WO2021182340A1 - Multilayered pressure-sensitive adhesive layer, multilayered pressure-sensitive adhesive layer with separator attached thereto and production method therefor, tack-type optical film, tack-type optical film with separator attached thereto and production method therefor, and image display device - Google Patents
Multilayered pressure-sensitive adhesive layer, multilayered pressure-sensitive adhesive layer with separator attached thereto and production method therefor, tack-type optical film, tack-type optical film with separator attached thereto and production method therefor, and image display device Download PDFInfo
- Publication number
- WO2021182340A1 WO2021182340A1 PCT/JP2021/008776 JP2021008776W WO2021182340A1 WO 2021182340 A1 WO2021182340 A1 WO 2021182340A1 JP 2021008776 W JP2021008776 W JP 2021008776W WO 2021182340 A1 WO2021182340 A1 WO 2021182340A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- sensitive adhesive
- pressure
- adhesive layer
- separator
- drying
- Prior art date
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- NMOALOSNPWTWRH-UHFFFAOYSA-N tert-butyl 7,7-dimethyloctaneperoxoate Chemical compound CC(C)(C)CCCCCC(=O)OOC(C)(C)C NMOALOSNPWTWRH-UHFFFAOYSA-N 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
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- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
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- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
-
- 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
- B32B27/00—Layered products comprising a layer of synthetic resin
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J201/00—Adhesives based on unspecified macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
-
- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
-
- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
- G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
- G09F9/301—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements flexible foldable or roll-able electronic displays, e.g. thin LCD, OLED
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K77/00—Constructional details of devices covered by this subclass and not covered by groups H10K10/80, H10K30/80, H10K50/80 or H10K59/80
- H10K77/10—Substrates, e.g. flexible substrates
- H10K77/111—Flexible substrates
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K2102/00—Constructional details relating to the organic devices covered by this subclass
- H10K2102/301—Details of OLEDs
- H10K2102/311—Flexible OLED
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/80—Constructional details
- H10K59/8791—Arrangements for improving contrast, e.g. preventing reflection of ambient light
Definitions
- the present invention relates to a multi-layered pressure-sensitive adhesive layer in which two or more pressure-sensitive adhesive layers are directly laminated, a multi-layered pressure-sensitive adhesive layer having a separator on one or both sides of the multi-layered pressure-sensitive adhesive layer, and a method for producing the same.
- the present invention relates to an adhesive optical film having a multilayer pressure-sensitive adhesive layer and an optical film, an adhesive-type optical film with a separator having the separator-attached multilayer pressure-sensitive adhesive layer and an optical film, a method for producing the same, and an image display device.
- the image display device include a liquid crystal display device (LCD), an organic EL display device, a CRT, and a PDP.
- a polarizing film is attached.
- various optical elements are used for the display panel such as the liquid crystal panel and the organic EL panel in order to improve the display quality of the display.
- a front plate is used to protect an image display device such as a liquid crystal display device, an organic EL display device, a CRT, and a PDP, to give a sense of quality, and to differentiate a design.
- the members used together with the image display device such as the liquid crystal display device and the organic EL display device and the image display device such as the front plate include, for example, a retardation plate for preventing coloring and a viewing angle of the liquid crystal display.
- a film that expands the viewing angle of the display a brightness-enhancing film that enhances the contrast of the display, a hard coat film that is used to impart scratch resistance to the surface, and an anti-glare treatment film that prevents reflection on an image display device.
- Surface-treated films such as anti-reflective films and anti-reflection films such as low-reflective films are used. These films are collectively called optical films.
- Deterioration of visibility due to unevenness of the optical film is one of the quality issues, and improvement is required.
- the surface unevenness of the pressure-sensitive adhesive layer and the adhesive layer used for bonding the optical films to each other or for bonding the optical films to the display panel is also visible. Therefore, it is necessary to take measures against it.
- Patent Document 1 an adhesive type optical film having an optical film and an adhesive layer provided on the optical film for the purpose of reducing the problem of unevenness related to visibility based on the adhesive layer.
- the pressure-sensitive adhesive layer a pressure-sensitive optical film having a thickness ( ⁇ m) standard deviation value of 0.12 ⁇ m or less has been proposed.
- the adhesive layer has been thickened in order to improve the durability of the flexible panel, but there is a problem that the thickening of the adhesive layer tends to cause surface unevenness.
- the present invention solves the above-mentioned problems, and an object of the present invention is to provide a multi-layered pressure-sensitive adhesive layer in which surface unevenness that affects visibility is suppressed even though the thickness is increased. Further, the present invention relates to a multi-layered pressure-sensitive adhesive layer having a separator on one side or both sides of the multi-layered pressure-sensitive adhesive layer and a method for producing the same, an adhesive optical film having the multi-layered pressure-sensitive adhesive layer and an optical film. It is an object of the present invention to provide an adhesive optical film with a separator having the multilayer pressure-sensitive adhesive layer with a separator and an optical film, a method for producing the same, and an image display device having the same.
- the present invention is a multi-layered pressure-sensitive adhesive layer in which two or more pressure-sensitive adhesive layers are directly laminated.
- Each of the pressure-sensitive adhesive layers has a thickness of 10 to 20 ⁇ m, and has a thickness of 10 to 20 ⁇ m.
- the multi-layered pressure-sensitive adhesive layer has a total thickness of 20 to 100 ⁇ m, and the multi-layered pressure-sensitive adhesive layer relates to a multi-layered pressure-sensitive adhesive layer having an ISC-S value of 50 or less.
- the multilayered pressure-sensitive adhesive layer includes at least a first pressure-sensitive adhesive layer and a second pressure-sensitive adhesive layer that are directly laminated.
- the pressure-sensitive adhesive composition which is a material for forming the first pressure-sensitive adhesive layer, contains a (meth) acrylic polymer A and contains.
- the pressure-sensitive adhesive composition which is a material for forming the second pressure-sensitive adhesive layer, contains a (meth) acrylic polymer B and contains.
- the monomer composition which is the material for forming the (meth) acrylic polymer A and the monomer composition which is the material for forming the (meth) acrylic polymer B are alkyl (meth) acrylates having an alkyl group having 1 to 18 carbon atoms. Is preferably contained in an amount of 50% by mass or more.
- the monomer composition which is the material for forming the (meth) acrylic polymer A and the monomer composition which is the material for forming the (meth) acrylic polymer B contain 50% by mass or more of the same alkyl (meth) acrylate. Is preferable.
- the multi-layered pressure-sensitive adhesive layer is preferably a multi-layered pressure-sensitive adhesive layer for an organic EL display device.
- the present invention also relates to a multi-layered pressure-sensitive adhesive layer with a separator having separators on one side or both sides of the multi-layered pressure-sensitive adhesive layer.
- the multilayer pressure-sensitive adhesive layer with a separator preferably has a separator peeling force of 0.15 N / 50 mm or less measured under the conditions of a tensile speed of 300 mm / min and a peeling angle of 180 degrees.
- the present invention also relates to an adhesive type optical film having the multi-layered pressure-sensitive adhesive layer and an optical film.
- the adhesive optical film is preferably an adhesive optical film for a flexible image display device.
- the present invention also relates to an adhesive optical film with a separator having the multilayer adhesive layer with a separator and an optical film.
- the present invention also relates to the multilayer pressure-sensitive adhesive layer or an image display device having the pressure-sensitive optical film.
- the present invention relates to a step of applying a pressure-sensitive adhesive composition on a separator, and a pressure-sensitive adhesive composition applied under conditions of a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 to 30 seconds.
- the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 85 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 10 to 120 seconds is dried.
- the drying step includes a third drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds after the second drying step.
- a step of forming an adhesive layer on a separator by a drying step Further, the separator comprising a step of applying another pressure-sensitive adhesive composition on the pressure-sensitive adhesive layer and a step of sequentially laminating another pressure-sensitive adhesive layer on the pressure-sensitive adhesive layer by repeating the drying step.
- the pressure-sensitive adhesive composition is applied under the conditions of a step of applying the pressure-sensitive adhesive composition on one separator, a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 to 30 seconds.
- the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 85 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 10 to 120 seconds is dried.
- a second drying step after the second drying step, a third drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds.
- the present invention relates to a method for producing a multilayer pressure-sensitive adhesive layer with a separator, which comprises a step of laminating a pressure-sensitive adhesive layer on the one separator and a pressure-sensitive adhesive layer on the other separator.
- the pressure-sensitive adhesive composition is applied under the conditions of a step of applying the pressure-sensitive adhesive composition on one separator, a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 to 30 seconds.
- the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 85 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 10 to 120 seconds is dried.
- a second drying step after the second drying step, a third drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds.
- the present invention relates to a method for producing an adhesive optical film with a separator, which comprises a step of laminating an adhesive layer on the optical film and an adhesive layer on the other separator.
- the multi-layered pressure-sensitive adhesive layer of the present invention achieves thickening while suppressing surface unevenness of each pressure-sensitive adhesive layer and suppressing surface unevenness of the entire pressure-sensitive adhesive layer by laminating a plurality of pressure-sensitive adhesive layers having a small thickness. It was done. The reason why the surface unevenness of each pressure-sensitive adhesive layer is suppressed by reducing the thickness of each pressure-sensitive adhesive layer is not clear, but it is considered as follows.
- the pressure-sensitive adhesive layer is usually formed by applying the pressure-sensitive adhesive composition on a base material such as a separator and drying (solidifying) the pressure-sensitive adhesive layer. However, when the coating film of the pressure-sensitive adhesive composition is thick.
- the multi-layered pressure-sensitive adhesive layer of the present invention has a total thickness of 20 to 100 ⁇ m, and although it has a sufficient thickness for improving the durability of the flexible panel, the ISC-S value indicating the streak unevenness ratio is exhibited. Is 50 or less, and surface unevenness that affects visibility is greatly suppressed.
- the multi-layered pressure-sensitive adhesive layer of the present invention has two or more pressure-sensitive adhesive layers directly laminated, has a total thickness of 20 to 100 ⁇ m, and has an ISC-S value of 50 or less.
- the thickness of each of the pressure-sensitive adhesive layers is 10 to 20 ⁇ m.
- Examples of the adhesive (adhesive composition) forming the multi-layer adhesive layer of the present invention include acrylic adhesive, rubber adhesive, vinyl alkyl ether adhesive, silicone adhesive, and polyester adhesive. , Polyamide-based pressure-sensitive adhesive, urethane-based pressure-sensitive adhesive, fluorine-based pressure-sensitive adhesive, epoxy-based pressure-sensitive adhesive, polyether-based pressure-sensitive adhesive, and the like.
- the pressure-sensitive adhesives constituting the respective pressure-sensitive adhesive layers may be the same type of pressure-sensitive adhesives or different types of pressure-sensitive adhesives, but the same type of pressure-sensitive adhesives may be used from the viewpoint of improving the adhesion between the pressure-sensitive adhesive layers. It is preferably an agent. Further, from the viewpoints of transparency, processability, durability, adhesion, bending resistance and the like, it is preferable to use an acrylic pressure-sensitive adhesive containing a (meth) acrylic polymer.
- the acrylic pressure-sensitive adhesive uses a (meth) acrylic polymer having an alkyl (meth) acrylate monomer unit as the main skeleton as a base polymer.
- (meth) acrylate means acrylate and / or methacrylate, and has the same meaning as (meth) of the present invention.
- the alkyl group of the alkyl (meth) acrylate, which constitutes the main skeleton of the (meth) acrylic polymer has about 1 to 14 carbon atoms.
- Specific examples of the alkyl (meth) acrylate include methyl (meth) acrylate and ethyl.
- an alkyl (meth) acrylate having an alkyl group having 1 to 18 carbon atoms is preferable, and an alkyl (meth) acrylate having an alkyl group having 1 to 9 carbon atoms is more preferable.
- the (meth) acrylic polymer one or more kinds of various monomers can be introduced by copolymerization for the purpose of improving adhesiveness and heat resistance.
- a copolymerization monomer include a carboxy group-containing monomer, a hydroxyl group-containing monomer, a nitrogen-containing monomer (including a heterocyclic ring-containing monomer), an aromatic-containing monomer, and the like.
- carboxy group-containing monomer examples include acrylic acid, methacrylic acid, carboxyethyl (meth) acrylate, carboxypentyl (meth) acrylate, itaconic acid, maleic acid, fumaric acid, and crotonic acid. Of these, acrylic acid and methacrylic acid are preferable.
- hydroxyl group-containing monomer examples include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, 6-hydroxyhexyl (meth) acrylate, and 8-hydroxyoctyl (meth) acrylate.
- examples thereof include 10-hydroxydecyl (meth) acrylate, 12-hydroxylauryl (meth) acrylate and (4-hydroxymethylcyclohexyl) -methyl acrylate.
- nitrogen-containing monomers examples include maleimide, N-cyclohexyl maleimide, N-phenylmaleimide; N-acryloylmorpholin; (meth) acrylamide, N, N-dimethyl (meth) acrylamide, N, N-diethyl (meth).
- N-hexyl (meth) acrylamide N-methyl (meth) acrylamide, N-butyl (meth) acrylamide, N-butyl (meth) acrylamide, N-methylol (meth) acrylamide, N-methylol propane (meth) acrylamide (N-substituted) amide-based monomers such as (meth) aminoethyl acrylate, aminopropyl (meth) acrylate, N, N-dimethylaminoethyl (meth) acrylate, t-butylaminoethyl (meth) acrylate.
- Alkylaminoalkyl (meth) acrylate monomers such as 3- (3-pyrinidyl) propyl (meth) acrylate; alkoxyalkyl (meth) acrylate such as methoxyethyl (meth) acrylate, ethoxyethyl (meth) acrylate System monomers: Succinimide-based monomers such as N- (meth) acryloyloxymethylene succinimide, N- (meth) acryloyl-6-oxyhexamethylene succinimide, N- (meth) acryloyl-8-oxyoctamethylene succinimide, and N-acryloylmorpholin. Is also given as an example of a monomer for the purpose of modification.
- aromatic-containing monomer examples include benzyl (meth) acrylate, phenyl (meth) acrylate, and phenoxyethyl (meth) acrylate.
- acid anhydride group-containing monomers such as maleic anhydride and itaconic anhydride; caprolactone adducts of acrylic acid; styrene sulfonic acid, allyl sulfonic acid, 2- (meth) acrylamide-2-methylpropan sulfonic acid.
- Vinyl-based monomers such as styrene, ⁇ -methylstyrene, N-vinylcaprolactam; cyanoacrylate-based monomers such as acrylonitrile and methacrylonitrile; epoxy group-containing acrylic monomers such as glycidyl (meth) acrylate; (meth) acrylic Glycol-based acrylic ester monomers such as polyethylene glycol acid acid, polypropylene glycol (meth) acrylate, methoxyethylene glycol (meth) acrylate, methoxypolypropylene glycol (meth) acrylate; tetrahydrofurfuryl (meth) acrylate, fluorine (meth) Acrylic acid ester-based monomers such as acrylate, silicone (meth) acrylate and 2-methoxyethyl acrylate can also be used.
- a hydroxyl group-containing monomer is preferably used because it has good reactivity with a cross-linking agent.
- a carboxy group-containing monomer such as acrylic acid is preferably used.
- the ratio of the copolymerization monomer in the (meth) acrylic polymer is not particularly limited, but is 20% by mass or less in terms of mass ratio. It is preferably 0.1 to 10% by mass, more preferably 0.5 to 8% by mass, and even more preferably 1 to 6% by mass.
- the mass ratio is preferably 0.01 to 5% by mass, more preferably 0.05 to 3% by mass, and further preferably 0.1 to 2% by mass.
- the mass ratio is preferably 0.01 to 15% by mass, more preferably 0.1 to 10% by mass, and further preferably 1 to 5% by mass.
- the average molecular weight of the (meth) acrylic polymer is not particularly limited, but the weight average molecular weight is preferably about 300,000 to 2.5 million.
- the (meth) acrylic polymer can be produced by various known methods, and for example, a radical polymerization method such as a bulk polymerization method, a solution polymerization method, or a suspension polymerization method can be appropriately selected.
- a radical polymerization method such as a bulk polymerization method, a solution polymerization method, or a suspension polymerization method can be appropriately selected.
- the radical polymerization initiator various known azo-based and peroxide-based radical polymerization initiators can be used.
- the reaction temperature is usually about 50 to 80 ° C., and the reaction time is 1 to 8 hours.
- the solution polymerization method is preferable, and ethyl acetate, toluene and the like are generally used as the solvent for the (meth) acrylic polymer.
- the pressure-sensitive adhesive composition forming the multi-layered pressure-sensitive adhesive layer of the present invention can contain a cross-linking agent in addition to the base polymer.
- the cross-linking agent can improve the adhesion and durability between the pressure-sensitive adhesive layers or between the pressure-sensitive adhesive layers and the optical film, and can maintain reliability at high temperatures and the shape of the pressure-sensitive adhesive itself.
- the base polymer is a (meth) acrylic polymer
- an isocyanate-based, epoxy-based, peroxide-based, metal chelate-based, oxazoline-based, or the like can be appropriately used as the cross-linking agent.
- These cross-linking agents may be used alone or in combination of two or more.
- An isocyanate compound is used as the isocyanate-based cross-linking agent.
- the isocyanate compound include isocyanate monomers such as tolylene diisocyanate, chlorphenylene diisocyanate, hexamethylene diisosianate, tetramethylene diisosianate, isophorone diisocyanate, xylylene diisocyanate, diphenylmethane diisocyanate, and hydrogenated diphenylmethane diisocyanate, and these isocyanates.
- Adduct-based isocyanate compound in which a monomer is added to trimethylolpropane or the like; isocyanurate product, burette type compound, and urethane pre-reacted by addition reaction of known polyether polyol, polyester polyol, acrylic polyol, polybutadiene polyol, polyisoprene polyol, etc. Examples include polymer type isocyanate.
- Examples of the epoxy-based cross-linking agent include bisphenol A epichlorohydrin type epoxy resin.
- Examples of the epoxy-based cross-linking agent include ethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether, glycerin diglycidyl ether, glycerin triglycidyl ether, 1,6-hexanediol diglycidyl ether, and trimethylolpropan triglycidyl ether.
- Diglycidylaniline N, N, N', N'-tetraglycidyl-m-xylylene diamine, 1,3-bis (N, N-diglycidylaminomethyl) cyclohexane, N, N, N', N'- Examples thereof include tetraglycidyl aminophenyl methane, triglycidyl isocyanurate, m-N, N-diglycidyl aminophenyl glycidyl ether, N, N-diglycidyl toluidine, and N, N-diglycidyl aniline.
- Peroxides include di (2-ethylhexyl) peroxydicarbonate, di (4-t-butylcyclohexyl) peroxydicarbonate, di-sec-butylperoxydicarbonate, and t-butylperoxyneodecanoate.
- di (4-t-butylcyclohexyl) peroxydicarbonate, dilauroyl peroxide, and dibenzoyl peroxide which are particularly excellent in cross-linking reaction efficiency, are preferably used.
- the amount of the cross-linking agent used is 10 parts by mass or less, preferably 0.01 to 5 parts by mass, and more preferably 0.1 to 1 part by mass with respect to 100 parts by mass of the (meth) acrylic polymer. If the proportion of the cross-linking agent used exceeds 10 parts by mass, the cross-linking may proceed too much and the adhesiveness may deteriorate.
- the pressure-sensitive adhesive composition includes, if necessary, a pressure-imparting agent, a plasticizing agent, a glass fiber, a glass bead, a metal powder, a filler made of other inorganic powder, a pigment, a colorant, a filler, and the like.
- a pressure-imparting agent e.g., a plasticizing agent
- a glass fiber e.g., a glass fiber
- a glass bead e.g., a metal powder
- a filler made of other inorganic powder e.g., a pigment, a colorant, a filler, and the like.
- Antioxidants, ultraviolet absorbers, silane coupling agents and the like can be appropriately used, and various additives can be appropriately used without departing from the object of the present invention.
- a pressure-sensitive adhesive composition is applied on a separator, and the pressure-sensitive adhesive composition is dried or hardened (solidified) to form a pressure-sensitive adhesive layer. It can be produced by sequentially forming an adhesive layer on the layer in the same manner and then peeling off the separator. Further, in the multi-layered pressure-sensitive adhesive layer of the present invention, for example, a pressure-sensitive adhesive composition is applied on one separator, and the pressure-sensitive adhesive composition is dried or hardened (solidified) to form one layer of the pressure-sensitive adhesive layer.
