p-ヒドロキシフェニル)スルホキソニウム、ジフェニル(p-メルカプトフェニル)スルホキソニウム、ジフェニル(p-メチルスルフィニルフェニル)スルホキソニウム、ジフェニル(p-メチルスルホニルフェニル)スルホキソニウム、ジフェニル(o-アセチルフェニル)スルホキソニウム、ジフェニル(o-ベンゾイルフェニル)スルホキソニウム、ジフェニル(p-メチルフェニル)スルホキソニウム、ジフェニル(p-イソプロピルフェニル)スルホキソニウム、ジフェニル(p-オクタデシルフェニル)スルホキソニウム、ジフェニル(p-シクロヘキシルフェニル)スルホキソニウム、ジフェニル(p-メトキシフェニル)スルホキソニウム、ジフェニル(o-メトキシカルボニルフェニル)スルホキソニウム、ジフェニル(p-フェニルスルファニルフェニル)スルホキソニウム、(7-メトキシ-2-オキソ-2H-クロメン-4-イル)ジフェニルスルホキソニウム、(4-メトキシナフタレン-1-イル)ジフェニルスルホキソニウム、ジフェニル(p-イソプロポキシカルボニルフェニル)スルホキソニウム、ジフェニル(2-ナフチル)スルホキソニウム、ジフェニル(9-アンスリル)スルホキソニウム、エチルジフェニルスルホキソニウム、メチルエチル(o-トリル) スルホキソニウム、メチルジ(p-トリル) スルホキソニウム、トリ(p-トリル) スルホキソニウム、ジイソプロピル(4-フェニルスルファニルフェニル) スルホキソニウム、ジフェニル(2-チエニル) スルホキソニウム、ジフェニル(2-フリル) スルホキソニウム、ジフェニル(9-エチル-9Hカルバゾール-3-イル) スルホキソニウム等を挙げることができるが、これらに限定されるものではない。
ホスホニウムカチオンの例:
トリメチルフェニルホスホニウム、トリエチルフェニルホスホニウム、テトラフェニルホスホニウム、トリフェニル(p-フルオロフェニル)ホスホニウム、トリフェニル(o-クロロフェニル)ホスホニウム、トリフェニル(m-ブロモフェニル)ホスホニウム、トリフェニル(p-シアノフェニル)ホスホニウム、トリフェニル(m-ニトロフェニル)ホスホニウム、トリフェニル(p-フェニルスルファニルフェニル)ホスホニウム、(7-メトキシ-2-オキソ-2H-クロメン-4-イル)トリフェニルホスホニウム、トリフェニル(o-ヒドロキシフェニル)ホスホニウム、トリフェニル(o-アセチルフェニル)ホスホニウム、トリフェニル(m-ベンゾイルフェニル)ホスホニウム、トリフェニル(p-メチルフェニル)ホスホニウム、トリフェニル(p-イソプロポキシフェニル)ホスホニウム、トリフェニル(o-メトキシカルボニルフェニル)ホスホニウム、トリフェニル(1-ナフチル)ホスホニウム、トリフェニル(9-アンスリル)ホスホニウム、トリフェニル(2-チエニル) ホスホニウム、トリフェニル(2-フリル) ホスホニウム、トリフェニル(9-エチル-9Hカルバゾール-3-イル) ホスホニウム等を挙げることができるが、これらに限定されるものではない。
ピリジニウムカチオンの例:
N-フェニルピリジニウム、N-(o-クロロフェニル)ピリジニウム、N-(m-クロロフェニル)ピリジニウム、N-(p-シアノフェニル)ピリジニウム、N-(o-ニトロフェニル)ピリジニウム、N-(p-アセチルフェニル)ピリジニウム、N-(p-イソプロピルフェニル)ピリジニウム、N-(p-オクタデシルオキシフェニル)ピリジニウム、N-(p-メトキシカルボニルフェニル)ピリジニウム、N-(9-アンスリル)ピリジニウム、2-クロロ-1-フェニルピリジニウム、2-シアノ-1-フェニルピリジニウム、2-メチル-1-フェニルピリジニウム、2-ビニル-1-フェニルピリジニウム、2-フェニル-1-フェニルピリジニウム、1,2-ジフェニルピリジニウム、2-メトキシ-1-フェニルピリジニウム、2-フェノキシ-1-フェニルピリジニウム、2-アセチル-1-(p-トリル)ピリジニウム、2-メトキシカルボニル-1-(p-トリル)ピリジニウム、3-フルオロ-1-ナフチルピリジニウム、4-メチル-1-(2-フリル)ピリジニウム、N-メチルピリジニウム、N-エチルピリジニウム等を挙げることができるが、これらに限定されるものではない。
キノリニウムカチオンの例:
N-メチルキノリニウム、N-エチルキノリニウム、N-フェニルキノリニウム、N-ナフチルキノリニウム、N-(o-クロロフェニル)キノリニウム、N-(m-クロロフェニル)キノリニウム、N-(p-シアノフェニル)キノリニウム、N-(o-ニトロフェニル)キノリニウム、N-(p-アセチルフェニル)キノリニウム、N-(p-イソプロピルフェニル)キノリニウム、N-(p-オクタデシルオキシフェニル)キノリニウム、N-(p-メトキシカルボニルフェニル)キノリニウム、N-(9-アンスリル)キノリニウム、2-クロロ-1-フェニルキノリニウム、2-シアノ-1-フェニルキノリニウム、2-メチル-1-フェニルキノリニウム、2-ビニル-1-フェニルキノリニウム、2-フェニル-1-フェニルキノリニウム、1,2-ジフェニルキノリニウム、2-メトキシ-1-フェニルキノリニウム、2-フェノキシ-1-フェニルキノリニウム、2-アセチル-1-フェニルキノリニウム、2-メトキシカルボニル-1-フェニルキノリニウム、3-フルオロ-1-フェニルキノリニウム、4-メチル-1-フェニルキノリニウム、2-メトキシ-1-(p-トリル)キノリニウム、2-フェノキシ-1-(2-フリル)キノリニウム、2-アセチル-1-(2-チエニル)キノリニウム、2-メトキシカルボニル-1-メチルキノリニウム、3-フルオロ-1-エチルキノリニウム、4-メチル-1-イソプロピルキノリニウム等を挙げることができるが、これらに限定されるものではない。
イソキノリニウムカチオンの例:
N-フェニルイソキノリニウム、N-メチルイソキノリニウム、N-エチルイソキノリニウム、N-(o-クロロフェニル)イソキノリニウム、N-(m-クロロフェニル)イソキノリニウム、N-(p-シアノフェニル)イソキノリニウム、N-(o-ニトロフェニル)イソキノリニウム、N-(p-アセチルフェニル)イソキノリニウム、N-(p-イソプロピルフェニル)イソキノリニウム、N-(p-オクタデシルオキシフェニル)イソキノリニウム、N-(p-メトキシカルボニルフェニル)イソキノリニウム、N-(9-アンスリル)イソキノリニウム、1,2-ジフェニルイソキノリニウム、N-(2-フリル)イソキノリニウム、N-(2-チエニル)イソキノリニウム、N-ナフチルイソキノリニウム等を挙げることができるが、これらに限定されるものではない。
ベンゾオキサゾリウムカチオンの例:
N-メチルベンゾオキサゾリウム、N-エチルベンゾオキサゾリウム、N-ナフチルベンゾオキサゾリウム、N-フェニルベンゾオキサゾリウム、N-(p-フルオロフェニル)ベンゾオキサゾリウム、N-(p-クロロフェニル)ベンゾオキサゾリウム、N-(p-シアノフェニル)ベンゾオキサゾリウム、N-(o-メトキシカルボニルフェニル)ベンゾオキサゾリウム、N-(2-フリル)ベンゾオキサゾリウム、N-(o-フルオロフェニル)ベンゾオキサゾリウム、N-(p-シアノフェニル)ベンゾオキサゾリウム、N-(m-ニトロフェニル)ベンゾオキサゾリウム、N-(p-イソプロポキシカルボニルフェニル)ベンゾオキサゾリウム、N-(2-チエニル)ベンゾオキサゾリウム、N-(m-カルボキシフェニル)ベンゾオキサゾリウム、2-メルカプト-3-フェニルベンゾオキサゾリウム、2-メチル-3-フェニルベンゾオキサゾリウム、2-メチルチオ-3-(4-フェニルスルファニルフェニル)ベンゾオキサゾリウム、6-ヒドロキシ-3-(p-トリル)ベンゾオキサゾリウム、7-メルカプト-3-フェニルベンゾオキサゾリウム、4,5-ジフルオロ-3-エチルベンゾオキサゾリウム等を挙げることができるが、これらに限定されるものではない。