- the pressure-sensitive adhesive composition is formed as described above, and the pressure-sensitive adhesive composition is applied onto the other separator, and the pressure-sensitive adhesive composition is dried or hardened (solidified) to form one or more pressure-sensitive adhesive layers, and one of them is formed. It can be produced by laminating one or more pressure-sensitive adhesive layers on a separator and one or more pressure-sensitive adhesive layers on the other separator, and then peeling off the separators on both sides.
- the pressure-sensitive adhesive composition may be either a solution or a dispersion.
- a solution for example, an aromatic solvent such as toluene and an ester solvent such as ethyl acetate are used.
- the solid content concentration of the pressure-sensitive adhesive composition is usually about 5 to 80% by mass, preferably 10 to 60% by mass, from the viewpoint of suppressing surface unevenness and obtaining the surface of the pressure-sensitive adhesive layer having an ISC-S value of 50 or less. , More preferably 10 to 40% by mass, still more preferably 10 to 20% by mass.
- the method of applying the pressure-sensitive adhesive composition on the separator or the pressure-sensitive adhesive layer is not particularly limited, and for example, a die coating method such as a closed edge die or a slot die; a roll coating method such as reverse coating or gravure coating, or spin coating.
- a coating method, a screen coating method, a fountain coating method, a dipping method, a spray method, etc. can be adopted.
- the thickness of each pressure-sensitive adhesive layer is from the viewpoint of suppressing surface unevenness to obtain a pressure-sensitive adhesive layer surface having an ISC-S value of 50 or less and from the viewpoint of manufacturing efficiency of a multi-layered pressure-sensitive adhesive layer having a total thickness of 20 to 100 ⁇ m. Therefore, it is 10 to 20 ⁇ m, preferably 10 to 15 ⁇ m, and more preferably 10 to 12 ⁇ m.
- Each of the pressure-sensitive adhesive layers has a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 from the viewpoint of suppressing surface unevenness and reducing the ISC-S value of the multilayer pressure-sensitive adhesive layer to 50 or less.
- the pressure-sensitive adhesive composition is dried under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds. It is preferably formed by a drying step including a third drying step.
- the solvent of the pressure-sensitive adhesive composition is gradually evaporated by the first and second drying steps, and the surface of the pressure-sensitive adhesive layer having an ISC-S value of 50 or less is formed. Then, the ISC- The surface of the pressure-sensitive adhesive layer having an S value of 50 or less is cured (solidified) to form a pressure-sensitive adhesive layer.
- the temperature in the first drying step is 30 to 105 ° C, preferably 40 to 100 ° C, more preferably 50 to 95 ° C, and even more preferably 70 to 95 ° C.
- the temperature is 30 ° C. or higher, the drying time of the solvent can be shortened, which is preferable from the viewpoint of production efficiency.
- the temperature is 105 ° C. or lower, rapid drying can be prevented and the surface of the pressure-sensitive adhesive layer having an ISC-S value of 50 or less can be easily formed, which is preferable.
- the wind speed in the first drying step is 0.5 to 7 m / sec, preferably 0.5 to 6 m / sec, more preferably 1 to 5 m / sec, and even more preferably 3 to 5 m / sec.
- the wind speed is 0.5 m / sec or more, the drying time of the solvent can be shortened, which is preferable from the viewpoint of production efficiency.
- the wind speed is 7 m / sec or less, rapid drying can be prevented and the surface of the pressure-sensitive adhesive layer having an ISC-S value of 50 or less can be easily formed, which is preferable.
- the drying time in the first drying step is 5 to 30 seconds, preferably 10 seconds to 25 seconds, and more preferably 15 seconds to 20 seconds.
- the drying time in the first drying step is controlled so that the ISC-S value of the pressure-sensitive adhesive layer is 50 or less in consideration of the relationship between the temperature and the wind speed.
- the temperature in the second drying step is 30 to 85 ° C, preferably 40 to 80 ° C, more preferably 50 to 75 ° C, and even more preferably 60 to 75 ° C.
- the temperature is 30 ° C. or higher, the drying time of the solvent can be shortened, which is preferable from the viewpoint of production efficiency.
- the temperature is 85 ° C. or lower, rapid drying can be prevented and the surface of the pressure-sensitive adhesive layer having an ISC-S value of 50 or less can be easily formed, which is preferable.
- the wind speed in the second drying step is 0.5 to 7 m / sec, preferably 0.5 to 6 m / sec, more preferably 1 to 5 m / sec, and even more preferably 3 to 5 m / sec.
- the wind speed is 0.5 m / sec or more, the drying time of the solvent can be shortened, which is preferable from the viewpoint of production efficiency.
- the wind speed is 7 m / sec or less, rapid drying can be prevented and the surface of the pressure-sensitive adhesive layer having an ISC-S value of 50 or less can be easily formed, which is preferable.
- the drying time in the second drying step is 10 to 120 seconds, preferably 30 seconds to 90 seconds, and more preferably 45 seconds to 60 seconds.
- the drying time in the second drying step is controlled so that the ISC-S value of the pressure-sensitive adhesive layer is 50 or less in consideration of the relationship between the temperature and the wind velocity.
- the temperature in the third drying step is 90 to 160 ° C, preferably 130 to 160 ° C, and more preferably 135 to 155 ° C.
- the temperature is 90 ° C. or higher, the drying time of the solvent can be shortened, which is preferable from the viewpoint of production efficiency.
- the temperature is 160 ° C. or lower, it is preferable because it is possible to prevent the pressure-sensitive adhesive layer from being colored.
- the wind velocity in the third drying step is 0.1 to 25 m / sec, preferably 1 to 23 m / sec, more preferably 5 to 20 m / sec, and even more preferably 10 to 20 m / sec.
- the wind speed is 0.1 m / sec or more, the drying time of the solvent can be shortened, which is preferable from the viewpoint of production efficiency.
- the wind speed is 25 m / sec or less, the running performance of the film is less likely to be adversely affected, which is preferable.
- the drying time in the third drying step is 10 to 180 seconds, preferably 20 seconds to 120 seconds, and more preferably 30 seconds to 60 seconds.
- the drying time in the third drying step is controlled so as to cure (solidify) the pressure-sensitive adhesive layer in consideration of the relationship between the temperature and the wind speed.
- an oven, a hot air blower, a heating roll, a far-infrared heater, or the like can be used as a means for controlling the temperature within the above range.
- a blowing means for controlling the wind velocity within the above range a counterflow method can be applied.
- the distance from the blower means is about 10 to 100 cm, preferably 10 to 50 cm.
- the wind speed can be measured by a mini-vane type digital anemometer.
- the wind velocity is measured by using a wind speed meter at a position 3 cm above the pressure-sensitive adhesive composition applied on the separator under the blower nozzle.
- an anemometer an anemometer MODEL1560 / SYSTEM 6243 manufactured by Kanomax Japan Incorporated is used.
- the multi-layered pressure-sensitive adhesive layer has two or more layers of the pressure-sensitive adhesive layer, and the pressure-sensitive adhesive layer may be three layers or four layers. From the viewpoint of manufacturing efficiency of the multilayer pressure-sensitive adhesive layer and from the viewpoint of reducing the thickness of the image display device, the number of layers is usually 5 or less.
- the pressure-sensitive adhesive composition that is a material for forming the first pressure-sensitive adhesive layer is (meth) acrylic.
- the pressure-sensitive adhesive composition containing the system polymer A and being the material for forming the second pressure-sensitive adhesive layer is the monomer composition containing the (meth) acrylic polymer B and being the material for forming the (meth) acrylic polymer A.
- the monomer composition which is the material for forming the (meth) acrylic polymer B preferably contains 50% by mass or more of an alkyl (meth) acrylate having an alkyl group having 1 to 18 carbon atoms, and more preferably 60% by mass.
- the alkyl group of the alkyl (meth) acrylate has more preferably 2 to 16 carbon atoms, and even more preferably 4 to 12 carbon atoms.
- the monomer composition which is the material for forming the (meth) acrylic polymer A and the monomer composition which is the material for forming the (meth) acrylic polymer B contain 50% by mass or more of the same alkyl (meth) acrylate. Is more preferable, more preferably 60% by mass or more, still more preferably 70% by mass or more, still more preferably 80% by mass or more, still more preferably 90% by mass or more.
- the adhesiveness and adhesiveness between the pressure-sensitive adhesive layers can be improved.
- the pressure-sensitive adhesive layer is also similar to the pressure-sensitive adhesive composition which is a material for forming the first pressure-sensitive adhesive layer and the second pressure-sensitive adhesive layer. It is preferably formed by using a pressure-sensitive adhesive composition having the same composition.
- the multi-layer adhesive layer has a total thickness of 20 to 100 ⁇ m, preferably 20 to 50 ⁇ m, from the viewpoint of improving the durability of the flexible panel (for example, a flexible organic EL panel) and reducing the thickness of the panel. It is preferably 20 to 40 ⁇ m.
- the multilayer pressure-sensitive adhesive layer has an ISC-S value representing a muscle unevenness ratio of 50 or less, preferably 45 or less, more preferably 35 or less, and further preferably 30 or less. According to the method for producing a multi-layered pressure-sensitive adhesive layer of the present invention, it is also possible to produce a multi-layered pressure-sensitive adhesive layer having an ISC-S value of 25 or less.
- the multi-layered pressure-sensitive adhesive layer with a separator of the present invention has a separator on one side or both sides of the multi-layered pressure-sensitive adhesive layer.
- the separator known ones can be used without particular limitation, and it is preferable to use a separator that has been peeled off.
- the multilayer pressure-sensitive adhesive layer with a separator of the present invention is, for example, coated with the pressure-sensitive adhesive composition on a separator, and the applied pressure-sensitive adhesive composition is cured (solidified) by a drying step including the first to third drying steps. )
- a drying step including the first to third drying steps To form a pressure-sensitive adhesive layer, and further repeat a step of applying another pressure-sensitive adhesive composition on the pressure-sensitive adhesive layer and a drying step including the first to third drying steps to obtain the pressure-sensitive adhesive. It can be produced by sequentially laminating another pressure-sensitive adhesive layer on the agent layer.
- a pressure-sensitive adhesive composition is applied on one of the separators, and the applied pressure-sensitive adhesive composition is subjected to a drying step including the first to third drying steps. It is cured (solidified) to form one or more pressure-sensitive adhesive layers on one separator, one or more pressure-sensitive adhesive layers on the other separator in the same manner, and adhesion on one separator. It can be produced by laminating the agent layer and the pressure-sensitive adhesive layer on the other separator.
- the multi-layer adhesive layer with a separator has a separator peeling force of 0.15 N / 50 mm measured under the conditions of a tensile speed of 300 mm / min and a peeling angle of 180 degrees from the viewpoint of improving handleability and panel manufacturing efficiency. It is preferably 0.14 N / 50 mm or less, more preferably 0.13 N / 50 mm or less.
- the coating thickness of the pressure-sensitive adhesive composition applied on the separator is large, the amount of peroxide contained in the pressure-sensitive adhesive composition is relatively large and reacts with the separator. It is considered that the separator is difficult to peel off because it becomes easy.
- the coating thickness of the pressure-sensitive adhesive composition applied on the separator is small, so that the amount of peroxide contained in the pressure-sensitive adhesive composition is relatively large. It is considered that the amount of the separator peeling force becomes small and the peeling becomes easy because the amount of the separator is reduced and the reaction with the separator becomes difficult.
- the pressure-sensitive optical film of the present invention has the multilayer pressure-sensitive adhesive layer and an optical film.
- the optical film is not particularly limited, and examples thereof include an optical film used in an image display device such as a liquid crystal display (LCD), an organic EL display device, a CRT, and a PDP. Specific examples thereof include a polarizing film and a phase difference. Examples thereof include a plate, a viewing angle expanding film, a brightness improving film, a hard coat film, an anti-glare treated film, an anti-reflective film, an anti-reflection film such as a low reflective film, and a film in which these are laminated.
- the pressure-sensitive optical film can be produced, for example, by laminating an optical film on one side or both sides of the multi-layered pressure-sensitive adhesive layer of the multi-layered pressure-sensitive adhesive layer with a separator.
- the pressure-sensitive adhesive film with a separator of the present invention has the multilayer pressure-sensitive adhesive layer with a separator and the optical film.
- the pressure-sensitive adhesive composition is coated on a separator, and the coated pressure-sensitive adhesive composition is cured (solidified) by a drying step including the first to third drying steps.
- the pressure-sensitive adhesive is formed by forming a pressure-sensitive adhesive layer, and further repeating a step of applying another pressure-sensitive adhesive composition on the pressure-sensitive adhesive layer and a drying step including the first to third drying steps are performed to obtain the pressure-sensitive adhesive.
- Another pressure-sensitive adhesive layer is sequentially laminated on the layer to prepare a multi-layered pressure-sensitive adhesive layer with a separator, and an optical film is bonded to one side of the multi-layered pressure-sensitive adhesive layer of the multi-layered pressure-sensitive adhesive layer with a separator. Can be done.
- a pressure-sensitive adhesive composition is applied onto one of the separators, and the coated pressure-sensitive adhesive composition is cured by a drying step including the first to third drying steps.
- a drying step including the first to third drying steps.
- one or more pressure-sensitive adhesive layers are formed on one separator, an optical film is laminated on the surface of the pressure-sensitive adhesive layer that does not have the separator, and then the separator is peeled off in the same manner. It can be produced by forming one or more pressure-sensitive adhesive layers on the other separator, and then laminating the pressure-sensitive adhesive layer on the optical film and the pressure-sensitive adhesive layer on the other separator.
- the adhesive optical film of the present invention is useful as a constituent member of a flexible image display device (for example, a flexible organic EL display device).
- the adhesive optical film for a flexible image display device of the present invention is characterized by including the multilayer pressure-sensitive adhesive layer and an optical film containing at least a polarizing film, and the optical film includes, in addition to the polarizing film, the polarizing film.
- the optical film refers to a film including a protective film or a retardation film formed from a transparent resin material.
- the optical film the polarizing film, the protective film of the transparent resin material provided on the first surface of the polarizing film, and the second surface different from the first surface of the polarizing film.
- the structure including the retardation film provided in the above is referred to as an optical laminate.
- the thickness of the optical film is preferably 92 ⁇ m or less, more preferably 60 ⁇ m or less, and further preferably 10 to 50 ⁇ m. If it is within the above range, it will be a preferable embodiment without inhibiting bending.
- the polarizing film may have a protective film bonded to at least one side by an adhesive (layer) (not shown in the drawing).
- An adhesive can be used for the bonding treatment between the polarizing film and the protective film.
- the adhesive include isocyanate-based adhesives, polyvinyl alcohol-based adhesives, gelatin-based adhesives, vinyl-based latex-based adhesives, and water-based polyesters.
- the adhesive is usually used as an adhesive composed of an aqueous solution, and usually contains 0.5 to 60% by mass of a solid content.
- examples of the adhesive between the polarizing film and the protective film include an ultraviolet curable adhesive and an electron beam curable adhesive.
- the electron beam curable polarizing film adhesive exhibits suitable adhesiveness to the above-mentioned various protective films.
- the adhesive used in the present invention may contain a metal compound filler.
- a polarizing film and a protective film bonded together with an adhesive (layer) may be referred to as a polarizing film (plate plate).
- the polarizing film (also referred to as a polarizer) contained in the optical film of the present invention is polyvinyl alcohol (PVA) in which iodine is oriented, which is stretched by a stretching step such as aerial stretching (dry stretching) or boric acid water stretching step.
- PVA polyvinyl alcohol
- a system resin can be used.
- the thickness of the polarizing film is 20 ⁇ m or less, preferably 12 ⁇ m or less, more preferably 9 ⁇ m or less, still more preferably 1 to 8 ⁇ m, and particularly preferably 3 to 6 ⁇ m. If it is within the above range, it will be a preferable embodiment without inhibiting bending.
- the optical film used in the present invention may include a retardation film, and the retardation film (also referred to as a retardation film) is obtained by stretching a polymer film or a liquid crystal material is oriented and fixed. It is possible to use a modified product.
- the retardation film refers to a film having birefringence in the in-plane and / or thickness direction.
- the retardation film examples include an antireflection retardation film (see Japanese Patent Application Laid-Open No. 2012-133303 [0221], [0222], and [0228]) and a viewing angle compensation retardation film (Japanese Patent Laid-Open No. 2012-133303 [0225]. ], [0226]), tilt-oriented retardation film for viewing angle compensation (see Japanese Patent Application Laid-Open No. 2012-133303 [0227]), and the like.
- the retardation film as long as it has substantially the above-mentioned functions, for example, the retardation value, the arrangement angle, the three-dimensional birefringence, and whether it is a single layer or a multilayer are not particularly limited and are known retardation films. Can be used.
- the thickness of the retardation film is preferably 20 ⁇ m or less, more preferably 10 ⁇ m or less, further preferably 1 to 9 ⁇ m, and particularly preferably 3 to 8 ⁇ m. If it is within the above range, it will be a preferable embodiment without inhibiting bending.
- the optical film used in the present invention can include a protective film formed from a transparent resin material, and the protective film (also referred to as a transparent protective film) is a cycloolefin resin such as a norbornene resin, polyethylene, or the like. Olefin-based resins such as polypropylene, polyester-based resins, (meth) acrylic-based resins, and the like can be used.
- the thickness of the protective film is preferably 5 to 60 ⁇ m, more preferably 10 to 40 ⁇ m, still more preferably 10 to 30 ⁇ m, and a surface treatment layer such as an anti-glare layer or an anti-reflection layer is appropriately provided. Can be done. If it is within the above range, it will be a preferable embodiment without inhibiting bending.
- the pressure-sensitive optical film for a flexible image display device of the present invention includes at least one of the multilayer pressure-sensitive adhesive layers.
- the adhesive optical film for a flexible image display device may have one of the multilayer adhesive layers, but in addition to the optical film, a transparent conductive film, an organic EL display panel, a window, a decorative printing film, and the like. Two or more may be provided for laminating the retardation layer, the protective film, etc. (for example, an adhesive optical film for a flexible image display device such as a first multilayer adhesive layer and a second multilayer adhesive layer). As a case where a plurality of multilayer pressure-sensitive adhesive layers are provided therein, for example, see FIG. 1 and the like). When having a plurality of multilayer pressure-sensitive adhesive layers, it is preferable to have two or more and five or less.
- the thickness of the entire adhesive optical film becomes thick, so that the strain difference between the outermost layer and the innermost layer at the bent portion of the adhesive optical film becomes large, and peeling or breakage is likely to occur, which is not preferable. ..
- the first multi-layered pressure-sensitive adhesive layer is on the side opposite to the surface in contact with the polarizing film with respect to the protective film. (See FIG. 1).
- the second multi-layered pressure-sensitive adhesive layer is opposite to the surface of the retardation film in contact with the polarizing film. It can be placed on the side (see FIG. 1).
- the third multi-layered pressure-sensitive adhesive layer is the second multi-layered adhesive layer with respect to the transparent conductive layer constituting the touch sensor.
- a third multilayer pressure-sensitive adhesive layer can be arranged on the side opposite to the surface in contact with the chemical pressure-sensitive adhesive layer (see FIG. 1).
- the third multi-layered pressure-sensitive adhesive layer is the first multi-layered adhesive layer with respect to the transparent conductive layer constituting the touch sensor. It can be arranged on the side opposite to the surface in contact with the chemical pressure-sensitive adhesive layer (see FIG. 2).
- the pressure-sensitive adhesive layer may have the same composition (same pressure-sensitive adhesive composition), the same properties, or different properties, and is not particularly limited, but from the viewpoints of workability, economy, and flexibility. Therefore, it is preferable that all the pressure-sensitive adhesive layers are pressure-sensitive adhesive layers having substantially the same composition and the same characteristics.
- the member having a transparent conductive layer is not particularly limited, and known members can be used, but a member having a transparent conductive layer on a transparent base material such as a transparent film, or a transparent conductive layer and a liquid crystal display. A member having a cell can be mentioned.
- the transparent base material may be any transparent material, and examples thereof include a base material made of a resin film or the like (for example, a sheet-like, film-like, plate-like base material, etc.).
- the thickness of the transparent base material is not particularly limited, but is preferably about 10 to 200 ⁇ m, more preferably about 15 to 150 ⁇ m.
- the material of the resin film is not particularly limited, and examples thereof include various transparent plastic materials.
- polyester resin such as polyethylene terephthalate and polyethylene naphthalate, acetate resin, polyether sulfone resin, polycarbonate resin, polyamide resin, polyimide resin, polyolefin resin, (meth) acrylic resin.
- polyester-based resins, polyimide-based resins and polyether sulfone-based resins are particularly preferable.