N-メチルベンゾチアゾリウム、N-エチルベンゾチアゾリウム、N-フェニルベンゾチアゾリウム、N-(1-ナフチル)ベンゾチアゾリウム、N-(p-フルオロフェニル)ベンゾチアゾリウム、N-(p-クロロフェニル)ベンゾチアゾリウム、N-(p-シアノフェニル)ベンゾチアゾリウム、N-(o-メトキシカルボニルフェニル)ベンゾチアゾリウム、N-(p-トリル)ベンゾチアゾリウム、N-(o-フルオロフェニル)ベンゾチアゾリウム、N-(m-ニトロフェニル)ベンゾチアゾリウム、N-(p-イソプロポキシカルボニルフェニル)ベンゾチアゾリウム、N-(2-フリル)ベンゾチアゾリウム、N-(4-メチルチオフェニル)ベンゾチアゾリウム、N-(4-フェニルスルファニルフェニル)ベンゾチアゾリウム、N-(2-ナフチル)ベンゾチアゾリウム、N-(m-カルボキシフェニル)ベンゾチアゾリウム、2-メルカプト-3-フェニルベンゾチアゾリウム、2-メチル-3-フェニルベンゾチアゾリウム、2-メチルチオ-3-フェニルベンゾチアゾリウム、6-ヒドロキシ-3-フェニルベンゾチアゾリウム、7-メルカプト-3-フェニルベンゾチアゾリウム、4,5-ジフルオロ-3-フェニルベンゾチアゾリウム等を挙げることができるが、これらに限定されるものではない。
ジフリルヨードニウム、ジチエニルヨードニウム、ビス(4,5-ジメチル-2-フリル)ヨードニウム、ビス(5-クロロ-2-チエニル)ヨードニウム、ビス(5-シアノ-2-フリル)ヨードニウム、ビス(5-ニトロ-2-チエニル)ヨードニウム、ビス(5-アセチル-2-フリル)ヨードニウム、ビス(5-カルボキシ-2-チエニル)ヨードニウム、ビス(5-メトキシカルボニル-2-フリル)ヨードニウム、ビス(5-フェニル-2-フリル)ヨードニウム、ビス(5-(p-メトキシフェニル)-2-チエニル)ヨードニウム、ビス(5-ビニル-2-フリル)ヨードニウム、ビス(5-エチニル-2-チエニル)ヨードニウム、ビス(5-シクロヘキシル-2-フリル)ヨードニウム、ビス(5-ヒドロキシ-2-チエニル)ヨードニウム、ビス(5-フェノキシ-2-フリル)ヨードニウム、ビス(5-メルカプト-2-チエニル)ヨードニウム、ビス(5-ブチルチオ-2-チエニル)ヨードニウム、ビス(5-フェニルチオ-2-チエニル)ヨードニウム等を挙げることができるが、これらに限定されるものではない。
ジフェニルヨードニウム、ビス(p-トリル)ヨードニウム、ビス(p-オクチルフェニル)ヨードニウム、ビス(p-オクタデシルフェニル)ヨードニウム、ビス(p-オクチルオキシフェニル)ヨードニウム、ビス(p-オクタデシルオキシフェニル)ヨードニウム、フェニル(p-オクタデシルオキシフェニル)ヨードニウム、4-イソプロピル-4’-メチルジフェニルヨードニウム、(4-イソブチルフェニル)-p-トリルヨードニウム、ビス(1-ナフチル)ヨードニウム、ビス(4-フェニルスルファニルフェニル)ヨードニウム、フェニル(6-ベンゾイル-9-エチル-9H-カルバゾール-3-イル)ヨードニウム、(7-メトキシ-2-オキソ-2H-クロメン-3-イル)-4’-イソプロピルフェニルヨードニウム等を挙げることができるが、これらに限定されるものではない。
分子内に1個以上のエポキシ基を有する化合物又は分子内に2個以上のエポキシ基を有する高分子(エポキシ樹脂)を用いる場合は、エポキシ基との反応性を有する官能基を分子内に二つ以上有する化合物を併用してもよい。ここでエポキシ基との反応性を有する官能基とは、例えば、カルボキシル基、フェノール性水酸基、メルカプト基、1級又は2級の芳香族アミノ基等が挙げられる。これらの官能基は、3次元硬化性を考慮して、一分子中に2つ以上有することが特に好ましい。