- the transparent base material is subjected to etching treatment such as sputtering, corona discharge, flame, ultraviolet irradiation, electron beam irradiation, chemical conversion, oxidation, etc., and undercoating treatment in advance on the surface, and the transparent conductive layer provided on the transparent base material.
- etching treatment such as sputtering, corona discharge, flame, ultraviolet irradiation, electron beam irradiation, chemical conversion, oxidation, etc.
- undercoating treatment in advance on the surface
- the adhesion to the transparent substrate may be improved.
- dust may be removed and cleaned by solvent cleaning, ultrasonic cleaning, or the like, if necessary.
- the constituent material of the transparent conductive layer is not particularly limited, and is selected from the group consisting of indium, tin, zinc, gallium, antimony, titanium, silicon, zirconium, magnesium, aluminum, gold, silver, copper, palladium, tungsten and molybdenum. At least one kind of metal or metal oxide to be used, or an organic conductive polymer such as polythiophene is used.
- the metal oxide may further contain the metal atoms shown in the above group, if necessary.
- indium oxide (ITO) containing tin oxide, tin oxide containing antimony, and the like are preferably used, and ITO is particularly preferably used.
- the ITO preferably contains 80 to 99% by mass of indium oxide and 1 to 20% by mass of tin oxide.
- examples of the ITO include crystalline ITO and non-crystalline (amorphous) ITO.
- the crystalline ITO can be obtained by applying a high temperature during sputtering or further heating the non-crystalline ITO.
- the thickness of the transparent conductive layer is preferably 0.005 to 10 ⁇ m, more preferably 0.01 to 3 ⁇ m, and further preferably 0.01 to 1 ⁇ m. If the thickness of the transparent conductive layer is less than 0.005 ⁇ m, the change in the electric resistance value of the transparent conductive layer tends to be large. On the other hand, if it exceeds 10 ⁇ m, the productivity of the transparent conductive layer tends to decrease, the cost also increases, and the optical characteristics tend to decrease.
- the total light transmittance of the transparent conductive layer is preferably 80% or more, more preferably 85% or more, and further preferably 90% or more.
- the density of the transparent conductive layer is preferably 1.0 to 10.5 g / cm 3 , and more preferably 1.3 to 3.0 g / cm 3 .
- the surface resistance value of the transparent conductive layer is preferably 0.1 to 1000 ⁇ / ⁇ , more preferably 0.5 to 500 ⁇ / ⁇ , and further preferably 1 to 250 ⁇ / ⁇ .
- the method for forming the transparent conductive layer is not particularly limited, and a conventionally known method can be adopted. Specifically, for example, a vacuum deposition method, a sputtering method, and an ion plating method can be exemplified. Further, an appropriate method can be adopted depending on the required film thickness.
- an undercoat layer, an oligomer prevention layer, etc. can be provided between the transparent conductive layer and the transparent base material, if necessary.
- the transparent conductive layer constitutes a touch sensor and is required to be bendable.
- the transparent conductive layer constituting the touch sensor is on the side opposite to the surface in contact with the retardation film with respect to the second multilayer adhesive layer. Can be placed in (see FIG. 1).
- the transparent conductive layer constituting the touch sensor is placed on the side opposite to the surface in contact with the protective film with respect to the first multilayer adhesive layer. It can be arranged (see FIG. 2).
- the transparent conductive layer constituting the touch sensor can be arranged between the protective film and the window film (OCA) (see FIG. 2).
- the transparent conductive layer can be suitably applied to a liquid crystal display device having a built-in touch sensor such as an in-cell type or an on-cell type when used in a flexible image display device, and in particular, the touch sensor is built in an organic EL display panel. It may be (incorporated).
- the adhesive optical film for a flexible image display device of the present invention may have a conductive layer (conductive layer, antistatic layer). Since the adhesive optical film for a flexible image display device has a bending function and has a very thin thickness structure, it is highly responsive to weak static electricity generated in a manufacturing process or the like and is easily damaged. By providing the conductive layer on the adhesive optical film, the load due to static electricity in the manufacturing process or the like is greatly reduced, which is a preferable embodiment.
- one of the major features of the flexible image display device including the adhesive optical film is that it has a bending function, but when it is continuously bent, static electricity is generated due to shrinkage between the films (base materials) of the bent portion. May occur. Therefore, when the adhesive optical film is imparted with conductivity, the generated static electricity can be quickly removed, and the damage caused by the static electricity of the image display device can be reduced, which is a preferable embodiment.
- the conductive layer may be an undercoat layer having a conductive function, an adhesive containing a conductive component, or a surface treatment layer containing a conductive component.
- a method of forming a conductive layer between a polarizing film and a multilayer pressure-sensitive adhesive layer by using an antistatic agent composition containing a conductive polymer such as polythiophene and a binder can be adopted.
- a pressure-sensitive adhesive containing an ionic compound which is an antistatic agent can also be used.
- the conductive layer preferably has one or more layers, and may include two or more layers.
- the flexible image display device of the present invention includes the above-mentioned adhesive optical film for a flexible image display device and an organic EL display panel, and the adhesive optical film for a flexible image display device is on the visual side with respect to the organic EL display panel. It is arranged and configured to be foldable. Although optional, a window can be arranged on the viewing side with respect to the adhesive optical film for a flexible image display device (see FIGS. 1 to 3).
- FIG. 1 is a cross-sectional view showing one embodiment of the flexible image display device according to the present invention.
- the flexible image display device 100 includes an adhesive optical film 11 for a flexible image display device and an organic EL display panel 10 configured to be foldable.
- An adhesive optical film 11 for a flexible image display device is arranged on the visual side with respect to the organic EL display panel 10, and the flexible image display device 100 is configured to be bendable.
- a transparent window 40 can be arranged on the visual side of the adhesive optical film 11 for a flexible image display device via the first multilayer adhesive layer 12-1.
- the adhesive optical film 11 for a flexible image display device comprises an optical laminate 20, a second multi-layered pressure-sensitive adhesive layer 12-2, and a third multi-layered pressure-sensitive adhesive layer 12-3. Including layers.
- the optical laminate 20 includes a polarizing film 1, a protective film 2 made of a transparent resin material, and a retardation film 3.
- the protective film 2 made of a transparent resin material is joined to the first surface of the polarizing film 1 on the visible side.
- the retardation film 3 is joined to a second surface different from the first surface of the polarizing film 1.
- the polarizing film 1 and the retardation film 3 generate circular polarization or have a viewing angle, for example, in order to prevent light incident on the inside of the polarizing film 1 from the viewing side from being internally reflected and emitted to the viewing side. It is for compensating for.
- the protective film is provided on both sides of the conventional polarizing film, whereas the protective film is provided on only one side, and the polarizing film itself is also used in the conventional organic EL display device.
- the thickness of the optical laminate 20 can be reduced by using a polarizing film having a thickness very thin (20 ⁇ m or less) as compared with the polarizing film. Further, since the polarizing film 1 is much thinner than the polarizing film used in the conventional organic EL display device, the stress due to expansion and contraction generated under temperature or humidity conditions becomes extremely small.
- the possibility that the stress caused by the shrinkage of the polarizing film causes deformation such as warpage in the adjacent organic EL display panel 10 is greatly reduced, and the deterioration of display quality and the destruction of the panel encapsulating material due to the deformation are greatly reduced. It becomes possible to suppress. Further, the use of a thin polarizing film does not hinder bending, which is a preferable embodiment.
- the thickness of the optical laminate 20 (for example, 92 ⁇ m or less) is reduced, and the first multilayer adhesive layer 12-1 is applied to the protective film 2.
- the thickness of the optical laminate 20 for example, 92 ⁇ m or less
- the first multilayer adhesive layer 12-1 is applied to the protective film 2.
- a bendable transparent conductive layer 6 constituting the touch sensor can be further arranged on the side opposite to the protective film 2 with respect to the retardation film 3.
- the transparent conductive layer 6 is configured to be directly bonded to the retardation film 3 by, for example, a manufacturing method as shown in Japanese Patent Application Laid-Open No. 2014-219667, whereby the thickness of the optical laminate 20 is reduced, and the optical laminate 20 is reduced. The stress applied to the optical laminate 20 when the product is bent can be further reduced.
- the pressure-sensitive adhesive layer constituting the third multilayer pressure-sensitive adhesive layer 12-3 can be further arranged on the side opposite to the retardation film 3 with respect to the transparent conductive layer 6.
- the second multilayer pressure-sensitive adhesive layer 12-2 is directly bonded to the transparent conductive layer 6.
- the flexible image display device shown in FIG. 2 is almost the same as that shown in FIG. 1, but in the flexible image display device of FIG. 1, a touch sensor is located on the opposite side of the retardation film 3 from the protective film 2.
- the protective film 2 is different from the first multilayer pressure-sensitive adhesive layer 12-1.
- the bendable transparent conductive layer 6 constituting the touch sensor is arranged on the opposite side.
- the third multilayer pressure-sensitive adhesive layer 12-3 is arranged on the side opposite to the retardation film 3 with respect to the transparent conductive layer 6, whereas FIG.
- the flexible image display device of No. 2 is different in that the second multilayer adhesive layer 12-2 is arranged on the side opposite to the protective film 2 with respect to the retardation film 3.
- the third multilayer adhesive layer 12-3 can be arranged. ..
- the flexible image display device of the present invention can be suitably used as a flexible liquid crystal display device, an organic EL (electroluminescence) display device, an image display device such as electronic paper, and the like. Further, it can be used regardless of a method such as a touch panel such as a resistance film method or a capacitance method.
- the flexible image display device of the present invention as shown in FIG. 3, it is also used as an in-cell type flexible image display device in which the transparent conductive layer 6 constituting the touch sensor is built in the organic EL display panel 10-1. It is possible to do.
- a solution containing an acrylic polymer (A) having a weight average molecular weight of 2.2 million and a dispersion ratio of 3.9 was obtained (solid content concentration: 30%).
- 0.6 parts by mass of trimethylolpropane tolylene diisocyanate manufactured by Nippon Polyurethane Industry Co., Ltd .: Coronate L
- Gamma-glycidoxypropylmethoxysilane manufactured by Shin-Etsu Chemical Co., Ltd .: KBM-403 was blended to prepare an acrylic pressure-sensitive adhesive (A).
- a solution containing an acrylic polymer (B) having a molecular weight of 1.7 million and a dispersion ratio of 4.1 was obtained (solid content concentration: 30%).
- 0.15 parts by mass of trimethylolpropane xylylene diisocyanate (Mitsui Takeda Pharmaceutical Co., Ltd .: Takeda D110N) and 0.2 parts by mass of trimethylolpropane xylylene diisocyanate per 100 parts by mass of the solid content of the solution containing the acrylic polymer (B).
- An acrylic pressure-sensitive adhesive (B) was prepared by blending a silane coupling agent (manufactured by Soken Kagaku Co., Ltd .: A-100, an acetoacetyl group-containing silane coupling agent).
- Example 1 Preparation of a multilayer pressure-sensitive adhesive layer with a separator consisting of a separator / first pressure-sensitive adhesive layer / second pressure-sensitive adhesive layer / separator>
- a second drying step was performed by sending a wind having a wind speed of 5 m / sec for 60 seconds.
- a third drying step was performed by sending a wind having a wind speed of 20 m / sec for 45 seconds to form a first pressure-sensitive adhesive layer on the separator.
- a second pressure-sensitive adhesive layer was formed on the separator in the same manner. Then, the first pressure-sensitive adhesive layer on the separator and the second pressure-sensitive adhesive layer on the separator are bonded to each other to form a multilayer pressure-sensitive adhesive layer with a separator composed of a separator / first pressure-sensitive adhesive layer / second pressure-sensitive adhesive layer / separator. Made.
- Examples 2-8 Multi-layer adhesive with separator in the same manner as in Example 1 except that the acrylic pressure-sensitive adhesive shown in Table 1, the thicknesses of the first pressure-sensitive adhesive layer and the second pressure-sensitive adhesive layer, and the drying conditions in the drying step were adopted. An agent layer was prepared.
- Comparative Example 1 ⁇ Preparation of a pressure-sensitive adhesive layer with a separator consisting of a separator / pressure-sensitive adhesive layer>
- the first drying step was performed by sending a wind having a wind speed of 8 m / sec for 15 seconds in an oven at 115 ° C.
- a second drying step was performed by sending a wind having a wind speed of 8 m / sec for 60 seconds.
- a third drying step is performed by sending a wind at a wind speed of 20 m / sec for 45 seconds to form an adhesive layer on the separator, and the adhesive having a separator composed of the separator / adhesive layer. Layers were made.
- Comparative Examples 2-4 A pressure-sensitive adhesive layer with a separator was prepared in the same manner as in Comparative Example 1 except that the acrylic pressure-sensitive adhesive shown in Table 1, the thickness of the pressure-sensitive adhesive layer, and the drying conditions in the drying step were adopted.
- the one in which the adhesive surface from which the other separator was peeled off was attached to a special jig was used as a sample. Further, a non-alkali glass plate (1737 manufactured by Corning Inc.) was attached to the adhesive surface of the adhesive layer with a separator prepared in Comparative Examples 1 to 4, and then the separator was peeled off. Then, the one in which the adhesive surface from which the separator was peeled off was attached to a special jig was used as a sample. The non-alkali glass plate used does not affect the ISC-S value.
- a light source, a sample (the light source is on the adhesive side), and a screen were installed in this order, and a transmitted image of the sample projected on the screen was measured by a CCD camera.
- the distance from the light source and the CCD camera to the sample was 30 cm.
- the distance from the light source and the CCD camera to the screen was 100 cm.
- the light source and the CCD camera were installed 20 cm apart so that the distance from the sample and the screen was the same.
- the ISC-S value is related to the evaluation of Sujimura, and if the ISC-S value is 50 or less, it can be determined that the unevenness can be controlled to be small.
- the produced adhesive optical film with a separator was cut into a size of 50 mm ⁇ 100 mm to prepare a measurement sample.
- the measurement sample was attached to a flat plate-shaped peeling jig via a double-sided tape with the optical film side facing down.
- the separator and the pressure-sensitive adhesive layer were peeled off from the short side of the measurement sample, the separator was chucked, pulled by a tensile tester, and the peeling force (N / 50 mm) was measured (tensile direction: optical film). 180 ° to the surface, tensile speed: 300 mm / min).
- the peeling force was measured for five measuring samples, and the average value of the measured values of each measuring sample was adopted as the separator peeling force (N / 50 mm).
- the multi-layered pressure-sensitive adhesive layer of the multi-layered pressure-sensitive adhesive layer with a separator produced in Examples 1 to 8 has an ISC-S value of 50 or less even though it is thickened, and has high visibility. It can be seen that the affecting surface unevenness is suppressed.
- the pressure-sensitive adhesive layers with separators produced in Comparative Examples 1 to 4 are thickened, but the ISC-S value greatly exceeds 50, and many surface irregularities that affect visibility occur. I understand.
- the multi-layered pressure-sensitive adhesive layer of the present invention is useful as a constituent member of an image display device such as a liquid crystal display device (LCD), an organic EL display device, a CRT, and a PDP.
- LCD liquid crystal display device
- organic EL display device a CRT
- PDP PDP
- Polarizing film Protective film 3 Phase difference layer 6 Transparent conductive layer 8 Transparent base material 10
- Organic EL display panel 10-1
- Organic EL display panel (with touch sensor) 11
- Adhesive optical film for flexible image display device Adhesive optical film for organic EL display device
- 12-1 First Multilayer Adhesive Layer 12-2
- Second Multilayer Adhesive Layer 12-3
- Third Multilayer Adhesive Layer 13
- Decorative Printing Film 20
- Optical Laminate 40 Window 100 Flexible Image Display Device ( Organic EL display device)
Abstract
A purpose of the present invention is to provide a multilayered pressure-sensitive adhesive layer which has an increased thickness and, despite this, is reduced in surface unevenness which may affect visibility. This multilayered pressure-sensitive adhesive layer comprises two or more pressure-sensitive adhesive layers directly superposed on each other and has a total thickness of 20-100 μm and an ISC-S value of 50 or less. The pressure sensitive adhesive layers each have a thickness of 10-20 μm.
Description
本発明は、２層以上の粘着剤層が直接積層されている多層化粘着剤層、前記多層化粘着剤層の片面又は両面にセパレータを有するセパレータ付き多層化粘着剤層及びその製造方法、前記多層化粘着剤層と、光学フィルムとを有する粘着型光学フィルム、前記セパレータ付き多層化粘着剤層と、光学フィルムとを有するセパレータ付き粘着型光学フィルム及びその製造方法、並びに画像表示装置に関する。画像表示装置としては、液晶表示装置（ＬＣＤ）、有機ＥＬ表示装置、ＣＲＴ、及びＰＤＰなどが挙げられる。
The present invention relates to a multi-layered pressure-sensitive adhesive layer in which two or more pressure-sensitive adhesive layers are directly laminated, a multi-layered pressure-sensitive adhesive layer having a separator on one or both sides of the multi-layered pressure-sensitive adhesive layer, and a method for producing the same. The present invention relates to an adhesive optical film having a multilayer pressure-sensitive adhesive layer and an optical film, an adhesive-type optical film with a separator having the separator-attached multilayer pressure-sensitive adhesive layer and an optical film, a method for producing the same, and an image display device. Examples of the image display device include a liquid crystal display device (LCD), an organic EL display device, a CRT, and a PDP.
液晶表示装置および有機ＥＬ表示装置等は、その画像形成方式から、例えば、液晶表示装置では、液晶セルの両側に偏光素子を配置することが必要不可欠であり、一般的には偏光フィルムが貼着されている。また液晶パネルおよび有機ＥＬパネル等の表示パネルには偏光フィルムの他に、ディスプレイの表示品位を向上させるために様々な光学素子が用いられている。また、液晶表示装置、有機ＥＬ表示装置、ＣＲＴ、及びＰＤＰ等の画像表示装置を保護したり、高級感を付与したり、デザインを差別化するために前面板が使用されている。これら液晶表示装置および有機ＥＬ表示装置等の画像表示装置や、前面板などの画像表示装置と共に使用される部材には、例えば、着色防止としての位相差板、液晶ディスプレイの視野角を改善するための視野角拡大フィルム、さらにはディスプレイのコントラストを高めるための輝度向上フィルム、表面の耐擦傷性を付与するために用いられるハードコートフィルム、画像表示装置に対する写り込みを防止するためのアンチグレア処理フィルム、アンチリフレクティブフィルム、及びローリフレクティブフィルムなどの反射防止フィルム等の表面処理フィルムが用いられている。これらのフィルムは総称して光学フィルムと呼ばれる。
Due to the image forming method of a liquid crystal display device, an organic EL display device, or the like, for example, in a liquid crystal display device, it is indispensable to arrange polarizing elements on both sides of the liquid crystal cell, and generally, a polarizing film is attached. Has been done. Further, in addition to the polarizing film, various optical elements are used for the display panel such as the liquid crystal panel and the organic EL panel in order to improve the display quality of the display. Further, a front plate is used to protect an image display device such as a liquid crystal display device, an organic EL display device, a CRT, and a PDP, to give a sense of quality, and to differentiate a design. The members used together with the image display device such as the liquid crystal display device and the organic EL display device and the image display device such as the front plate include, for example, a retardation plate for preventing coloring and a viewing angle of the liquid crystal display. A film that expands the viewing angle of the display, a brightness-enhancing film that enhances the contrast of the display, a hard coat film that is used to impart scratch resistance to the surface, and an anti-glare treatment film that prevents reflection on an image display device. Surface-treated films such as anti-reflective films and anti-reflection films such as low-reflective films are used. These films are collectively called optical films.
光学フィルムのムラ等に起因する視認性の低下は、品質課題の一つであり、その改善が求められている。また、光学フィルムを作製する際に発生するムラだけでなく、光学フィルム同士を貼り合わせるため、又は光学フィルムを表示パネルへ貼り合わせるために用いられる粘着剤層や接着剤層の表面ムラも視認性に影響を与えるため、その対策が必要となってきている。
Deterioration of visibility due to unevenness of the optical film is one of the quality issues, and improvement is required. In addition to the unevenness that occurs when manufacturing an optical film, the surface unevenness of the pressure-sensitive adhesive layer and the adhesive layer used for bonding the optical films to each other or for bonding the optical films to the display panel is also visible. Therefore, it is necessary to take measures against it.