分子内にアルコキシル基を有する化合物としては、分子内に1個以上のアルコキシル基を有するものであれば特に制限なく、公知のものを使用できる。このような化合物としては、メラミン化合物、アミノ樹脂、シランカップリング剤などが代表として挙げられる。なお、接着剤層のガラス転移温度Tgを計算する際には、アルコキシル基を有する化合物及び高分子(H)を計算には入れないこととする。
(式中、R1およびR2は-H、-CH2CH3、-iPrまたはClを示し、R1およびR2は同一または異なっても良い)を単独で使用するか、あるいは一般式(1)で表される化合物と後述する380nm以上の光に対して高感度な光重合開始剤とを併用することが好ましい。一般式(1)で表される化合物を使用した場合、380nm以上の光に対して高感度な光重合開始剤を単独で使用した場合に比べて接着性に優れる。一般式(1)で表される化合物の中でも、R1およびR2が-CH2CH3であるジエチルチオキサントンが特に好ましい。組成物中の一般式(1)で表される化合物の組成比率は、組成物全量を100重量%としたとき、0.1~5.0重量%であることが好ましく、0.5~4.0重量%であることがより好ましく、0.9~3.0重量%であることがさらに好ましい。
(式中、R3、R4およびR5は-H、-CH3、-CH2CH3、-iPrまたはClを示し、R3、R4およびR5は同一または異なっても良い)を使用することが好ましい。一般式(2)で表される化合物としては、市販品でもある2-メチル-1-(4-メチルチオフェニル)-2-モルフォリノプロパン-1-オン(商品名:IRGACURE907 メーカー:BASF)が好適に使用可能である。その他、2-ベンジル-2-ジメチルアミノ-1-(4-モルフォリノフェニル)-ブタノン-1(商品名:IRGACURE369 メーカー:BASF)、2-(ジメチルアミノ)-2-[(4-メチルフェニル)メチル]-1-[4-(4-モルホリニル)フェニル]-1-ブタノン(商品名:IRGACURE379 メーカー:BASF)が感度が高いため好ましい。
活性エネルギー線として、紫外線(ガリウム封入メタルハライドランプ) 照射装置:Fusion UV Systems,Inc社製Light HAMMER10 バルブ:Vバルブ ピーク照度:1600mW/cm2、積算照射量1000/mJ/cm2(波長380~440nm)を使用した。なお、紫外線の照度は、Solatell社製Sola-Checkシステムを使用して測定した。
フィルム基材、接着剤層の膜厚は、膜厚計(Peacock社製のデジタルダイアルゲージDG‐205)を用いて測定した。なお、直接厚みを計測することが困難な層の場合は、各層を設けた基材の総厚みを測定し、基材の厚みを差し引くことで各層の膜厚を算出した。
表2に記載の配合表に従い、各成分を混合して50℃で1時間撹拌し、活性エネルギー線硬化型接着剤組成物を得た。表中の数値は組成物全量を100重量%としたときの重量%を示す。使用した各成分は以下のとおりである。
(2)ラジカル重合性化合物(B):ARONIX M-220(トリプロピレングリコールジアクリレート)、SP値19.0、東亞合成社製;
ラジカル重合性化合物(B):ライトアクリレートDCP-A(ジメチロール-トリシクロデカンジアクリレート)、SP値20.3、共栄社化学社製;
(3)ラジカル重合性化合物(C):ACMO(アクリロイルモルホリン)、SP値22.9、興人社製;
ラジカル重合性化合物(C):IB‐XA(イソボニルアクリレート)、SP値22.4、共栄社化学社製;
(4)(メタ)アクリルモノマーを重合してなるアクリル系オリゴマー(D):ARUFON UP-1190、東亞合成社製;
(5)ラジカル重合性化合物(E):2HEA(2-ヒドロキシエチルアクリレート)、SP値25.5、三菱レイヨン社製;
(6)光重合開始剤:KAYACURE DETX-S(ジエチルチオキサントン),日本化薬社製、IRGACURE907(2-メチル-1-(4-メチルチオフェニル)-2-モルフォリノプロパン-1-オン),BASF社製。
(7)活性メチレン基を有するラジカル重合性化合物(F)
AAEM(2-アセトアセトキシエチルメタクリレート)、SP値 20.23(KJ/M3)1/2、ホモポリマーのTg 9℃、日本合成化学社製
(8)水素引き抜き作用のあるラジカル重合開始剤(G)
KAYACURE DETX-S(DETX-S)(ジエチルチオキサントン)、日本化薬社製
(9)光重合開始剤(一般式(2)で表される化合物))
IRGACURE907(IRG907)(2-メチル-1-(4-メチルチオフェニル)-2-モルフォリノプロパン-1-オン)、BASF社製
(10)光酸発生剤(H)
CPI-100P(トリアリールスルホニウムヘキサフルオロホスフェートを主成分とする有効成分50%のプロピレンカーボネート溶液)、サンアプロ社製
(11)アルコキシ基、エポキシ基いずれかを含む化合物(I)
デナコールEX-611(ソルビトールポリグリシジルエーテル)、ナガセケムテックス社製
ニカレジンS-260(メチロール化メラミン)、 日本カーバイト工業社製
KBM-5103(3-アクリロキシプロピルトリメトキシシラン)、信越化学工業社製
(12)アミノ基を有するシランカップリング剤(J)
KBM-603(γ-(2-アミノエチル)アミノプロピルトリメトキシシラン)、信越化学工業社製
KBM-602(γ-(2-アミノエチル)アミノプロピルメチルジメトキシシラン)、信越化学工業社製
KBE-9103 3-トリエトキシシリル-N-(1,3-ジメチル-ブチリデン)プロピルアミン、信越化学工業社製
(第1透明導電層の形成)
厚さは25μmのポリエンレンテレフタレートフィルム(第1フィルム基材)の片面に、酸化インジウム97重量%、酸化スズ3重量%のインジウムスズ酸化物の焼結体ターゲットを備えたスパッタ装置を用いて、厚さは22nmのインジウムスズ酸化物(ITO)層を形成した。
た。
次に、ポリエチレンテレフタレートフィルム(第1フィルム基材)の、インジウムスズ酸化物層の反対側の面に、MCDコーター(富士機械社製,セル形状:ハニカム,グラビアロール線数:300本/inch,回転速度150%/対ライン速)を用いて、表2に示す配合で調製した活性エネルギー線硬化型接着剤組成物を塗布して、厚み1μmの透明未硬化接着剤層を形成した。次いで、当該未硬化接着剤層に、厚さ100μmのポリエチレンテレフタレートフィルム(第2フィルム基材)を貼り合わせた。その後、第2フィルム基材の側から、照射装置:Fusion UV Systems,Inc社製Light HAMMER10 バルブ:Vバルブ ピーク照度:1600mW/cm2、積算照射量1000/mJ/cm2(波長380~440nm)を照射して、前記接着剤層を硬化させて、透明導電性積層フィルムを得た。
実施例1において、第1フィルム基材、第2フィルム基材の厚み、活性エネルギー線硬化型接着剤組成物の配合割合、接着剤層の厚みを表2,3に示すように変えたこと以外は実施例1と同様にして、透明導電性積層フィルムを作製した。なお、実施例9では、第2フィルム基材についても、第1フィルム基材と同様にして、厚さ22nmの第2透明導電層を形成したものを用いた。透明導電性積層フィルムの作製にあたっては、第2フィルム基材は、第2透明導電層を形成した反対側を、未硬化接着剤層に貼り合わせた。
実施例及び比較例で得られた透明導電性積層フィルムについて、下記評価を行なった。結果を表2,3に示す。表2,3には、フィルム基材、接着剤層の厚みを併せて示す。