例えば、特許文献１では、粘着剤層に基づく視認性に係るムラの問題を低減することを目的として、光学フィルムと、前記光学フィルムに設けられた粘着剤層を有する粘着型光学フィルムであって、前記粘着剤層は、厚み（μｍ）の標準偏差値が０．１２μｍ以下であることを特徴とする粘着型光学フィルムが提案されている。
For example, in Patent Document 1, an adhesive type optical film having an optical film and an adhesive layer provided on the optical film for the purpose of reducing the problem of unevenness related to visibility based on the adhesive layer. As the pressure-sensitive adhesive layer, a pressure-sensitive optical film having a thickness (μm) standard deviation value of 0.12 μm or less has been proposed.
一方、近年、フレキシブルパネルの耐久性を向上させるために粘着剤層は厚手化されているが、粘着剤層を厚手化すると表面ムラが生じやすくなるという問題があった。
On the other hand, in recent years, the adhesive layer has been thickened in order to improve the durability of the flexible panel, but there is a problem that the thickening of the adhesive layer tends to cause surface unevenness.
本発明は、上記課題を解決したものであり、厚手化されているにもかかわらず、視認性に影響を与える表面ムラが抑制された多層化粘着剤層を提供することを目的とする。また、本発明は、前記多層化粘着剤層の片面又は両面にセパレータを有するセパレータ付き多層化粘着剤層及びその製造方法、前記多層化粘着剤層と、光学フィルムとを有する粘着型光学フィルム、前記セパレータ付き多層化粘着剤層と、光学フィルムとを有するセパレータ付き粘着型光学フィルム及びその製造方法、並びにこれらを有する画像表示装置を提供することを目的とする。
The present invention solves the above-mentioned problems, and an object of the present invention is to provide a multi-layered pressure-sensitive adhesive layer in which surface unevenness that affects visibility is suppressed even though the thickness is increased. Further, the present invention relates to a multi-layered pressure-sensitive adhesive layer having a separator on one side or both sides of the multi-layered pressure-sensitive adhesive layer and a method for producing the same, an adhesive optical film having the multi-layered pressure-sensitive adhesive layer and an optical film. It is an object of the present invention to provide an adhesive optical film with a separator having the multilayer pressure-sensitive adhesive layer with a separator and an optical film, a method for producing the same, and an image display device having the same.
本発明者らは前記課題を解決すべく鋭意検討を重ねた結果、下記の多層化粘着剤層等により上記課題を解決できることを見出し、本発明を完成するに至った。
As a result of diligent studies to solve the above problems, the present inventors have found that the above problems can be solved by the following multi-layered pressure-sensitive adhesive layer and the like, and have completed the present invention.
即ち本発明は、２層以上の粘着剤層が直接積層されている多層化粘着剤層であって、
前記粘着剤層は、それぞれ厚みが１０～２０μｍであり、
前記多層化粘着剤層は、総厚みが２０～１００μｍであり、かつ
前記多層化粘着剤層は、ＩＳＣ－Ｓ値が５０以下であることを特徴とする多層化粘着剤層、に関する。 That is, the present invention is a multi-layered pressure-sensitive adhesive layer in which two or more pressure-sensitive adhesive layers are directly laminated.
Each of the pressure-sensitive adhesive layers has a thickness of 10 to 20 μm, and has a thickness of 10 to 20 μm.
The multi-layered pressure-sensitive adhesive layer has a total thickness of 20 to 100 μm, and the multi-layered pressure-sensitive adhesive layer relates to a multi-layered pressure-sensitive adhesive layer having an ISC-S value of 50 or less.
前記粘着剤層は、それぞれ厚みが１０～２０μｍであり、
前記多層化粘着剤層は、総厚みが２０～１００μｍであり、かつ
前記多層化粘着剤層は、ＩＳＣ－Ｓ値が５０以下であることを特徴とする多層化粘着剤層、に関する。 That is, the present invention is a multi-layered pressure-sensitive adhesive layer in which two or more pressure-sensitive adhesive layers are directly laminated.
Each of the pressure-sensitive adhesive layers has a thickness of 10 to 20 μm, and has a thickness of 10 to 20 μm.
The multi-layered pressure-sensitive adhesive layer has a total thickness of 20 to 100 μm, and the multi-layered pressure-sensitive adhesive layer relates to a multi-layered pressure-sensitive adhesive layer having an ISC-S value of 50 or less.
前記多層化粘着剤層は、少なくとも直接積層されている第１粘着剤層と第２粘着剤層を含み、
前記第１粘着剤層の形成材料である粘着剤組成物は、（メタ）アクリル系ポリマーＡを含み、
前記第２粘着剤層の形成材料である粘着剤組成物は、（メタ）アクリル系ポリマーＢを含み、
前記（メタ）アクリル系ポリマーＡの形成材料であるモノマー組成物と前記（メタ）アクリル系ポリマーＢの形成材料であるモノマー組成物は、炭素数１～１８のアルキル基を有するアルキル（メタ）アクリレートを５０質量％以上含むことが好ましい。 The multilayered pressure-sensitive adhesive layer includes at least a first pressure-sensitive adhesive layer and a second pressure-sensitive adhesive layer that are directly laminated.
The pressure-sensitive adhesive composition, which is a material for forming the first pressure-sensitive adhesive layer, contains a (meth) acrylic polymer A and contains.
The pressure-sensitive adhesive composition, which is a material for forming the second pressure-sensitive adhesive layer, contains a (meth) acrylic polymer B and contains.
The monomer composition which is the material for forming the (meth) acrylic polymer A and the monomer composition which is the material for forming the (meth) acrylic polymer B are alkyl (meth) acrylates having an alkyl group having 1 to 18 carbon atoms. Is preferably contained in an amount of 50% by mass or more.
前記第１粘着剤層の形成材料である粘着剤組成物は、（メタ）アクリル系ポリマーＡを含み、
前記第２粘着剤層の形成材料である粘着剤組成物は、（メタ）アクリル系ポリマーＢを含み、
前記（メタ）アクリル系ポリマーＡの形成材料であるモノマー組成物と前記（メタ）アクリル系ポリマーＢの形成材料であるモノマー組成物は、炭素数１～１８のアルキル基を有するアルキル（メタ）アクリレートを５０質量％以上含むことが好ましい。 The multilayered pressure-sensitive adhesive layer includes at least a first pressure-sensitive adhesive layer and a second pressure-sensitive adhesive layer that are directly laminated.
The pressure-sensitive adhesive composition, which is a material for forming the first pressure-sensitive adhesive layer, contains a (meth) acrylic polymer A and contains.
The pressure-sensitive adhesive composition, which is a material for forming the second pressure-sensitive adhesive layer, contains a (meth) acrylic polymer B and contains.
The monomer composition which is the material for forming the (meth) acrylic polymer A and the monomer composition which is the material for forming the (meth) acrylic polymer B are alkyl (meth) acrylates having an alkyl group having 1 to 18 carbon atoms. Is preferably contained in an amount of 50% by mass or more.
さらに、前記（メタ）アクリル系ポリマーＡの形成材料であるモノマー組成物と前記（メタ）アクリル系ポリマーＢの形成材料であるモノマー組成物は、同じアルキル（メタ）アクリレートを５０質量％以上含むことが好ましい。
Further, the monomer composition which is the material for forming the (meth) acrylic polymer A and the monomer composition which is the material for forming the (meth) acrylic polymer B contain 50% by mass or more of the same alkyl (meth) acrylate. Is preferable.
また、前記多層化粘着剤層は、有機ＥＬ表示装置用多層化粘着剤層であることが好ましい。
Further, the multi-layered pressure-sensitive adhesive layer is preferably a multi-layered pressure-sensitive adhesive layer for an organic EL display device.
また本発明は、前記多層化粘着剤層の片面又は両面にセパレータを有するセパレータ付き多層化粘着剤層、に関する。
The present invention also relates to a multi-layered pressure-sensitive adhesive layer with a separator having separators on one side or both sides of the multi-layered pressure-sensitive adhesive layer.
前記セパレータ付き多層化粘着剤層は、引張速度３００ｍｍ／分、剥離角度１８０度の条件で測定されるセパレータ剥離力が０．１５Ｎ／５０ｍｍ以下であることが好ましい。
The multilayer pressure-sensitive adhesive layer with a separator preferably has a separator peeling force of 0.15 N / 50 mm or less measured under the conditions of a tensile speed of 300 mm / min and a peeling angle of 180 degrees.
また本発明は、前記多層化粘着剤層と、光学フィルムとを有する粘着型光学フィルム、に関する。
The present invention also relates to an adhesive type optical film having the multi-layered pressure-sensitive adhesive layer and an optical film.
また、前記粘着型光学フィルムは、フレキシブル画像表示装置用粘着型光学フィルムであることが好ましい。
Further, the adhesive optical film is preferably an adhesive optical film for a flexible image display device.
また本発明は、前記セパレータ付き多層化粘着剤層と、光学フィルムとを有するセパレータ付き粘着型光学フィルム、に関する。
The present invention also relates to an adhesive optical film with a separator having the multilayer adhesive layer with a separator and an optical film.
また本発明は、前記多層化粘着剤層、又は前記粘着型光学フィルムを有する画像表示装置、に関する。
The present invention also relates to the multilayer pressure-sensitive adhesive layer or an image display device having the pressure-sensitive optical film.
また本発明は、セパレータ上に粘着剤組成物を塗布する工程、及び温度３０～１０５℃、風速０．５～７ｍ／秒、及び乾燥時間５～３０秒間の条件で塗布した粘着剤組成物を乾燥する第１乾燥工程、前記第１乾燥工程後、温度３０～８５℃、風速０．５～７ｍ／秒、及び乾燥時間１０～１２０秒間の条件で塗布した粘着剤組成物を乾燥する第２乾燥工程、前記第２乾燥工程後、温度９０～１６０℃、風速０．１～２５ｍ／秒、及び乾燥時間１０～１８０秒間の条件で塗布した粘着剤組成物を乾燥する第３乾燥工程を含む乾燥工程により、セパレータ上に粘着剤層を形成する工程、
さらに、前記粘着剤層上に別の粘着剤組成物を塗布する工程、及び前記乾燥工程を繰り返し行うことにより、前記粘着剤層上に別の粘着剤層を順次積層する工程を含む、前記セパレータ付き多層化粘着剤層の製造方法、に関する。 Further, the present invention relates to a step of applying a pressure-sensitive adhesive composition on a separator, and a pressure-sensitive adhesive composition applied under conditions of a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 to 30 seconds. After the first drying step of drying and the first drying step, the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 85 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 10 to 120 seconds is dried. The drying step includes a third drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds after the second drying step. A step of forming an adhesive layer on a separator by a drying step,
Further, the separator comprising a step of applying another pressure-sensitive adhesive composition on the pressure-sensitive adhesive layer and a step of sequentially laminating another pressure-sensitive adhesive layer on the pressure-sensitive adhesive layer by repeating the drying step. With respect to a method of manufacturing a multi-layer adhesive layer.
さらに、前記粘着剤層上に別の粘着剤組成物を塗布する工程、及び前記乾燥工程を繰り返し行うことにより、前記粘着剤層上に別の粘着剤層を順次積層する工程を含む、前記セパレータ付き多層化粘着剤層の製造方法、に関する。 Further, the present invention relates to a step of applying a pressure-sensitive adhesive composition on a separator, and a pressure-sensitive adhesive composition applied under conditions of a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 to 30 seconds. After the first drying step of drying and the first drying step, the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 85 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 10 to 120 seconds is dried. The drying step includes a third drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds after the second drying step. A step of forming an adhesive layer on a separator by a drying step,
Further, the separator comprising a step of applying another pressure-sensitive adhesive composition on the pressure-sensitive adhesive layer and a step of sequentially laminating another pressure-sensitive adhesive layer on the pressure-sensitive adhesive layer by repeating the drying step. With respect to a method of manufacturing a multi-layer adhesive layer.
また本発明は、一方のセパレータ上に粘着剤組成物を塗布する工程、及び温度３０～１０５℃、風速０．５～７ｍ／秒、及び乾燥時間５～３０秒間の条件で塗布した粘着剤組成物を乾燥する第１乾燥工程、前記第１乾燥工程後、温度３０～８５℃、風速０．５～７ｍ／秒、及び乾燥時間１０～１２０秒間の条件で塗布した粘着剤組成物を乾燥する第２乾燥工程、前記第２乾燥工程後、温度９０～１６０℃、風速０．１～２５ｍ／秒、及び乾燥時間１０～１８０秒間の条件で塗布した粘着剤組成物を乾燥する第３乾燥工程を含む乾燥工程を少なくとも１回行うことにより、一方のセパレータ上に粘着剤層を１層以上形成する工程、
他方のセパレータ上に粘着剤組成物を塗布する工程、及び前記乾燥工程を少なくとも１回行うことにより、他方のセパレータ上に粘着剤層を１層以上形成する工程、
さらに、前記一方のセパレータ上の粘着剤層と前記他方のセパレータ上の粘着剤層とを積層する工程を含む、前記セパレータ付き多層化粘着剤層の製造方法、に関する。 Further, in the present invention, the pressure-sensitive adhesive composition is applied under the conditions of a step of applying the pressure-sensitive adhesive composition on one separator, a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 to 30 seconds. After the first drying step of drying the product, the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 85 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 10 to 120 seconds is dried. A second drying step, after the second drying step, a third drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds. A step of forming one or more pressure-sensitive adhesive layers on one of the separators by performing the drying step including at least once.
A step of applying the pressure-sensitive adhesive composition on the other separator and a step of forming one or more pressure-sensitive adhesive layers on the other separator by performing the drying step at least once.
Further, the present invention relates to a method for producing a multilayer pressure-sensitive adhesive layer with a separator, which comprises a step of laminating a pressure-sensitive adhesive layer on the one separator and a pressure-sensitive adhesive layer on the other separator.
他方のセパレータ上に粘着剤組成物を塗布する工程、及び前記乾燥工程を少なくとも１回行うことにより、他方のセパレータ上に粘着剤層を１層以上形成する工程、
さらに、前記一方のセパレータ上の粘着剤層と前記他方のセパレータ上の粘着剤層とを積層する工程を含む、前記セパレータ付き多層化粘着剤層の製造方法、に関する。 Further, in the present invention, the pressure-sensitive adhesive composition is applied under the conditions of a step of applying the pressure-sensitive adhesive composition on one separator, a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 to 30 seconds. After the first drying step of drying the product, the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 85 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 10 to 120 seconds is dried. A second drying step, after the second drying step, a third drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds. A step of forming one or more pressure-sensitive adhesive layers on one of the separators by performing the drying step including at least once.
A step of applying the pressure-sensitive adhesive composition on the other separator and a step of forming one or more pressure-sensitive adhesive layers on the other separator by performing the drying step at least once.
Further, the present invention relates to a method for producing a multilayer pressure-sensitive adhesive layer with a separator, which comprises a step of laminating a pressure-sensitive adhesive layer on the one separator and a pressure-sensitive adhesive layer on the other separator.
また本発明は、一方のセパレータ上に粘着剤組成物を塗布する工程、及び温度３０～１０５℃、風速０．５～７ｍ／秒、及び乾燥時間５～３０秒間の条件で塗布した粘着剤組成物を乾燥する第１乾燥工程、前記第１乾燥工程後、温度３０～８５℃、風速０．５～７ｍ／秒、及び乾燥時間１０～１２０秒間の条件で塗布した粘着剤組成物を乾燥する第２乾燥工程、前記第２乾燥工程後、温度９０～１６０℃、風速０．１～２５ｍ／秒、及び乾燥時間１０～１８０秒間の条件で塗布した粘着剤組成物を乾燥する第３乾燥工程を含む乾燥工程を少なくとも１回行うことにより、一方のセパレータ上に粘着剤層を１層以上形成する工程、
前記粘着剤層の前記セパレータを有しない面に光学フィルムを積層し、前記セパレータを剥離する工程、
他方のセパレータ上に粘着剤組成物を塗布する工程、及び前記乾燥工程を少なくとも１回行うことにより、他方のセパレータ上に粘着剤層を１層以上形成する工程、
さらに、前記光学フィルム上の粘着剤層と前記他方のセパレータ上の粘着剤層とを積層する工程を含む、前記セパレータ付き粘着型光学フィルムの製造方法、に関する。 Further, in the present invention, the pressure-sensitive adhesive composition is applied under the conditions of a step of applying the pressure-sensitive adhesive composition on one separator, a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 to 30 seconds. After the first drying step of drying the product, the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 85 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 10 to 120 seconds is dried. A second drying step, after the second drying step, a third drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds. A step of forming one or more pressure-sensitive adhesive layers on one of the separators by performing the drying step including at least once.
A step of laminating an optical film on a surface of the pressure-sensitive adhesive layer that does not have the separator and peeling the separator.
A step of applying the pressure-sensitive adhesive composition on the other separator and a step of forming one or more pressure-sensitive adhesive layers on the other separator by performing the drying step at least once.
Further, the present invention relates to a method for producing an adhesive optical film with a separator, which comprises a step of laminating an adhesive layer on the optical film and an adhesive layer on the other separator.
前記粘着剤層の前記セパレータを有しない面に光学フィルムを積層し、前記セパレータを剥離する工程、
他方のセパレータ上に粘着剤組成物を塗布する工程、及び前記乾燥工程を少なくとも１回行うことにより、他方のセパレータ上に粘着剤層を１層以上形成する工程、
さらに、前記光学フィルム上の粘着剤層と前記他方のセパレータ上の粘着剤層とを積層する工程を含む、前記セパレータ付き粘着型光学フィルムの製造方法、に関する。 Further, in the present invention, the pressure-sensitive adhesive composition is applied under the conditions of a step of applying the pressure-sensitive adhesive composition on one separator, a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 to 30 seconds. After the first drying step of drying the product, the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 85 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 10 to 120 seconds is dried. A second drying step, after the second drying step, a third drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds. A step of forming one or more pressure-sensitive adhesive layers on one of the separators by performing the drying step including at least once.
A step of laminating an optical film on a surface of the pressure-sensitive adhesive layer that does not have the separator and peeling the separator.
A step of applying the pressure-sensitive adhesive composition on the other separator and a step of forming one or more pressure-sensitive adhesive layers on the other separator by performing the drying step at least once.
Further, the present invention relates to a method for producing an adhesive optical film with a separator, which comprises a step of laminating an adhesive layer on the optical film and an adhesive layer on the other separator.
本発明の多層化粘着剤層は、厚みが小さい粘着剤層を複数積層することにより、各粘着剤層の表面ムラを抑制して粘着剤層全体の表面ムラを抑制しつつ、厚手化を達成したものである。各粘着剤層の厚みを小さくすることにより、各粘着剤層の表面ムラが抑制された理由は定かではないが、以下のように考えられる。粘着剤層は、通常、粘着剤組成物をセパレータ等の基材上に塗布し、乾燥等することにより硬化（固化）して形成されるが、粘着剤組成物の塗布膜の厚みが厚い場合には、乾燥時に粘着剤組成物中の溶剤の流動性が大きくなったり、乾燥時の熱風によって塗布膜の表面が波打ちやすくなることにより、表面ムラが生じやすくなると考えられる。一方、粘着剤組成物の塗布膜の厚みが薄い場合には、乾燥時に粘着剤組成物中の溶剤の流動性が小さくなり、乾燥時の熱風によって塗布膜の表面が波打ちにくくなるため、表面ムラが生じにくくなると考えられる。
The multi-layered pressure-sensitive adhesive layer of the present invention achieves thickening while suppressing surface unevenness of each pressure-sensitive adhesive layer and suppressing surface unevenness of the entire pressure-sensitive adhesive layer by laminating a plurality of pressure-sensitive adhesive layers having a small thickness. It was done. The reason why the surface unevenness of each pressure-sensitive adhesive layer is suppressed by reducing the thickness of each pressure-sensitive adhesive layer is not clear, but it is considered as follows. The pressure-sensitive adhesive layer is usually formed by applying the pressure-sensitive adhesive composition on a base material such as a separator and drying (solidifying) the pressure-sensitive adhesive layer. However, when the coating film of the pressure-sensitive adhesive composition is thick. It is considered that surface unevenness is likely to occur because the fluidity of the solvent in the pressure-sensitive adhesive composition increases during drying and the surface of the coating film tends to undulate due to hot air during drying. On the other hand, when the coating film of the pressure-sensitive adhesive composition is thin, the fluidity of the solvent in the pressure-sensitive adhesive composition becomes small during drying, and the surface of the coating film is less likely to undulate due to hot air during drying, resulting in surface unevenness. Is considered to be less likely to occur.