貯蔵弾性率は、TAインスツルメンツ製動的粘弾性測定装置RSAIIIを用い以下の測定条件で測定した。
サンプルサイズ:幅10mm、長さ30mm、
クランプ距離20mm、
測定モード:引っ張り、周波数:1Hz、昇温速度:5℃/分
動的粘弾性の測定を行い、貯蔵弾性率の140℃での測定値とした。
透明導電性積層フィルムにおける第1フィルム基材の延伸方向と平行に200mm、直行方向に20mmの大きさに切り出した。次いで、切り出した透明導電性フィルムの第1フィルム基材と第2フィルム基材の間にカッターナイフで切り込みを入れた。
テンシロンにより、第1フィルムと第2フィルムとを剥離速度300mm/minでT字剥離し、その剥離強度を測定した。また、剥離後の剥離面の赤外吸収スペクトルをATR法によって測定し、剥離界面を下記の基準に基づき評価した。
A:フィルムの凝集破壊
B:フィルム/接着剤層間の界面剥離
上記基準において、Aは、接着力がフィルムの凝集力以上であるため、接着力が非常に優れることを意味する。一方、Bは、フィルム/接着剤層の界面の接着力が不足している(接着力が劣る)ことを意味する。これらを勘案して、Aの場合の接着力を○、A・B(「フィルムの凝集破壊」と「フィルム/接着剤層間の界面剥離」とが同時に発生)である場合の接着力を△、Bのみの場合の接着力を×とする。
透明導電性積層フィルムを140℃で90分間加熱処理して、透明導電層(インジウムスズ酸化物層)を結晶化させた。その後、透明導電体層を50℃の10%塩酸水溶液に10分間浸漬して透明導電体層を除去した際の透明導電性積層フィルム端部のハガレ、浮きを目視で評価した。
○;ハガレ、浮きなし
△:1mm未満のハガレ、浮きが発生
×:1mm以上のハガレ、浮きが発生
透明導電性積層フィルムを140℃で90分間加熱処理して、透明導電層(インジウムスズ酸化物層)を結晶化させた。その後、第1透明導電層(第1フィルム基材側)の表面に所望のパターンフォトレジストを形成した。次いで、第1透明導電体層を50℃の10%塩酸水溶液に10分間浸漬して不要な第1透明導電体層を除去した。次いで、140℃で30分間乾燥させて、ストライプ状の透明電極パターンを形成した(エッチング工程)。得られた透明導電性積層フィルムにおける透明電極パターンのある部分とない部分のうねり(高低差:μm)を評価した。うねりは(高低差:μm)は光学式プロファイロメーター(Veeco Instruments社製のOptical Profilometer NT3000)を用いて測定した。
10cm×10cmの大きさに切り出し、四隅に印をつけた透明導電性積層フィルムを、140℃で90分間加熱処理して透明導電層(インジウムスズ酸化物層)を結晶化させた。その後、透明導電層(第1透明導電層,但し実施例9では両側の第1および第2透明導電層)の全面をポリイミドテープで覆ったサンプル1とポリイミドテープで全く覆わないサンプル2を作成した。
次に、サンプル1とサンプル2を10%塩酸に浸漬した。サンプル2からは透明導電層を除去した(これが、積層フィルムA´に対応)。サンプル1では、浸漬後に、ポリイミドテープを剥離した(これが、透明導電性積層フィルムAに対応)。その時のサンプル1とサンプル2の正確な大きさを測定した(処理前)。次いで、サンプル1とサンプル2を、140℃で30分間乾燥させてから、再度、サンプル1とサンプル2の大きさを測定した(処理後)。
収縮率は、前記処理前と処理後の大きさから、下記式により求めた。
収縮率(%)={(処理前の大きさ-処理後の大きさ)/(処理前の大きさ)}×100
収縮率差は、サンプル1の収縮率-サンプル2の収縮率、である。
各サンプル1、2の大きさの測定は画像測定機クイックビジョン(ミツトヨ社製)を用いて測定した。
12 第2フィルム基材
13 第3フィルム基材
21 第1透明導電層