また、本発明の多層化粘着剤層は、総厚みが２０～１００μｍであり、フレキシブルパネルの耐久性を向上させるための十分な厚みを有するにもかかわらず、筋ムラ率を表すＩＳＣ－Ｓ値が５０以下であり、視認性に影響を与える表面ムラが非常に抑制されたものである。
Further, the multi-layered pressure-sensitive adhesive layer of the present invention has a total thickness of 20 to 100 μm, and although it has a sufficient thickness for improving the durability of the flexible panel, the ISC-S value indicating the streak unevenness ratio is exhibited. Is 50 or less, and surface unevenness that affects visibility is greatly suppressed.
＜多層化粘着剤層＞
本発明の多層化粘着剤層は、２層以上の粘着剤層が直接積層されており、総厚みが２０～１００μｍであり、かつＩＳＣ－Ｓ値が５０以下である。そして、前記粘着剤層は、それぞれ厚みが１０～２０μｍである。 <Multi-layer adhesive layer>
The multi-layered pressure-sensitive adhesive layer of the present invention has two or more pressure-sensitive adhesive layers directly laminated, has a total thickness of 20 to 100 μm, and has an ISC-S value of 50 or less. The thickness of each of the pressure-sensitive adhesive layers is 10 to 20 μm.
本発明の多層化粘着剤層は、２層以上の粘着剤層が直接積層されており、総厚みが２０～１００μｍであり、かつＩＳＣ－Ｓ値が５０以下である。そして、前記粘着剤層は、それぞれ厚みが１０～２０μｍである。 <Multi-layer adhesive layer>
The multi-layered pressure-sensitive adhesive layer of the present invention has two or more pressure-sensitive adhesive layers directly laminated, has a total thickness of 20 to 100 μm, and has an ISC-S value of 50 or less. The thickness of each of the pressure-sensitive adhesive layers is 10 to 20 μm.
本発明の多層化粘着剤層を形成する粘着剤（粘着剤組成物)としては、例えば、アクリル系粘着剤、ゴム系粘着剤、ビニルアルキルエーテル系粘着剤、シリコーン系粘着剤、ポリエステル系粘着剤、ポリアミド系粘着剤、ウレタン系粘着剤、フッ素系粘着剤、エポキシ系粘着剤、ポリエーテル系粘着剤などが挙げられる。なお、前記各粘着剤層を構成する粘着剤は、同種の粘着剤であってもよく、異種の粘着剤であってもよいが、粘着剤層同士の密着性を向上させる観点から同種の粘着剤であることが好ましい。また、透明性、加工性、耐久性、密着性、耐屈曲性などの点から、（メタ）アクリル系ポリマーを含有するアクリル系粘着剤を用いることが好ましい。
Examples of the adhesive (adhesive composition) forming the multi-layer adhesive layer of the present invention include acrylic adhesive, rubber adhesive, vinyl alkyl ether adhesive, silicone adhesive, and polyester adhesive. , Polyamide-based pressure-sensitive adhesive, urethane-based pressure-sensitive adhesive, fluorine-based pressure-sensitive adhesive, epoxy-based pressure-sensitive adhesive, polyether-based pressure-sensitive adhesive, and the like. The pressure-sensitive adhesives constituting the respective pressure-sensitive adhesive layers may be the same type of pressure-sensitive adhesives or different types of pressure-sensitive adhesives, but the same type of pressure-sensitive adhesives may be used from the viewpoint of improving the adhesion between the pressure-sensitive adhesive layers. It is preferably an agent. Further, from the viewpoints of transparency, processability, durability, adhesion, bending resistance and the like, it is preferable to use an acrylic pressure-sensitive adhesive containing a (meth) acrylic polymer.
アクリル系粘着剤は、アルキル（メタ）アクリレートのモノマーユニットを主骨格とする（メタ）アクリル系ポリマーをベースポリマーとする。なお、（メタ）アクリレートはアクリレートおよび／またはメタクリレートをいい、本発明の（メタ）とは同様の意味である。（メタ）アクリル系ポリマーの主骨格を構成する、アルキル（メタ）アクリレートのアルキル基の炭素数は１～１４程度であり、アルキル（メタ）アクリレートの具体例としては、メチル（メタ）アクリレート、エチル（メタ）アクリレート、プロピル（メタ）アクリレート、イソプロピル（メタ）アクリレート、ｎ－ブチル（メタ）アクリレート、イソブチル（メタ）アクリレート、ペンチル（メタ）アクリレート、ヘキシル（メタ）アクリレート、２－エチルヘキシル（メタ）アクリレート、オクチル（メタ）アクリレート、イソオクチル（メタ）アクリレート、ノニル（メタ）アクリレート、イソノニル（メタ）アクリレート、デシル（メタ）アクリレート、ドデシル（メタ）アクリレート、ステアリル（メタ）アクリレート、等を例示でき、これらは単独または組み合わせて使用できる。これらの中でも炭素数１～１８のアルキル基を有するアルキル（メタ）アクリレートが好ましく、より好ましくは炭素数１～９のアルキル基を有するアルキル（メタ）アクリレートである。
The acrylic pressure-sensitive adhesive uses a (meth) acrylic polymer having an alkyl (meth) acrylate monomer unit as the main skeleton as a base polymer. In addition, (meth) acrylate means acrylate and / or methacrylate, and has the same meaning as (meth) of the present invention. The alkyl group of the alkyl (meth) acrylate, which constitutes the main skeleton of the (meth) acrylic polymer, has about 1 to 14 carbon atoms. Specific examples of the alkyl (meth) acrylate include methyl (meth) acrylate and ethyl. (Meta) acrylate, propyl (meth) acrylate, isopropyl (meth) acrylate, n-butyl (meth) acrylate, isobutyl (meth) acrylate, pentyl (meth) acrylate, hexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate , Octyl (meth) acrylate, isooctyl (meth) acrylate, nonyl (meth) acrylate, isononyl (meth) acrylate, decyl (meth) acrylate, dodecyl (meth) acrylate, stearyl (meth) acrylate, etc. Can be used alone or in combination. Among these, an alkyl (meth) acrylate having an alkyl group having 1 to 18 carbon atoms is preferable, and an alkyl (meth) acrylate having an alkyl group having 1 to 9 carbon atoms is more preferable.
前記（メタ）アクリル系ポリマー中には、接着性や耐熱性の改善を目的に、１種類以上の各種モノマーを共重合により導入することができる。そのような共重合モノマーの具体例としては、カルボキシ基含有モノマー、水酸基含有モノマー、窒素含有モノマー（複素環含有モノマーを含む）、芳香族含有モノマー等があげられる。
In the (meth) acrylic polymer, one or more kinds of various monomers can be introduced by copolymerization for the purpose of improving adhesiveness and heat resistance. Specific examples of such a copolymerization monomer include a carboxy group-containing monomer, a hydroxyl group-containing monomer, a nitrogen-containing monomer (including a heterocyclic ring-containing monomer), an aromatic-containing monomer, and the like.
カルボキシ基含有モノマーとしては、例えば、アクリル酸、メタクリル酸、カルボキシエチル（メタ）アクリレート、カルボキシペンチル（メタ）アクリレート、イタコン酸、マレイン酸、フマール酸、クロトン酸などがあげられる。これらのなかでもアクリル酸、メタクリル酸が好ましい。
Examples of the carboxy group-containing monomer include acrylic acid, methacrylic acid, carboxyethyl (meth) acrylate, carboxypentyl (meth) acrylate, itaconic acid, maleic acid, fumaric acid, and crotonic acid. Of these, acrylic acid and methacrylic acid are preferable.
水酸基含有モノマーとしては、２－ヒドロキシエチル(メタ)アクリレート、２－ヒドロキシプロピル(メタ)アクリレート、４－ヒドロキシブチル(メタ)アクリレート、６－ヒドロキシヘキシル(メタ)アクリレート、８－ヒドロキシオクチル(メタ)アクリレート、１０－ヒドロキシデシル(メタ)アクリレート、１２－ヒドロキシラウリル(メタ)アクリレートや（４－ヒドロキシメチルシクロヘキシル)－メチルアクリレートなどがあげられる。
Examples of the hydroxyl group-containing monomer include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, 6-hydroxyhexyl (meth) acrylate, and 8-hydroxyoctyl (meth) acrylate. Examples thereof include 10-hydroxydecyl (meth) acrylate, 12-hydroxylauryl (meth) acrylate and (4-hydroxymethylcyclohexyl) -methyl acrylate.
窒素含有モノマーとしては、例えば、マレイミド、Ｎ－シクロへキシルマレイミド、Ｎ－フェニルマレイミド；Ｎ－アクリロイルモルホリン；（メタ）アクリルアミド、Ｎ，Ｎ－ジメチル（メタ）アクリルアミド、Ｎ，Ｎ－ジエチル（メタ）アクリルアミド、Ｎ－ヘキシル（メタ）アクリルアミド、Ｎ－メチル（メタ）アクリルアミド、Ｎ－ブチル（メタ）アクリルアミド、Ｎ－ブチル（メタ）アクリルアミドやＮ－メチロール（メタ）アクリルアミド、Ｎ－メチロールプロパン（メタ）アクリルアミドなどの（Ｎ－置換）アミド系モノマー；（メタ）アクリル酸アミノエチル、（メタ）アクリル酸アミノプロピル、（メタ）アクリル酸Ｎ，Ｎ－ジメチルアミノエチル、（メタ）アクリル酸ｔ－ブチルアミノエチル、３－（３－ピリニジル）プロピル（メタ）アクリレートなどの（メタ）アクリル酸アルキルアミノアルキル系モノマー；（メタ）アクリル酸メトキシエチル、（メタ）アクリル酸エトキシエチルなどの（メタ）アクリル酸アルコキシアルキル系モノマー；Ｎ－（メタ）アクリロイルオキシメチレンスクシンイミドやＮ－（メタ）アクリロイル－６－オキシヘキサメチレンスクシンイミド、Ｎ－（メタ）アクリロイル－８－オキシオクタメチレンスクシンイミド、Ｎ－アクリロイルモルホリンなどのスクシンイミド系モノマーなども改質目的のモノマー例としてあげられる。
Examples of nitrogen-containing monomers include maleimide, N-cyclohexyl maleimide, N-phenylmaleimide; N-acryloylmorpholin; (meth) acrylamide, N, N-dimethyl (meth) acrylamide, N, N-diethyl (meth). Acrylamide, N-hexyl (meth) acrylamide, N-methyl (meth) acrylamide, N-butyl (meth) acrylamide, N-butyl (meth) acrylamide, N-methylol (meth) acrylamide, N-methylol propane (meth) acrylamide (N-substituted) amide-based monomers such as (meth) aminoethyl acrylate, aminopropyl (meth) acrylate, N, N-dimethylaminoethyl (meth) acrylate, t-butylaminoethyl (meth) acrylate. Alkylaminoalkyl (meth) acrylate monomers such as 3- (3-pyrinidyl) propyl (meth) acrylate; alkoxyalkyl (meth) acrylate such as methoxyethyl (meth) acrylate, ethoxyethyl (meth) acrylate System monomers: Succinimide-based monomers such as N- (meth) acryloyloxymethylene succinimide, N- (meth) acryloyl-6-oxyhexamethylene succinimide, N- (meth) acryloyl-8-oxyoctamethylene succinimide, and N-acryloylmorpholin. Is also given as an example of a monomer for the purpose of modification.
芳香族含有モノマーとしては、例えば、ベンジル（メタ）アクリレート、フェニル（メタ）アクリレート、フェノキシエチル（メタ）アクリレート等があげられる。
Examples of the aromatic-containing monomer include benzyl (meth) acrylate, phenyl (meth) acrylate, and phenoxyethyl (meth) acrylate.
上記モノマーの他に、無水マレイン酸、無水イタコン酸などの酸無水物基含有モノマー；アクリル酸のカプロラクトン付加物；スチレンスルホン酸やアリルスルホン酸、２－（メタ）アクリルアミド－２－メチルプロパンスルホン酸、（メタ）アクリルアミドプロパンスルホン酸、スルホプロピル（メタ）アクリレート、（メタ）アクリロイルオキシナフタレンスルホン酸などのスルホン酸基含有モノマー；２－ヒドロキシエチルアクリロイルホスフェートなどの燐酸基含有モノマーなどがあげられる。
In addition to the above monomers, acid anhydride group-containing monomers such as maleic anhydride and itaconic anhydride; caprolactone adducts of acrylic acid; styrene sulfonic acid, allyl sulfonic acid, 2- (meth) acrylamide-2-methylpropan sulfonic acid. , (Meta) acrylamide propane sulfonic acid, sulfopropyl (meth) acrylate, (meth) acryloyloxynaphthalene sulfonic acid and other sulfonic acid group-containing monomers; and 2-hydroxyethyl acryloyl phosphate and other phosphoric acid group-containing monomers.
さらに、酢酸ビニル、プロピオン酸ビニル、Ｎ－ビニルピロリドン、メチルビニルピロリドン、ビニルピリジン、ビニルピペリドン、ビニルピリミジン、ビニルピペラジン、ビニルピラジン、ビニルピロール、ビニルイミダゾール、ビニルオキサゾール、ビニルモルホリン、Ｎ－ビニルカルボン酸アミド類、スチレン、α－メチルスチレン、Ｎ－ビニルカプロラクタムなどのビニル系モノマー；アクリロニトリル、メタクリロニトリルなどのシアノアクリレート系モノマー；（メタ）アクリル酸グリシジルなどのエポキシ基含有アクリル系モノマー；（メタ）アクリル酸ポリエチレングリコール、（メタ）アクリル酸ポリプロピレングリコール、（メタ）アクリル酸メトキシエチレングリコール、（メタ）アクリル酸メトキシポリプロピレングリコールなどのグリコール系アクリルエステルモノマー；（メタ）アクリル酸テトラヒドロフルフリル、フッ素（メタ）アクリレート、シリコーン（メタ）アクリレートや２－メトキシエチルアクリレートなどのアクリル酸エステル系モノマーなども使用することができる。
In addition, vinyl acetate, vinyl propionate, N-vinylpyrrolidone, methylvinylpyrrolidone, vinylpyridine, vinylpiperidone, vinylpyrimidine, vinylpiperazin, vinylpyrazine, vinylpyrrole, vinylimidazole, vinyloxazole, vinylmorpholin, N-vinylcarboxylic acid amide. Vinyl-based monomers such as styrene, α-methylstyrene, N-vinylcaprolactam; cyanoacrylate-based monomers such as acrylonitrile and methacrylonitrile; epoxy group-containing acrylic monomers such as glycidyl (meth) acrylate; (meth) acrylic Glycol-based acrylic ester monomers such as polyethylene glycol acid acid, polypropylene glycol (meth) acrylate, methoxyethylene glycol (meth) acrylate, methoxypolypropylene glycol (meth) acrylate; tetrahydrofurfuryl (meth) acrylate, fluorine (meth) Acrylic acid ester-based monomers such as acrylate, silicone (meth) acrylate and 2-methoxyethyl acrylate can also be used.
これらの中でも、架橋剤との反応性が良好である点から、水酸基含有モノマーが好適に用いられる。また、接着性、接着耐久性の点から、アクリル酸などのカルボキシ基含有モノマーが好ましく用いられる。
Among these, a hydroxyl group-containing monomer is preferably used because it has good reactivity with a cross-linking agent. Further, from the viewpoint of adhesiveness and adhesive durability, a carboxy group-containing monomer such as acrylic acid is preferably used.
（メタ）アクリル系ポリマー中の前記共重合モノマーの割合は、特に制限されないが、質量比率において、２０質量％以下である。好ましくは０．１～１０質量％、より好ましくは０．５～８質量％、さらに好ましくは１～６質量％である。前記水酸基含有モノマーを含有する場合には、質量比率において、好ましくは０．０１～５質量％、より好ましくは０．０５～３質量％、更に好ましくは０．１～２質量％である。前記カルボキシ基含有モノマーを含有する場合には、質量比率において、好ましくは０．０１～１５質量％、より好ましくは０．１～１０質量％、更に好ましくは１～５質量％である。
The ratio of the copolymerization monomer in the (meth) acrylic polymer is not particularly limited, but is 20% by mass or less in terms of mass ratio. It is preferably 0.1 to 10% by mass, more preferably 0.5 to 8% by mass, and even more preferably 1 to 6% by mass. When the hydroxyl group-containing monomer is contained, the mass ratio is preferably 0.01 to 5% by mass, more preferably 0.05 to 3% by mass, and further preferably 0.1 to 2% by mass. When the carboxy group-containing monomer is contained, the mass ratio is preferably 0.01 to 15% by mass, more preferably 0.1 to 10% by mass, and further preferably 1 to 5% by mass.
（メタ）アクリル系ポリマーの平均分子量は特に制限されないが、重量平均分子量は、３０万～２５０万程度であるのが好ましい。前記（メタ）アクリル系ポリマーの製造は、各種公知の手法により製造でき、たとえば、バルク重合法、溶液重合法、懸濁重合法等のラジカル重合法を適宜選択できる。ラジカル重合開始剤としては、アゾ系、過酸化物系の各種公知のものを使用できる。反応温度は通常５０～８０℃程度、反応時間は１～８時間とされる。また、前記製造法の中でも溶液重合法が好ましく、（メタ）アクリル系ポリマーの溶媒としては一般に酢酸エチル、トルエン等が用いられる。
The average molecular weight of the (meth) acrylic polymer is not particularly limited, but the weight average molecular weight is preferably about 300,000 to 2.5 million. The (meth) acrylic polymer can be produced by various known methods, and for example, a radical polymerization method such as a bulk polymerization method, a solution polymerization method, or a suspension polymerization method can be appropriately selected. As the radical polymerization initiator, various known azo-based and peroxide-based radical polymerization initiators can be used. The reaction temperature is usually about 50 to 80 ° C., and the reaction time is 1 to 8 hours. Further, among the above-mentioned production methods, the solution polymerization method is preferable, and ethyl acetate, toluene and the like are generally used as the solvent for the (meth) acrylic polymer.
本発明の多層化粘着剤層を形成する粘着剤組成物は、ベースポリマーに加えて架橋剤を含有することができる。架橋剤により、粘着剤層同士、あるいは粘着剤層と光学フィルムとの密着性や耐久性を向上でき、また高温での信頼性や粘着剤自体の形状の保持を図ることができる。ベースポリマーが（メタ）アクリル系ポリマーの場合、架橋剤としては、イソシアネート系、エポキシ系、過酸化物系、金属キレート系、オキサゾリン系などを適宜に使用可能である。これら架橋剤は１種を、または２種以上を組み合わせて用いることができる。
The pressure-sensitive adhesive composition forming the multi-layered pressure-sensitive adhesive layer of the present invention can contain a cross-linking agent in addition to the base polymer. The cross-linking agent can improve the adhesion and durability between the pressure-sensitive adhesive layers or between the pressure-sensitive adhesive layers and the optical film, and can maintain reliability at high temperatures and the shape of the pressure-sensitive adhesive itself. When the base polymer is a (meth) acrylic polymer, an isocyanate-based, epoxy-based, peroxide-based, metal chelate-based, oxazoline-based, or the like can be appropriately used as the cross-linking agent. These cross-linking agents may be used alone or in combination of two or more.
イソシアネート系架橋剤は、イソシアネート化合物が用いられる。イソシアネート化合物としては、トリレンジイソシアネート、クロルフェニレンジイソシアナート、ヘキサメチレンジイソシアナート、テトラメチレンジイソシアナート、イソホロンジイソシアネート、キシリレンジイソシアネート、ジフェニルメタンジイソシアネート、水添されたジフェニルメタンジイソシアネートなどのイソシアネートモノマー及びこれらイソシアネートモノマーをトリメチロールプロパンなどと付加したアダクト系イソシアネート化合物；イソシアヌレート化物、ビュレット型化合物、さらには公知のポリエーテルポリオールやポリエステルポリオール、アクリルポリオール、ポリブタジエンポリオール、ポリイソプレンポリオールなどを付加反応させたウレタンプレポリマー型のイソシアネートなどが挙げられる。
An isocyanate compound is used as the isocyanate-based cross-linking agent. Examples of the isocyanate compound include isocyanate monomers such as tolylene diisocyanate, chlorphenylene diisocyanate, hexamethylene diisosianate, tetramethylene diisosianate, isophorone diisocyanate, xylylene diisocyanate, diphenylmethane diisocyanate, and hydrogenated diphenylmethane diisocyanate, and these isocyanates. Adduct-based isocyanate compound in which a monomer is added to trimethylolpropane or the like; isocyanurate product, burette type compound, and urethane pre-reacted by addition reaction of known polyether polyol, polyester polyol, acrylic polyol, polybutadiene polyol, polyisoprene polyol, etc. Examples include polymer type isocyanate.