22 第2透明導電層
3 透明硬化接着剤層
A 透明導電性積層フィルム
A´ 積層フィルム
Claims (30)
- 透明な第1フィルム基材と透明な第2フィルム基材を有する複数の透明なフィルム基材が、140℃における貯蔵弾性率が1×107Pa以上である透明硬化接着剤層を介して積層されている積層フィルムと、
前記第1フィルム基材の、前記透明硬化接着剤層とは反対の面に積層された第1透明導電層とを有することを特徴とする透明導電性積層フィルム。 - 前記透明導電性積層フィルムと、前記積層フィルムとは、140℃で30分間加熱処理した際の収縮率の差が0.3%以下であることを特徴とする請求項1記載の透明導電性積層フィルム。
- 前記透明硬化接着剤層が、硬化性成分としてのラジカル重合性化合物(A)、(B)および(C)を含有する活性エネルギー線硬化型接着剤組成物から形成されていて、
前記ラジカル重合性化合物(A)は、SP値が29.0(kJ/m3)1/2以上32.0以下(kJ/m3)1/2であり、
前記ラジカル重合性化合物(B)は、SP値が18.0(kJ/m3)1/2以上21.0(kJ/m3)1/2未満であり、
前記ラジカル重合性化合物(C)は、SP値が21.0(kJ/m3)1/2以上23.0(kJ/m3)1/2以下であり、
組成物全量を100重量%としたとき、前記ラジカル重合性化合物(B)を25~80重量%含有することを特徴とする請求項1または2記載の透明導電性積層フィルム。 - 前記活性エネルギー線硬化型接着剤組成物は、さらに、(メタ)アクリルモノマーを重合してなるアクリル系オリゴマー(D)を含有することを特徴とする請求項3記載の透明導電性積層フィルム。
- 前記活性エネルギー線硬化型接着剤組成物は、組成物全量を100重量%としたとき、(メタ)アクリルモノマーを重合してなるアクリル系オリゴマー(D)を20重量%以下の範囲で含有することを特徴とする請求項4記載の透明導電性積層フィルム。
- 前記活性エネルギー線硬化型接着剤組成物は、組成物全量を100重量%としたとき、前記ラジカル重合性化合物(A)を3~40重量%、前記ラジカル重合性化合物(C)を5~55重量%含有することを特徴とする請求項3~5のいずれかに記載の透明導電性積層フィルム。
- 前記活性エネルギー線硬化型接着剤組成物は、前記ラジカル重合性化合物の全量を100重量部としたとき、前記ラジカル重合性化合物(A)、(B)および(C)を合計で85重量部以上含有し、さらにSP値が23.0(kJ/m3)1/2を超えて29.0(kJ/m3)1/2未満であるラジカル重合性化合物(E)を15重量部以下の範囲で含有することを特徴とする請求項3~6のいずれかに記載の透明導電性積層フィルム。
- 前記活性エネルギー線硬化型接着剤組成物が、活性メチレン基を有するラジカル重合性化合物(F)と、水素引き抜き作用のあるラジカル重合開始剤(G)とを含有する請求項1~7のいずれかに記載の透明導電性積層フィルム。
- 前記活性メチレン基がアセトアセチル基である請求項8に記載の透明導電性積層フィルム。
- 前記活性メチレン基を有するラジカル重合性化合物(F)が、アセトアセトキシアルキル(メタ)アクリレートである請求項8または9に記載の透明導電性積層フィルム。
- 前記ラジカル重合開始剤(F)が、チオキサントン系ラジカル重合開始剤である請求項8~10のいずれかに記載の透明導電性積層フィルム。
- 前記活性エネルギー線硬化型接着剤組成物全量を100重量%としたとき、前記活性メチレン基を有するラジカル重合性化合物(F)を1~50重量%、およびラジカル重合開始剤(G)を0.1~10重量%含有する請求項8~11のいずれかに記載の透明導電性積層フィルム。
- 前記活性エネルギー線硬化型接着剤組成物が、光酸発生剤(H)を含有することを特徴とする請求項1~12のいずれかに記載の透明導電性積層フィルム。