エポキシ系架橋剤としては、例えば、ビスフェノールＡエピクロルヒドリン型のエポキシ樹脂があげられる。また、エポキシ系架橋剤としては、例えば、エチレングリコールジグリシジルエーテル、ポリエチレングリコールジグリシジルエーテル、グリセリンジグリシジルエーテル、グリセリントリグリシジルエーテル、１，６－ヘキサンジオールジグリシジルエーテル、トリメチロールプロパントリグリシジルエーテル、ジグリシジルアニリン、Ｎ，Ｎ，Ｎ´，Ｎ´－テトラグリシジル－ｍ－キシリレンジアミン、１，３－ビス（Ｎ，Ｎ－ジグリシジルアミノメチル）シクロヘキサン、Ｎ，Ｎ，Ｎ´，Ｎ´－テトラグリシジルアミノフェニルメタン、トリグリシジルイソシアヌレート、ｍ－Ｎ，Ｎ－ジグリシジルアミノフェニルグリシジルエーテル、Ｎ，Ｎ－ジグリシジルトルイジン、及びＮ，Ｎ－ジグリシジルアニリンなどが挙げられる。
Examples of the epoxy-based cross-linking agent include bisphenol A epichlorohydrin type epoxy resin. Examples of the epoxy-based cross-linking agent include ethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether, glycerin diglycidyl ether, glycerin triglycidyl ether, 1,6-hexanediol diglycidyl ether, and trimethylolpropan triglycidyl ether. Diglycidylaniline, N, N, N', N'-tetraglycidyl-m-xylylene diamine, 1,3-bis (N, N-diglycidylaminomethyl) cyclohexane, N, N, N', N'- Examples thereof include tetraglycidyl aminophenyl methane, triglycidyl isocyanurate, m-N, N-diglycidyl aminophenyl glycidyl ether, N, N-diglycidyl toluidine, and N, N-diglycidyl aniline.
過酸化物系架橋剤としては、各種過酸化物が用いられる。過酸化物としては、ジ（２‐エチルヘキシル）パーオキシジカーボネート、ジ（４‐ｔ‐ブチルシクロヘキシル）パーオキシジカーボネート、ジ‐ｓｅｃ‐ブチルパーオキシジカーボネート、ｔ－ブチルパーオキシネオデカノエート、ｔ‐へキシルパーオキシピバレート、ｔ‐ブチルパーオキシピバレート、ジラウロイルパーオキシド、ジ‐ｎ‐オクタノイルパーオキシド、１，１，３，３‐テトラメチルブチルパーオキシイソブチレート、１，１，３，３‐テトラメチルブチルパーオキシ２‐エチルヘキサノエート、ジ（４‐メチルベンゾイル）パーオキシド、ジベンゾイルパーオキシド、ｔ‐ブチルパーオキシイソブチレート、などが挙げられる。これらのなかでも、特に架橋反応効率に優れる、ジ（４‐t‐ブチルシクロヘキシル）パーオキシジカルボネート、ジラウロイルパーオキシド、ジベンゾイルパーオキシドが好ましく用いられる。
Various peroxides are used as the peroxide-based cross-linking agent. Peroxides include di (2-ethylhexyl) peroxydicarbonate, di (4-t-butylcyclohexyl) peroxydicarbonate, di-sec-butylperoxydicarbonate, and t-butylperoxyneodecanoate. , T-hexyl peroxypivalate, t-butylperoxypivalate, dilauroyl peroxide, di-n-octanoyl peroxide, 1,1,3,3-tetramethylbutylperoxyisobutyrate, 1 , 1,3,3-Tetramethylbutylperoxy2-ethylhexanoate, di (4-methylbenzoyl) peroxide, dibenzoyl peroxide, t-butylperoxyisobutyrate, and the like. Among these, di (4-t-butylcyclohexyl) peroxydicarbonate, dilauroyl peroxide, and dibenzoyl peroxide, which are particularly excellent in cross-linking reaction efficiency, are preferably used.
架橋剤の使用量は、（メタ）アクリル系ポリマー１００質量部に対して、１０質量部以下、好ましくは０．０１～５質量部、さらに好ましくは０．１～１質量部である。架橋剤の使用割合が、１０質量部を超えると架橋が進みすぎて接着性が低下するおそれがある。
The amount of the cross-linking agent used is 10 parts by mass or less, preferably 0.01 to 5 parts by mass, and more preferably 0.1 to 1 part by mass with respect to 100 parts by mass of the (meth) acrylic polymer. If the proportion of the cross-linking agent used exceeds 10 parts by mass, the cross-linking may proceed too much and the adhesiveness may deteriorate.
さらには、前記粘着剤組成物には、必要に応じて、粘着付与剤、可塑剤、ガラス繊維、ガラスビーズ、金属粉、その他の無機粉末等からなる充填剤、顔料、着色剤、充填剤、酸化防止剤、紫外線吸収剤、シランカップリング剤等を、また本発明の目的を逸脱しない範囲で各種の添加剤を適宜に使用することもできる。
Further, the pressure-sensitive adhesive composition includes, if necessary, a pressure-imparting agent, a plasticizing agent, a glass fiber, a glass bead, a metal powder, a filler made of other inorganic powder, a pigment, a colorant, a filler, and the like. Antioxidants, ultraviolet absorbers, silane coupling agents and the like can be appropriately used, and various additives can be appropriately used without departing from the object of the present invention.
本発明の多層化粘着剤層は、例えば、セパレータ上に粘着剤組成物を塗布し、前記粘着剤組成物を乾燥等して硬化（固化）して粘着剤層を形成し、形成した粘着剤層上に同様の方法で順次粘着剤層を形成し、その後、セパレータを剥離することにより製造することができる。また、本発明の多層化粘着剤層は、例えば、一方のセパレータ上に粘着剤組成物を塗布し、前記粘着剤組成物を乾燥等して硬化（固化）することにより粘着剤層を１層以上形成し、また、他方のセパレータ上に粘着剤組成物を塗布し、前記粘着剤組成物を乾燥等して硬化（固化）することにより粘着剤層を１層以上形成し、そして、一方のセパレータ上の１層以上の粘着剤層と他方のセパレータ上の１層以上の粘着剤層とを積層し、その後、両側のセパレータを剥離することにより製造することができる。
In the multilayered pressure-sensitive adhesive layer of the present invention, for example, a pressure-sensitive adhesive composition is applied on a separator, and the pressure-sensitive adhesive composition is dried or hardened (solidified) to form a pressure-sensitive adhesive layer. It can be produced by sequentially forming an adhesive layer on the layer in the same manner and then peeling off the separator. Further, in the multi-layered pressure-sensitive adhesive layer of the present invention, for example, a pressure-sensitive adhesive composition is applied on one separator, and the pressure-sensitive adhesive composition is dried or hardened (solidified) to form one layer of the pressure-sensitive adhesive layer. The pressure-sensitive adhesive composition is formed as described above, and the pressure-sensitive adhesive composition is applied onto the other separator, and the pressure-sensitive adhesive composition is dried or hardened (solidified) to form one or more pressure-sensitive adhesive layers, and one of them is formed. It can be produced by laminating one or more pressure-sensitive adhesive layers on a separator and one or more pressure-sensitive adhesive layers on the other separator, and then peeling off the separators on both sides.
粘着剤組成物は、溶液または分散液のいずれでもよい。溶液の場合、溶剤としては、例えば、トルエン等の芳香族系溶剤、酢酸エチル等のエステル系溶剤が用いられる。粘着剤組成物の固形分濃度は、表面ムラを抑制し、ＩＳＣ－Ｓ値５０以下の粘着剤層表面を得る観点から、通常、５～８０質量％程度であり、好ましくは１０～６０質量％、さらに好ましくは１０～４０質量％、さらに好ましくは１０～２０質量％である。
The pressure-sensitive adhesive composition may be either a solution or a dispersion. In the case of a solution, as the solvent, for example, an aromatic solvent such as toluene and an ester solvent such as ethyl acetate are used. The solid content concentration of the pressure-sensitive adhesive composition is usually about 5 to 80% by mass, preferably 10 to 60% by mass, from the viewpoint of suppressing surface unevenness and obtaining the surface of the pressure-sensitive adhesive layer having an ISC-S value of 50 or less. , More preferably 10 to 40% by mass, still more preferably 10 to 20% by mass.
セパレータ上や粘着剤層上への粘着剤組成物の塗工方法は、特に制限されず、例えば、クローズドエッジダイ、スロットダイ等のダイコーティング法；リバースコーティング、グラビアコーティング等のロールコーティング法、スピンコーティング法、スクリーンコーティング法、ファウンテンコーティング法、ディッピング法、スプレー法などを採用できる。
The method of applying the pressure-sensitive adhesive composition on the separator or the pressure-sensitive adhesive layer is not particularly limited, and for example, a die coating method such as a closed edge die or a slot die; a roll coating method such as reverse coating or gravure coating, or spin coating. A coating method, a screen coating method, a fountain coating method, a dipping method, a spray method, etc. can be adopted.
本発明において、各粘着剤層の厚みは、表面ムラを抑制し、ＩＳＣ－Ｓ値５０以下の粘着剤層表面を得る観点及び総厚みが２０～１００μｍの多層化粘着剤層の製造効率の観点から、１０～２０μｍであり、好ましくは１０～１５μｍ、より好ましくは１０～１２μｍである。
In the present invention, the thickness of each pressure-sensitive adhesive layer is from the viewpoint of suppressing surface unevenness to obtain a pressure-sensitive adhesive layer surface having an ISC-S value of 50 or less and from the viewpoint of manufacturing efficiency of a multi-layered pressure-sensitive adhesive layer having a total thickness of 20 to 100 μm. Therefore, it is 10 to 20 μm, preferably 10 to 15 μm, and more preferably 10 to 12 μm.
前記各粘着剤層は、表面ムラを抑制し、多層化粘着剤層のＩＳＣ－Ｓ値を５０以下にする観点から、温度３０～１０５℃、風速０．５～７ｍ／秒、及び乾燥時間５～３０秒間の条件で粘着剤組成物を乾燥する第１乾燥工程、前記第１乾燥工程後、温度３０～８５℃、風速０．５～７ｍ／秒、及び乾燥時間１０～１２０秒間の条件で粘着剤組成物を乾燥する第２乾燥工程、前記第２乾燥工程後、温度９０～１６０℃、風速０．１～２５ｍ／秒、及び乾燥時間１０～１８０秒間の条件で粘着剤組成物を乾燥する第３乾燥工程を含む乾燥工程により形成することが好ましい。
Each of the pressure-sensitive adhesive layers has a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 from the viewpoint of suppressing surface unevenness and reducing the ISC-S value of the multilayer pressure-sensitive adhesive layer to 50 or less. The first drying step of drying the pressure-sensitive adhesive composition under the condition of about 30 seconds, after the first drying step, under the conditions of a temperature of 30 to 85 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 10 to 120 seconds. After the second drying step of drying the pressure-sensitive adhesive composition, the pressure-sensitive adhesive composition is dried under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds. It is preferably formed by a drying step including a third drying step.
前記第１及び第２乾燥工程により、粘着剤組成物の溶剤を徐々に蒸発させるとともに、ＩＳＣ－Ｓ値５０以下の粘着剤層表面を形成し、次いで、前記第３乾燥工程により、前記ＩＳＣ－Ｓ値５０以下の粘着剤層表面を硬化（固化）して粘着剤層を形成する。このように、段階的に乾燥工程を行うことにより、ＩＳＣ－Ｓ値５０以下の粘着剤層を形成し易くなる。
The solvent of the pressure-sensitive adhesive composition is gradually evaporated by the first and second drying steps, and the surface of the pressure-sensitive adhesive layer having an ISC-S value of 50 or less is formed. Then, the ISC- The surface of the pressure-sensitive adhesive layer having an S value of 50 or less is cured (solidified) to form a pressure-sensitive adhesive layer. By performing the drying step step by step in this way, it becomes easy to form the pressure-sensitive adhesive layer having an ISC-S value of 50 or less.
前記第１乾燥工程における温度は、３０～１０５℃であり、好ましくは４０～１００℃、より好ましくは５０～９５℃、さらに好ましくは７０～９５℃である。前記温度が３０℃以上であれば、溶剤の乾燥時間を短縮でき、製造効率の観点で好ましい。一方、前記温度が１０５℃以下であれば、急速な乾燥を防止でき、ＩＳＣ－Ｓ値５０以下の粘着剤層表面を形成し易くなるため好ましい。
The temperature in the first drying step is 30 to 105 ° C, preferably 40 to 100 ° C, more preferably 50 to 95 ° C, and even more preferably 70 to 95 ° C. When the temperature is 30 ° C. or higher, the drying time of the solvent can be shortened, which is preferable from the viewpoint of production efficiency. On the other hand, when the temperature is 105 ° C. or lower, rapid drying can be prevented and the surface of the pressure-sensitive adhesive layer having an ISC-S value of 50 or less can be easily formed, which is preferable.
前記第１乾燥工程における風速は、０．５～７ｍ／秒であり、好ましくは０．５～６ｍ／秒、より好ましくは１～５ｍ／秒、さらに好ましくは３～５ｍ／秒である。前記風速が０．５ｍ／秒以上であれば、溶剤の乾燥時間を短縮でき、製造効率の観点で好ましい。一方、前記風速が７ｍ／秒以下であれば、急速な乾燥を防止でき、ＩＳＣ－Ｓ値５０以下の粘着剤層表面を形成し易くなるため好ましい。
The wind speed in the first drying step is 0.5 to 7 m / sec, preferably 0.5 to 6 m / sec, more preferably 1 to 5 m / sec, and even more preferably 3 to 5 m / sec. When the wind speed is 0.5 m / sec or more, the drying time of the solvent can be shortened, which is preferable from the viewpoint of production efficiency. On the other hand, when the wind speed is 7 m / sec or less, rapid drying can be prevented and the surface of the pressure-sensitive adhesive layer having an ISC-S value of 50 or less can be easily formed, which is preferable.
前記第１乾燥工程における乾燥時間は、５～３０秒間であり、好ましくは１０秒～２５秒間、より好ましくは１５秒～２０秒間である。なお、第１乾燥工程における乾燥時間は、温度及び風速との関係を考慮して、粘着剤層のＩＳＣ－Ｓ値が５０以下になるように制御する。
The drying time in the first drying step is 5 to 30 seconds, preferably 10 seconds to 25 seconds, and more preferably 15 seconds to 20 seconds. The drying time in the first drying step is controlled so that the ISC-S value of the pressure-sensitive adhesive layer is 50 or less in consideration of the relationship between the temperature and the wind speed.
前記第２乾燥工程における温度は、３０～８５℃であり、好ましくは４０～８０℃、より好ましくは５０～７５℃、さらに好ましくは６０～７５℃である。前記温度が３０℃以上であれば、溶剤の乾燥時間を短縮でき、製造効率の観点で好ましい。一方、前記温度が８５℃以下であれば、急速な乾燥を防止でき、ＩＳＣ－Ｓ値５０以下の粘着剤層表面を形成し易くなるため好ましい。
The temperature in the second drying step is 30 to 85 ° C, preferably 40 to 80 ° C, more preferably 50 to 75 ° C, and even more preferably 60 to 75 ° C. When the temperature is 30 ° C. or higher, the drying time of the solvent can be shortened, which is preferable from the viewpoint of production efficiency. On the other hand, when the temperature is 85 ° C. or lower, rapid drying can be prevented and the surface of the pressure-sensitive adhesive layer having an ISC-S value of 50 or less can be easily formed, which is preferable.
前記第２乾燥工程における風速は、０．５～７ｍ／秒であり、好ましくは０．５～６ｍ／秒、より好ましくは１～５ｍ／秒、さらに好ましくは３～５ｍ／秒である。前記風速が０．５ｍ／秒以上であれば、溶剤の乾燥時間を短縮でき、製造効率の観点で好ましい。一方、前記風速が７ｍ／秒以下であれば、急速な乾燥を防止でき、ＩＳＣ－Ｓ値５０以下の粘着剤層表面を形成し易くなるため好ましい。
The wind speed in the second drying step is 0.5 to 7 m / sec, preferably 0.5 to 6 m / sec, more preferably 1 to 5 m / sec, and even more preferably 3 to 5 m / sec. When the wind speed is 0.5 m / sec or more, the drying time of the solvent can be shortened, which is preferable from the viewpoint of production efficiency. On the other hand, when the wind speed is 7 m / sec or less, rapid drying can be prevented and the surface of the pressure-sensitive adhesive layer having an ISC-S value of 50 or less can be easily formed, which is preferable.
前記第２乾燥工程における乾燥時間は、１０～１２０秒間であり、好ましくは３０秒～９０秒間、より好ましくは４５秒～６０秒間である。なお、第２乾燥工程における乾燥時間は、温度及び風速との関係を考慮して、粘着剤層のＩＳＣ－Ｓ値が５０以下になるように制御する。
The drying time in the second drying step is 10 to 120 seconds, preferably 30 seconds to 90 seconds, and more preferably 45 seconds to 60 seconds. The drying time in the second drying step is controlled so that the ISC-S value of the pressure-sensitive adhesive layer is 50 or less in consideration of the relationship between the temperature and the wind velocity.
前記第３乾燥工程における温度は、９０～１６０℃であり、好ましくは１３０～１６０℃、より好ましくは１３５～１５５℃である。前記温度が９０℃以上であれば、溶剤の乾燥時間を短縮でき、製造効率の観点で好ましい。一方、前記温度が１６０℃以下であれば、粘着剤層に色味が付くことを防止できるため好ましい。
The temperature in the third drying step is 90 to 160 ° C, preferably 130 to 160 ° C, and more preferably 135 to 155 ° C. When the temperature is 90 ° C. or higher, the drying time of the solvent can be shortened, which is preferable from the viewpoint of production efficiency. On the other hand, when the temperature is 160 ° C. or lower, it is preferable because it is possible to prevent the pressure-sensitive adhesive layer from being colored.
前記第３乾燥工程における風速は、０．１～２５ｍ／秒であり、好ましくは１～２３ｍ／秒、より好ましくは５～２０ｍ／秒、さらに好ましくは１０～２０ｍ／秒である。前記風速が０．１ｍ／秒以上であれば、溶剤の乾燥時間を短縮でき、製造効率の観点で好ましい。一方、前記風速が２５ｍ／秒以下であれば、フィルムの走行性に悪影響が生じにくくなるため好ましい。
The wind velocity in the third drying step is 0.1 to 25 m / sec, preferably 1 to 23 m / sec, more preferably 5 to 20 m / sec, and even more preferably 10 to 20 m / sec. When the wind speed is 0.1 m / sec or more, the drying time of the solvent can be shortened, which is preferable from the viewpoint of production efficiency. On the other hand, when the wind speed is 25 m / sec or less, the running performance of the film is less likely to be adversely affected, which is preferable.
前記第３乾燥工程における乾燥時間は、１０～１８０秒間であり、好ましくは２０秒～１２０秒間、より好ましくは３０秒～６０秒間である。なお、第３乾燥工程における乾燥時間は、温度及び風速との関係を考慮して、粘着剤層を硬化（固化）するように制御する。
The drying time in the third drying step is 10 to 180 seconds, preferably 20 seconds to 120 seconds, and more preferably 30 seconds to 60 seconds. The drying time in the third drying step is controlled so as to cure (solidify) the pressure-sensitive adhesive layer in consideration of the relationship between the temperature and the wind speed.
前記第１～第３乾燥工程において、温度を前記範囲に制御する手段としては、例えば、オーブン、温風器、加熱ロール、遠赤外線ヒーター等を用いることができる。また、前記第１～第３乾燥工程において、風速を前記範囲に制御する送風手段としては、カウンターフロー式により施すことができる。前記送風手段との距離は１０～１００ｃｍ程度、好ましくは１０～５０ｃｍである。前記風速は、ミニベーン型デジタル風速計により測定することができる。風速測定は、送風ノズルの下、セパレータ上に塗布した粘着剤組成物の上３ｃｍの位置の風速を、風速計を用いて測定する。風速計は、日本カノマックス（株）製の風速計ＭＯＤＥＬ１５６０／ＳＹＳＴＥＭ ６２４３を用いる。
In the first to third drying steps, for example, an oven, a hot air blower, a heating roll, a far-infrared heater, or the like can be used as a means for controlling the temperature within the above range. Further, in the first to third drying steps, as a blowing means for controlling the wind velocity within the above range, a counterflow method can be applied. The distance from the blower means is about 10 to 100 cm, preferably 10 to 50 cm. The wind speed can be measured by a mini-vane type digital anemometer. The wind velocity is measured by using a wind speed meter at a position 3 cm above the pressure-sensitive adhesive composition applied on the separator under the blower nozzle. As the anemometer, an anemometer MODEL1560 / SYSTEM 6243 manufactured by Kanomax Japan Incorporated is used.