- 光酸発生剤(H)として、PF6 -、SbF6 -およびAsF6 -からなる群より選択される少なくとも1種をカウンターアニオンとして有する光酸発生剤を含有する請求項13に記載の透明導電性積層フィルム。
- 前記活性エネルギー線硬化型接着剤組成物中に光酸発生剤(H)とアルコキシ基、エポキシ基いずれかを含む化合物(I)を併用することを特徴とする請求項1~14のいずれかに記載の透明導電性積層フィルム。
- 前記活性エネルギー線硬化型接着剤組成物が、アミノ基を有するシランカップリング剤(J)を含有する請求項1~15のいずれかに記載の透明導電性積層フィルム。
- 前記活性エネルギー線硬化型接着剤組成物全量を100重量%としたとき、アミノ基を有するシランカップリング剤(J)を0.01~20重量%含有する請求項16の透明導電性積層フィルム。
- 前記第1フィルム基材の厚さが、15μm~75μmであることを特徴とする請求項1~17のいずれかに記載の透明導電性積層フィルム。
- 前記透明硬化接着剤層の厚さが0.01μm以上10μm以下であることを特徴とする請求項1~18のいずれかに記載の透明導電性積層フィルム。
- 前記積層フィルムの第1透明導電層とは反対側の面に第2透明導電層を有することを特徴とする請求項1~19のいずれかに記載の透明導電性積層フィルム。
- 前記フィルム基材を形成する材料は、ポリエステル樹脂、環状ポリオレフィン樹脂、またはポリカーボネート樹脂のいずれかであることを特徴とする請求項1~20のいずれかに記載の透明導電性積層フィルム。
- 前記透明導電層を形成する材料は、インジウムスズ酸化物またはインジウム亜鉛酸化物のいずれかであることを特徴とする請求項1~21いずれかに記載の透明導電性積層フィルム。
- 前記透明導電層が結晶化していることを特徴とする請求項1~22のいずれかに記載の透明導電性積層フィルム。
- 前記透明導電層がパターニングされていることを特徴とする請求項1~23のいずれかに記載の透明導電性積層フィルム。
- 請求項1~24のいずれかに記載の透明導電性積層フィルムを少なくとも1つ備えていることを特徴とするタッチパネル。
- 請求項1~24のいずれかに記載の透明導電性積層フィルムの製造方法であって、
第1フィルム基材の一方の面に第1透明導電層が設けられた透明導電性フィルムを準備する工程aと、
前記透明導電性フィルムにおける、前記第1透明導電層を有しない前記第1フィルム基材の他方の面と、第2フィルム基材を、硬化によって、140℃における貯蔵弾性率が1×107Pa以上である透明硬化接着剤層を形成することができる、透明未硬化接着剤層により貼り合わせる工程b、および、
前記透明未硬化接着剤層を硬化させる工程cを有することを特徴とする透明導電性積層フィルムの製造方法。 - 工程cの後に、さらに、前記透明導電層を加熱処理して結晶化する工程dを有することを特徴とする請求項26記載の透明導電性積層フィルムの製造方法。
- 工程cの後に、さらに、前記透明導電層をパターニングする工程eを有することを特徴とする請求項26または27記載の透明導電性積層フィルムの製造方法。
- 前記工程cは、活性エネルギー線を前記透明未硬化接着剤層に照射することにより、前記透明未硬化接着剤層を硬化させる工程であり、
前記活性エネルギー線は、波長範囲380~450nmの可視光線を含むものである請求項26~28のいずれかに記載の透明導電性積層フィルムの製造方法。 - 前記活性エネルギー線は、波長範囲380~440nmの積算照度と波長範囲250~370nmの積算照度との比が100:0~100:50である請求項29に記載の透明導電性積層フィルムの製造方法。
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