前記多層化粘着剤層は、前記粘着剤層を２層以上有するものであり、前記粘着剤層は３層であってもよく、４層であってもよい。なお、多層化粘着剤層の製造効率の観点、及び画像表示装置の薄型化の観点から、通常、５層以下である。
The multi-layered pressure-sensitive adhesive layer has two or more layers of the pressure-sensitive adhesive layer, and the pressure-sensitive adhesive layer may be three layers or four layers. From the viewpoint of manufacturing efficiency of the multilayer pressure-sensitive adhesive layer and from the viewpoint of reducing the thickness of the image display device, the number of layers is usually 5 or less.
前記多層化粘着剤層が、少なくとも直接積層されている第１粘着剤層と第２粘着剤層を含む場合、前記第１粘着剤層の形成材料である粘着剤組成物は、（メタ）アクリル系ポリマーＡを含み、前記第２粘着剤層の形成材料である粘着剤組成物は、（メタ）アクリル系ポリマーＢを含み、前記（メタ）アクリル系ポリマーＡの形成材料であるモノマー組成物と前記（メタ）アクリル系ポリマーＢの形成材料であるモノマー組成物は、それぞれ炭素数１～１８のアルキル基を有するアルキル（メタ）アクリレートを５０質量％以上含むことが好ましく、より好ましくは６０質量％以上、さらに好ましくは７０質量％以上、さらに好ましくは８０質量％以上、さらに好ましくは９０質量％以上である。また、前記アルキル（メタ）アクリレートのアルキル基の炭素数は、より好ましくは２～１６、さらに好ましくは４～１２である。また、前記（メタ）アクリル系ポリマーＡの形成材料であるモノマー組成物と前記（メタ）アクリル系ポリマーＢの形成材料であるモノマー組成物は、同じアルキル（メタ）アクリレートを５０質量％以上含むことが好ましく、より好ましくは６０質量％以上、さらに好ましくは７０質量％以上、さらに好ましくは８０質量％以上、さらに好ましくは９０質量％以上である。このように、第１粘着剤層と第２粘着剤層を近似する組成の粘着剤組成物で形成することにより、粘着剤層同士の密着性や接着性を向上させることができる。また、前記多層化粘着剤層が、第３以上の粘着剤層を含む場合、その粘着剤層についても、第１粘着剤層や第２粘着剤層の形成材料である粘着剤組成物に近似する組成の粘着剤組成物を用いて形成することが好ましい。
When the multi-layered pressure-sensitive adhesive layer includes at least a first pressure-sensitive adhesive layer and a second pressure-sensitive adhesive layer that are directly laminated, the pressure-sensitive adhesive composition that is a material for forming the first pressure-sensitive adhesive layer is (meth) acrylic. The pressure-sensitive adhesive composition containing the system polymer A and being the material for forming the second pressure-sensitive adhesive layer is the monomer composition containing the (meth) acrylic polymer B and being the material for forming the (meth) acrylic polymer A. The monomer composition which is the material for forming the (meth) acrylic polymer B preferably contains 50% by mass or more of an alkyl (meth) acrylate having an alkyl group having 1 to 18 carbon atoms, and more preferably 60% by mass. As mentioned above, it is more preferably 70% by mass or more, further preferably 80% by mass or more, still more preferably 90% by mass or more. The alkyl group of the alkyl (meth) acrylate has more preferably 2 to 16 carbon atoms, and even more preferably 4 to 12 carbon atoms. Further, the monomer composition which is the material for forming the (meth) acrylic polymer A and the monomer composition which is the material for forming the (meth) acrylic polymer B contain 50% by mass or more of the same alkyl (meth) acrylate. Is more preferable, more preferably 60% by mass or more, still more preferably 70% by mass or more, still more preferably 80% by mass or more, still more preferably 90% by mass or more. As described above, by forming the first pressure-sensitive adhesive layer and the second pressure-sensitive adhesive layer with a pressure-sensitive adhesive composition having a composition similar to that of the first pressure-sensitive adhesive layer, the adhesiveness and adhesiveness between the pressure-sensitive adhesive layers can be improved. When the multi-layered pressure-sensitive adhesive layer contains a third or higher pressure-sensitive adhesive layer, the pressure-sensitive adhesive layer is also similar to the pressure-sensitive adhesive composition which is a material for forming the first pressure-sensitive adhesive layer and the second pressure-sensitive adhesive layer. It is preferably formed by using a pressure-sensitive adhesive composition having the same composition.
前記多層化粘着剤層は、フレキシブルパネル（例えば、フレキシブル有機ＥＬパネル）の耐久性を向上させる観点及びパネルの薄型化の観点から、総厚みが２０～１００μｍであり、好ましくは２０～５０μｍ、より好ましくは２０～４０μｍである。
The multi-layer adhesive layer has a total thickness of 20 to 100 μm, preferably 20 to 50 μm, from the viewpoint of improving the durability of the flexible panel (for example, a flexible organic EL panel) and reducing the thickness of the panel. It is preferably 20 to 40 μm.
また、前記多層化粘着剤層は、筋ムラ率を表すＩＳＣ－Ｓ値が５０以下であり、好ましくは４５以下、より好ましくは３５以下、さらに好ましくは３０以下である。本発明の多層化粘着剤層の製造方法によれば、ＩＳＣ－Ｓ値が２５以下である多層化粘着剤層を製造することも可能である。
Further, the multilayer pressure-sensitive adhesive layer has an ISC-S value representing a muscle unevenness ratio of 50 or less, preferably 45 or less, more preferably 35 or less, and further preferably 30 or less. According to the method for producing a multi-layered pressure-sensitive adhesive layer of the present invention, it is also possible to produce a multi-layered pressure-sensitive adhesive layer having an ISC-S value of 25 or less.
＜セパレータ付き多層化粘着剤層＞
本発明のセパレータ付き多層化粘着剤層は、前記多層化粘着剤層の片面又は両面にセパレータを有するものである。セパレータは、公知のものを特に制限なく使用することができ、剥離処理したセパレータを用いることが好ましい。 <Multi-layer adhesive layer with separator>
The multi-layered pressure-sensitive adhesive layer with a separator of the present invention has a separator on one side or both sides of the multi-layered pressure-sensitive adhesive layer. As the separator, known ones can be used without particular limitation, and it is preferable to use a separator that has been peeled off.
本発明のセパレータ付き多層化粘着剤層は、前記多層化粘着剤層の片面又は両面にセパレータを有するものである。セパレータは、公知のものを特に制限なく使用することができ、剥離処理したセパレータを用いることが好ましい。 <Multi-layer adhesive layer with separator>
The multi-layered pressure-sensitive adhesive layer with a separator of the present invention has a separator on one side or both sides of the multi-layered pressure-sensitive adhesive layer. As the separator, known ones can be used without particular limitation, and it is preferable to use a separator that has been peeled off.
本発明のセパレータ付き多層化粘着剤層は、例えば、セパレータ上に前記粘着剤組成物を塗布し、塗布した前記粘着剤組成物を前記第１～第３乾燥工程を含む乾燥工程により硬化（固化）して粘着剤層を形成し、さらに、前記粘着剤層上に別の粘着剤組成物を塗布する工程、及び前記第１～第３乾燥工程を含む乾燥工程を繰り返し行うことにより、前記粘着剤層上に別の粘着剤層を順次積層することにより製造することができる。
The multilayer pressure-sensitive adhesive layer with a separator of the present invention is, for example, coated with the pressure-sensitive adhesive composition on a separator, and the applied pressure-sensitive adhesive composition is cured (solidified) by a drying step including the first to third drying steps. ) To form a pressure-sensitive adhesive layer, and further repeat a step of applying another pressure-sensitive adhesive composition on the pressure-sensitive adhesive layer and a drying step including the first to third drying steps to obtain the pressure-sensitive adhesive. It can be produced by sequentially laminating another pressure-sensitive adhesive layer on the agent layer.
また、本発明のセパレータ付き多層化粘着剤層は、例えば、一方のセパレータ上に粘着剤組成物を塗布し、塗布した前記粘着剤組成物を前記第１～第３乾燥工程を含む乾燥工程により硬化（固化）して、一方のセパレータ上に粘着剤層を１層以上形成し、他方のセパレータ上にも同様の方法で粘着剤層を１層以上形成し、そして、一方のセパレータ上の粘着剤層と他方のセパレータ上の粘着剤層とを積層することにより製造することができる。
Further, in the multilayer pressure-sensitive adhesive layer with a separator of the present invention, for example, a pressure-sensitive adhesive composition is applied on one of the separators, and the applied pressure-sensitive adhesive composition is subjected to a drying step including the first to third drying steps. It is cured (solidified) to form one or more pressure-sensitive adhesive layers on one separator, one or more pressure-sensitive adhesive layers on the other separator in the same manner, and adhesion on one separator. It can be produced by laminating the agent layer and the pressure-sensitive adhesive layer on the other separator.
前記セパレータ付き多層化粘着剤層は、ハンドリング性の向上及びパネルの製造効率の向上の観点から、引張速度３００ｍｍ／分、剥離角度１８０度の条件で測定されるセパレータ剥離力が０．１５Ｎ／５０ｍｍ以下であることが好ましく、より好ましくは０．１４Ｎ／５０ｍｍ以下、さらに好ましくは０．１３Ｎ／５０ｍｍ以下である。粘着剤層の形成材料である粘着剤組成物中に含まれる過酸化物が多いほどセパレータと反応しやすくなるため、セパレータ剥離力は高くなり、剥離しにくくなる。従来の粘着剤層の製造方法では、セパレータ上に塗布された粘着剤組成物の塗布厚が大きいため粘着剤組成物中に含まれる過酸化物の量も相対的に多くなり、セパレータと反応しやすくなるため、セパレータが剥離しにくくなると考えられる。一方、本発明のセパレータ付き多層化粘着剤層の製造方法では、セパレータ上に塗布された粘着剤組成物の塗布厚が小さいため粘着剤組成物中に含まれる過酸化物の量も相対的に少なくなり、セパレータと反応しにくくなるため、セパレータ剥離力は小さくなり、剥離しやすくなると考えられる。
The multi-layer adhesive layer with a separator has a separator peeling force of 0.15 N / 50 mm measured under the conditions of a tensile speed of 300 mm / min and a peeling angle of 180 degrees from the viewpoint of improving handleability and panel manufacturing efficiency. It is preferably 0.14 N / 50 mm or less, more preferably 0.13 N / 50 mm or less. The greater the amount of peroxide contained in the pressure-sensitive adhesive composition, which is the material for forming the pressure-sensitive adhesive layer, the easier it is to react with the separator, so that the separator peeling power becomes higher and peeling becomes more difficult. In the conventional method for producing the pressure-sensitive adhesive layer, since the coating thickness of the pressure-sensitive adhesive composition applied on the separator is large, the amount of peroxide contained in the pressure-sensitive adhesive composition is relatively large and reacts with the separator. It is considered that the separator is difficult to peel off because it becomes easy. On the other hand, in the method for producing a multilayer pressure-sensitive adhesive layer with a separator of the present invention, the coating thickness of the pressure-sensitive adhesive composition applied on the separator is small, so that the amount of peroxide contained in the pressure-sensitive adhesive composition is relatively large. It is considered that the amount of the separator peeling force becomes small and the peeling becomes easy because the amount of the separator is reduced and the reaction with the separator becomes difficult.
＜粘着型光学フィルム＞
本発明の粘着型光学フィルムは、前記多層化粘着剤層と、光学フィルムとを有するものである。光学フィルムは特に制限されず、例えば、液晶表示装置（ＬＣＤ）、有機ＥＬ表示装置、ＣＲＴ、及びＰＤＰなどの画像表示装置に用いられる光学フィルムが挙げられ、具体的には、偏光フィルム、位相差板、視野角拡大フィルム、輝度向上フィルム、ハードコートフィルム、アンチグレア処理フィルム、アンチリフレクティブフィルム、及びローリフレクティブフィルムなどの反射防止フィルム、これらを積層したフィルムなどが挙げられる。前記粘着型光学フィルムは、例えば、前記セパレータ付き多層化粘着剤層の多層化粘着剤層の片面又は両面に光学フィルムを貼り合わせることにより製造することができる。 <Adhesive optical film>
The pressure-sensitive optical film of the present invention has the multilayer pressure-sensitive adhesive layer and an optical film. The optical film is not particularly limited, and examples thereof include an optical film used in an image display device such as a liquid crystal display (LCD), an organic EL display device, a CRT, and a PDP. Specific examples thereof include a polarizing film and a phase difference. Examples thereof include a plate, a viewing angle expanding film, a brightness improving film, a hard coat film, an anti-glare treated film, an anti-reflective film, an anti-reflection film such as a low reflective film, and a film in which these are laminated. The pressure-sensitive optical film can be produced, for example, by laminating an optical film on one side or both sides of the multi-layered pressure-sensitive adhesive layer of the multi-layered pressure-sensitive adhesive layer with a separator.
本発明の粘着型光学フィルムは、前記多層化粘着剤層と、光学フィルムとを有するものである。光学フィルムは特に制限されず、例えば、液晶表示装置（ＬＣＤ）、有機ＥＬ表示装置、ＣＲＴ、及びＰＤＰなどの画像表示装置に用いられる光学フィルムが挙げられ、具体的には、偏光フィルム、位相差板、視野角拡大フィルム、輝度向上フィルム、ハードコートフィルム、アンチグレア処理フィルム、アンチリフレクティブフィルム、及びローリフレクティブフィルムなどの反射防止フィルム、これらを積層したフィルムなどが挙げられる。前記粘着型光学フィルムは、例えば、前記セパレータ付き多層化粘着剤層の多層化粘着剤層の片面又は両面に光学フィルムを貼り合わせることにより製造することができる。 <Adhesive optical film>
The pressure-sensitive optical film of the present invention has the multilayer pressure-sensitive adhesive layer and an optical film. The optical film is not particularly limited, and examples thereof include an optical film used in an image display device such as a liquid crystal display (LCD), an organic EL display device, a CRT, and a PDP. Specific examples thereof include a polarizing film and a phase difference. Examples thereof include a plate, a viewing angle expanding film, a brightness improving film, a hard coat film, an anti-glare treated film, an anti-reflective film, an anti-reflection film such as a low reflective film, and a film in which these are laminated. The pressure-sensitive optical film can be produced, for example, by laminating an optical film on one side or both sides of the multi-layered pressure-sensitive adhesive layer of the multi-layered pressure-sensitive adhesive layer with a separator.
＜セパレータ付き粘着型光学フィルム＞
本発明のセパレータ付き粘着型光学フィルムは、前記セパレータ付き多層化粘着剤層と、前記光学フィルムとを有するものである。 <Adhesive optical film with separator>
The pressure-sensitive adhesive film with a separator of the present invention has the multilayer pressure-sensitive adhesive layer with a separator and the optical film.
本発明のセパレータ付き粘着型光学フィルムは、前記セパレータ付き多層化粘着剤層と、前記光学フィルムとを有するものである。 <Adhesive optical film with separator>
The pressure-sensitive adhesive film with a separator of the present invention has the multilayer pressure-sensitive adhesive layer with a separator and the optical film.
本発明のセパレータ付き粘着型光学フィルムは、例えば、セパレータ上に前記粘着剤組成物を塗布し、塗布した前記粘着剤組成物を前記第１～第３乾燥工程を含む乾燥工程により硬化（固化）して粘着剤層を形成し、さらに、前記粘着剤層上に別の粘着剤組成物を塗布する工程、及び前記第１～第３乾燥工程を含む乾燥工程を繰り返し行うことにより、前記粘着剤層上に別の粘着剤層を順次積層してセパレータ付き多層化粘着剤層を作製し、セパレータ付き多層化粘着剤層の多層化粘着剤層の片面に光学フィルムを貼り合わせることにより製造することができる。
In the pressure-sensitive optical film with a separator of the present invention, for example, the pressure-sensitive adhesive composition is coated on a separator, and the coated pressure-sensitive adhesive composition is cured (solidified) by a drying step including the first to third drying steps. The pressure-sensitive adhesive is formed by forming a pressure-sensitive adhesive layer, and further repeating a step of applying another pressure-sensitive adhesive composition on the pressure-sensitive adhesive layer and a drying step including the first to third drying steps are performed to obtain the pressure-sensitive adhesive. Another pressure-sensitive adhesive layer is sequentially laminated on the layer to prepare a multi-layered pressure-sensitive adhesive layer with a separator, and an optical film is bonded to one side of the multi-layered pressure-sensitive adhesive layer of the multi-layered pressure-sensitive adhesive layer with a separator. Can be done.
また、本発明のセパレータ付き粘着型光学フィルムは、例えば、一方のセパレータ上に粘着剤組成物を塗布し、塗布した前記粘着剤組成物を前記第１～第３乾燥工程を含む乾燥工程により硬化（固化）して、一方のセパレータ上に粘着剤層を１層以上形成し、前記粘着剤層の前記セパレータを有しない面に光学フィルムを積層した後、前記セパレータを剥離し、同様の方法で他方のセパレータ上に粘着剤層を１層以上形成し、その後、前記光学フィルム上の粘着剤層と他方のセパレータ上の粘着剤層とを積層することにより製造することができる。
Further, in the pressure-sensitive adhesive film with a separator of the present invention, for example, a pressure-sensitive adhesive composition is applied onto one of the separators, and the coated pressure-sensitive adhesive composition is cured by a drying step including the first to third drying steps. After (solidification), one or more pressure-sensitive adhesive layers are formed on one separator, an optical film is laminated on the surface of the pressure-sensitive adhesive layer that does not have the separator, and then the separator is peeled off in the same manner. It can be produced by forming one or more pressure-sensitive adhesive layers on the other separator, and then laminating the pressure-sensitive adhesive layer on the optical film and the pressure-sensitive adhesive layer on the other separator.
＜フレキシブル画像表示装置＞
本発明の粘着型光学フィルムは、フレキシブル画像表示装置（例えば、フレキシブル有機ＥＬ表示装置）の構成部材として有用である。 <Flexible image display device>
The adhesive optical film of the present invention is useful as a constituent member of a flexible image display device (for example, a flexible organic EL display device).
本発明の粘着型光学フィルムは、フレキシブル画像表示装置（例えば、フレキシブル有機ＥＬ表示装置）の構成部材として有用である。 <Flexible image display device>
The adhesive optical film of the present invention is useful as a constituent member of a flexible image display device (for example, a flexible organic EL display device).
本発明のフレキシブル画像表示装置用粘着型光学フィルムは、前記多層化粘着剤層と、少なくとも偏光膜を含む光学フィルムとを含むことを特徴とし、前記光学フィルムとしては、前記偏光膜に加えて、例えば、透明樹脂材料から形成される保護膜や位相差膜などのフィルムを含むものを指す。また、本発明において、前記光学フィルムとして、前記偏光膜と、前記偏光膜の第１の面に有する透明樹脂材料の保護膜と、前記偏光膜の前記第１の面とは異なる第２の面に有する位相差膜と、を含む構成を光学積層体という。
The adhesive optical film for a flexible image display device of the present invention is characterized by including the multilayer pressure-sensitive adhesive layer and an optical film containing at least a polarizing film, and the optical film includes, in addition to the polarizing film, the polarizing film. For example, it refers to a film including a protective film or a retardation film formed from a transparent resin material. Further, in the present invention, as the optical film, the polarizing film, the protective film of the transparent resin material provided on the first surface of the polarizing film, and the second surface different from the first surface of the polarizing film. The structure including the retardation film provided in the above is referred to as an optical laminate.
前記光学フィルムの厚さは、好ましくは９２μｍ以下であり、より好ましくは６０μｍ以下であり、更に好ましくは１０～５０μｍである。前記範囲内であれば、屈曲を阻害することなく、好ましい態様となる。
The thickness of the optical film is preferably 92 μm or less, more preferably 60 μm or less, and further preferably 10 to 50 μm. If it is within the above range, it will be a preferable embodiment without inhibiting bending.
前記偏光膜は、少なくとも片側には、保護膜が接着剤（層）により貼り合わされていても構わない（図面により図示せず）。偏光膜と保護膜との接着処理には、接着剤を用いることができる。接着剤としては、イソシアネート系接着剤、ポリビニルアルコール系接着剤、ゼラチン系接着剤、ビニル系ラテックス系、水系ポリエステル等を例示できる。前記接着剤は、通常、水溶液からなる接着剤として用いられ、通常、０．５～６０質量％の固形分を含有してなる。上記の他、偏光膜と保護膜との接着剤としては、紫外硬化型接着剤、電子線硬化型接着剤等が挙げられる。電子線硬化型偏光フィルム用接着剤は、上記各種の保護膜に対して、好適な接着性を示す。また本発明で用いる接着剤には、金属化合物フィラーを含有させることができる。なお、本発明においては、偏光膜と保護膜を接着剤（層）により貼り合わせたものを、偏光フィルム(偏光板)という場合がある。
The polarizing film may have a protective film bonded to at least one side by an adhesive (layer) (not shown in the drawing). An adhesive can be used for the bonding treatment between the polarizing film and the protective film. Examples of the adhesive include isocyanate-based adhesives, polyvinyl alcohol-based adhesives, gelatin-based adhesives, vinyl-based latex-based adhesives, and water-based polyesters. The adhesive is usually used as an adhesive composed of an aqueous solution, and usually contains 0.5 to 60% by mass of a solid content. In addition to the above, examples of the adhesive between the polarizing film and the protective film include an ultraviolet curable adhesive and an electron beam curable adhesive. The electron beam curable polarizing film adhesive exhibits suitable adhesiveness to the above-mentioned various protective films. Further, the adhesive used in the present invention may contain a metal compound filler. In the present invention, a polarizing film and a protective film bonded together with an adhesive (layer) may be referred to as a polarizing film (plate plate).
＜偏光膜＞
本発明の光学フィルムに含まれる偏光膜（偏光子ともいう。）は、空中延伸（乾式延伸）やホウ酸水中延伸工程等の延伸工程によって延伸された、ヨウ素を配向させたポリビニルアルコール（ＰＶＡ）系樹脂を用いることができる。 <Polarizing film>
The polarizing film (also referred to as a polarizer) contained in the optical film of the present invention is polyvinyl alcohol (PVA) in which iodine is oriented, which is stretched by a stretching step such as aerial stretching (dry stretching) or boric acid water stretching step. A system resin can be used.
本発明の光学フィルムに含まれる偏光膜（偏光子ともいう。）は、空中延伸（乾式延伸）やホウ酸水中延伸工程等の延伸工程によって延伸された、ヨウ素を配向させたポリビニルアルコール（ＰＶＡ）系樹脂を用いることができる。 <Polarizing film>
The polarizing film (also referred to as a polarizer) contained in the optical film of the present invention is polyvinyl alcohol (PVA) in which iodine is oriented, which is stretched by a stretching step such as aerial stretching (dry stretching) or boric acid water stretching step. A system resin can be used.
前記偏光膜の厚さは、２０μｍ以下であり、好ましくは１２μｍ以下であり、より好ましくは９μｍ以下であり、さらに好ましくは１～８μｍであり、特に好ましくは３～６μｍである。前記範囲内であれば、屈曲を阻害することなく、好ましい態様となる。
The thickness of the polarizing film is 20 μm or less, preferably 12 μm or less, more preferably 9 μm or less, still more preferably 1 to 8 μm, and particularly preferably 3 to 6 μm. If it is within the above range, it will be a preferable embodiment without inhibiting bending.
＜位相差膜＞
本発明に用いられる光学フィルムには、位相差膜を含むことができ、前記位相差膜（位相差フィルムともいう。）は、高分子フィルムを延伸させて得られるものや液晶材料を配向、固定化させたものを用いることができる。本明細書において、位相差膜は、面内及び／又は厚み方向に複屈折を有するものをいう。 <Phase difference film>
The optical film used in the present invention may include a retardation film, and the retardation film (also referred to as a retardation film) is obtained by stretching a polymer film or a liquid crystal material is oriented and fixed. It is possible to use a modified product. In the present specification, the retardation film refers to a film having birefringence in the in-plane and / or thickness direction.
本発明に用いられる光学フィルムには、位相差膜を含むことができ、前記位相差膜（位相差フィルムともいう。）は、高分子フィルムを延伸させて得られるものや液晶材料を配向、固定化させたものを用いることができる。本明細書において、位相差膜は、面内及び／又は厚み方向に複屈折を有するものをいう。 <Phase difference film>
The optical film used in the present invention may include a retardation film, and the retardation film (also referred to as a retardation film) is obtained by stretching a polymer film or a liquid crystal material is oriented and fixed. It is possible to use a modified product. In the present specification, the retardation film refers to a film having birefringence in the in-plane and / or thickness direction.
位相差膜としては、反射防止用位相差膜（特開２０１２－１３３３０３号公報〔０２２１〕、〔０２２２〕、〔０２２８〕参照）、視野角補償用相差膜（特開２０１２－１３３３０３号公報〔０２２５〕、〔０２２６〕参照）、視野角補償用の傾斜配向位相差膜（特開２０１２－１３３３０３号公報〔０２２７〕参照）等が挙げられる。
Examples of the retardation film include an antireflection retardation film (see Japanese Patent Application Laid-Open No. 2012-133303 [0221], [0222], and [0228]) and a viewing angle compensation retardation film (Japanese Patent Laid-Open No. 2012-133303 [0225]. ], [0226]), tilt-oriented retardation film for viewing angle compensation (see Japanese Patent Application Laid-Open No. 2012-133303 [0227]), and the like.
位相差膜としては、実質的に上記の機能を有するものであれば、例えば、位相差値、配置角度、３次元複屈折率、単層か多層かなどは特に限定されず公知の位相差膜を使用することができる。
As the retardation film, as long as it has substantially the above-mentioned functions, for example, the retardation value, the arrangement angle, the three-dimensional birefringence, and whether it is a single layer or a multilayer are not particularly limited and are known retardation films. Can be used.
前記位相差膜の厚さは、好ましくは２０μｍ以下であり、より好ましくは１０μｍ以下であり、更に好ましくは１～９μｍであり、特に好ましくは３～８μｍである。前記範囲内であれば、屈曲を阻害することなく、好ましい態様となる。
The thickness of the retardation film is preferably 20 μm or less, more preferably 10 μm or less, further preferably 1 to 9 μm, and particularly preferably 3 to 8 μm. If it is within the above range, it will be a preferable embodiment without inhibiting bending.
＜保護膜＞
本発明に用いられる光学フィルムには、透明樹脂材料から形成される保護膜を含むことができ、前記保護膜（透明保護フィルムともいう。）は、ノルボルネン系樹脂等のシクロオレフィン系樹脂、ポリエチレン、ポリプロピレン等のオレフィン系樹脂、ポリエステル系樹脂、（メタ）アクリル系樹脂などを用いることができる。 <Protective film>
The optical film used in the present invention can include a protective film formed from a transparent resin material, and the protective film (also referred to as a transparent protective film) is a cycloolefin resin such as a norbornene resin, polyethylene, or the like. Olefin-based resins such as polypropylene, polyester-based resins, (meth) acrylic-based resins, and the like can be used.
本発明に用いられる光学フィルムには、透明樹脂材料から形成される保護膜を含むことができ、前記保護膜（透明保護フィルムともいう。）は、ノルボルネン系樹脂等のシクロオレフィン系樹脂、ポリエチレン、ポリプロピレン等のオレフィン系樹脂、ポリエステル系樹脂、（メタ）アクリル系樹脂などを用いることができる。 <Protective film>
The optical film used in the present invention can include a protective film formed from a transparent resin material, and the protective film (also referred to as a transparent protective film) is a cycloolefin resin such as a norbornene resin, polyethylene, or the like. Olefin-based resins such as polypropylene, polyester-based resins, (meth) acrylic-based resins, and the like can be used.
前記保護膜の厚さは、好ましくは５～６０μｍであり、より好ましくは１０～４０μｍであり、更に好ましくは１０～３０μｍであり、適宜、アンチグレア層や反射防止層などの表面処理層を設けることができる。前記範囲内であれば、屈曲を阻害することなく、好ましい態様となる。
The thickness of the protective film is preferably 5 to 60 μm, more preferably 10 to 40 μm, still more preferably 10 to 30 μm, and a surface treatment layer such as an anti-glare layer or an anti-reflection layer is appropriately provided. Can be done. If it is within the above range, it will be a preferable embodiment without inhibiting bending.
［多層化粘着剤層］
本発明のフレキシブル画像表示装置用粘着型光学フィルムは、前記多層化粘着剤層を少なくとも１つ含む。 [Multi-layer adhesive layer]
The pressure-sensitive optical film for a flexible image display device of the present invention includes at least one of the multilayer pressure-sensitive adhesive layers.
本発明のフレキシブル画像表示装置用粘着型光学フィルムは、前記多層化粘着剤層を少なくとも１つ含む。 [Multi-layer adhesive layer]
The pressure-sensitive optical film for a flexible image display device of the present invention includes at least one of the multilayer pressure-sensitive adhesive layers.
フレキシブル画像表示装置用粘着型光学フィルムは、前記多層化粘着剤層を１つ有していてもよいが、光学フィルムの他に透明導電フィルム、有機ＥＬ表示パネル、ウインドウ、加飾印刷フィルム、位相差層、保護膜等の積層のために２つ以上有していてもよい(例えば、第１の多層化粘着剤層及び第２の多層化粘着剤層などフレキシブル画像表示装置用粘着型光学フィルム中に複数の多層化粘着剤層を有する場合として、例えば、図１等を参照)。複数の多層化粘着剤層を有する場合は、２つ以上５つ以下有することが好ましい。５つより多くなると、粘着型光学フィルム全体の厚みが厚くなるため、粘着型光学フィルムの屈曲部における最外層と最内層の歪み差が大きくなり、剥れや破断が生じやすくなるため、好ましくない。
The adhesive optical film for a flexible image display device may have one of the multilayer adhesive layers, but in addition to the optical film, a transparent conductive film, an organic EL display panel, a window, a decorative printing film, and the like. Two or more may be provided for laminating the retardation layer, the protective film, etc. (for example, an adhesive optical film for a flexible image display device such as a first multilayer adhesive layer and a second multilayer adhesive layer). As a case where a plurality of multilayer pressure-sensitive adhesive layers are provided therein, for example, see FIG. 1 and the like). When having a plurality of multilayer pressure-sensitive adhesive layers, it is preferable to have two or more and five or less. If the number is more than 5, the thickness of the entire adhesive optical film becomes thick, so that the strain difference between the outermost layer and the innermost layer at the bent portion of the adhesive optical film becomes large, and peeling or breakage is likely to occur, which is not preferable. ..
［第１の多層化粘着剤層］
本発明のフレキシブル画像表示装置用粘着型光学フィルムに用いる多層化粘着剤層の内、第１の多層化粘着剤層は、前記保護膜に対して、前記偏光膜と接している面と反対側に、配置されることが好ましい（図１参照）。 [First multilayer adhesive layer]
Among the multi-layered pressure-sensitive adhesive layers used in the pressure-sensitive adhesive film for a flexible image display device of the present invention, the first multi-layered pressure-sensitive adhesive layer is on the side opposite to the surface in contact with the polarizing film with respect to the protective film. (See FIG. 1).
本発明のフレキシブル画像表示装置用粘着型光学フィルムに用いる多層化粘着剤層の内、第１の多層化粘着剤層は、前記保護膜に対して、前記偏光膜と接している面と反対側に、配置されることが好ましい（図１参照）。 [First multilayer adhesive layer]
Among the multi-layered pressure-sensitive adhesive layers used in the pressure-sensitive adhesive film for a flexible image display device of the present invention, the first multi-layered pressure-sensitive adhesive layer is on the side opposite to the surface in contact with the polarizing film with respect to the protective film. (See FIG. 1).
［その他の多層化粘着剤層］
本発明のフレキシブル画像表示装置用粘着型光学フィルムに用いる多層化粘着剤層の内、第２の多層化粘着剤層を、前記位相差膜に対して、前記偏光膜と接している面と反対側に配置することができる（図１参照）。 [Other multi-layer adhesive layer]
Of the multi-layered pressure-sensitive adhesive layers used in the pressure-sensitive adhesive film for a flexible image display device of the present invention, the second multi-layered pressure-sensitive adhesive layer is opposite to the surface of the retardation film in contact with the polarizing film. It can be placed on the side (see FIG. 1).
本発明のフレキシブル画像表示装置用粘着型光学フィルムに用いる多層化粘着剤層の内、第２の多層化粘着剤層を、前記位相差膜に対して、前記偏光膜と接している面と反対側に配置することができる（図１参照）。 [Other multi-layer adhesive layer]
Of the multi-layered pressure-sensitive adhesive layers used in the pressure-sensitive adhesive film for a flexible image display device of the present invention, the second multi-layered pressure-sensitive adhesive layer is opposite to the surface of the retardation film in contact with the polarizing film. It can be placed on the side (see FIG. 1).
本発明のフレキシブル画像表示装置用粘着型光学フィルムに用いる多層化粘着剤層の内、第３の多層化粘着剤層は、前記タッチセンサを構成する透明導電層に対して、前記第２の多層化粘着剤層と接している面と反対側に、第３の多層化粘着剤層を配置することができる（図１参照）。
Among the multi-layered pressure-sensitive adhesive layers used in the adhesive-type optical film for a flexible image display device of the present invention, the third multi-layered pressure-sensitive adhesive layer is the second multi-layered adhesive layer with respect to the transparent conductive layer constituting the touch sensor. A third multilayer pressure-sensitive adhesive layer can be arranged on the side opposite to the surface in contact with the chemical pressure-sensitive adhesive layer (see FIG. 1).
本発明のフレキシブル画像表示装置用粘着型光学フィルムに用いる多層化粘着剤層の内、第３の多層化粘着剤層を、前記タッチセンサを構成する透明導電層に対して、前記第１の多層化粘着剤層と接している面と反対側に配置することができる（図２参照）。
Among the multi-layered pressure-sensitive adhesive layers used in the adhesive-type optical film for a flexible image display device of the present invention, the third multi-layered pressure-sensitive adhesive layer is the first multi-layered adhesive layer with respect to the transparent conductive layer constituting the touch sensor. It can be arranged on the side opposite to the surface in contact with the chemical pressure-sensitive adhesive layer (see FIG. 2).
なお、第１の多層化粘着剤層に加えて、第２の多層化粘着剤層、及び、更にはその他粘着剤層（例えば、第３の多層化粘着剤層など）を使用する場合、これら粘着剤層は、同一組成(同一粘着剤組成物)、同一特性を有するものであっても、異なる特性を有するものであっても、特に制限されないが、作業性、経済性、屈曲性の観点から、全ての粘着剤層が、実質的に同一組成、同一特性を有する粘着剤層であることが好ましい。
When a second multi-layered pressure-sensitive adhesive layer and other pressure-sensitive adhesive layers (for example, a third multi-layered pressure-sensitive adhesive layer) are used in addition to the first multi-layered pressure-sensitive adhesive layer, these are used. The pressure-sensitive adhesive layer may have the same composition (same pressure-sensitive adhesive composition), the same properties, or different properties, and is not particularly limited, but from the viewpoints of workability, economy, and flexibility. Therefore, it is preferable that all the pressure-sensitive adhesive layers are pressure-sensitive adhesive layers having substantially the same composition and the same characteristics.
［透明導電層］
透明導電層を有する部材としては、特に限定されるものではなく、公知のものを使用することができるが、透明フィルム等の透明基材上に透明導電層を有するものや、透明導電層と液晶セルを有する部材を挙げることができる。 [Transparent conductive layer]
The member having a transparent conductive layer is not particularly limited, and known members can be used, but a member having a transparent conductive layer on a transparent base material such as a transparent film, or a transparent conductive layer and a liquid crystal display. A member having a cell can be mentioned.
透明導電層を有する部材としては、特に限定されるものではなく、公知のものを使用することができるが、透明フィルム等の透明基材上に透明導電層を有するものや、透明導電層と液晶セルを有する部材を挙げることができる。 [Transparent conductive layer]
The member having a transparent conductive layer is not particularly limited, and known members can be used, but a member having a transparent conductive layer on a transparent base material such as a transparent film, or a transparent conductive layer and a liquid crystal display. A member having a cell can be mentioned.
透明基材としては、透明性を有するものであればよく、例えば、樹脂フィルム等からなる基材（例えば、シート状やフィルム状、板状の基材等）等が挙げられる。透明基材の厚さは、特に限定されないが、１０～２００μｍ程度が好ましく、１５～１５０μｍ程度がより好ましい。
The transparent base material may be any transparent material, and examples thereof include a base material made of a resin film or the like (for example, a sheet-like, film-like, plate-like base material, etc.). The thickness of the transparent base material is not particularly limited, but is preferably about 10 to 200 μm, more preferably about 15 to 150 μm.
前記樹脂フィルムの材料としては、特に制限されないが、透明性を有する各種のプラスチック材料が挙げられる。例えば、その材料として、ポリエチレンテレフタレート、ポリエチレンナフタレート等のポリエステル系樹脂、アセテート系樹脂、ポリエーテルスルホン系樹脂、ポリカーボネート系樹脂、ポリアミド系樹脂、ポリイミド系樹脂、ポリオレフィン系樹脂、（メタ）アクリル系樹脂、ポリ塩化ビニル系樹脂、ポリ塩化ビニリデン系樹脂、ポリスチレン系樹脂、ポリビニルアルコール系樹脂、ポリアリレート系樹脂、ポリフェニレンサルファイド系樹脂等が挙げられる。これらの中で特に好ましいのは、ポリエステル系樹脂、ポリイミド系樹脂及びポリエーテルスルホン系樹脂である。
The material of the resin film is not particularly limited, and examples thereof include various transparent plastic materials. For example, as the material, polyester resin such as polyethylene terephthalate and polyethylene naphthalate, acetate resin, polyether sulfone resin, polycarbonate resin, polyamide resin, polyimide resin, polyolefin resin, (meth) acrylic resin. , Polyvinyl chloride resin, polyvinylidene chloride resin, polystyrene resin, polyvinyl alcohol resin, polyallylate resin, polyphenylene sulfide resin and the like. Of these, polyester-based resins, polyimide-based resins and polyether sulfone-based resins are particularly preferable.
また、前記透明基材には、表面に予めスパッタリング、コロナ放電、火炎、紫外線照射、電子線照射、化成、酸化等のエッチング処理や下塗り処理を施して、この上に設けられる透明導電層の前記透明基材に対する密着性を向上させるようにしてもよい。また、透明導電層を設ける前に、必要に応じて溶剤洗浄や超音波洗浄等により除塵、清浄化してもよい。
Further, the transparent base material is subjected to etching treatment such as sputtering, corona discharge, flame, ultraviolet irradiation, electron beam irradiation, chemical conversion, oxidation, etc., and undercoating treatment in advance on the surface, and the transparent conductive layer provided on the transparent base material. The adhesion to the transparent substrate may be improved. Further, before providing the transparent conductive layer, dust may be removed and cleaned by solvent cleaning, ultrasonic cleaning, or the like, if necessary.
前記透明導電層の構成材料としては特に限定されず、インジウム、スズ、亜鉛、ガリウム、アンチモン、チタン、珪素、ジルコニウム、マグネシウム、アルミニウム、金、銀、銅、パラジウム、タングステン、モリブデンからなる群より選択される少なくとも１種の金属又は金属酸化物や、ポリチオフェン等の有機導電ポリマーが用いられる。当該金属酸化物には、必要に応じて、さらに上記群に示された金属原子を含んでいてもよい。例えば、酸化スズを含有する酸化インジウム（ＩＴＯ）、アンチモンを含有する酸化スズ等が好ましく用いられ、ＩＴＯが特に好ましく用いられる。ＩＴＯとしては、酸化インジウム８０～９９質量％及び酸化スズ１～２０質量％を含有することが好ましい。
The constituent material of the transparent conductive layer is not particularly limited, and is selected from the group consisting of indium, tin, zinc, gallium, antimony, titanium, silicon, zirconium, magnesium, aluminum, gold, silver, copper, palladium, tungsten and molybdenum. At least one kind of metal or metal oxide to be used, or an organic conductive polymer such as polythiophene is used. The metal oxide may further contain the metal atoms shown in the above group, if necessary. For example, indium oxide (ITO) containing tin oxide, tin oxide containing antimony, and the like are preferably used, and ITO is particularly preferably used. The ITO preferably contains 80 to 99% by mass of indium oxide and 1 to 20% by mass of tin oxide.
また、前記ＩＴＯとしては、結晶性のＩＴＯ、非結晶性（アモルファス）のＩＴＯを挙げることができる。結晶性ＩＴＯは、スパッタ時に高温をかけたり、非結晶性ＩＴＯをさらに加熱することにより得ることができる。
Further, examples of the ITO include crystalline ITO and non-crystalline (amorphous) ITO. The crystalline ITO can be obtained by applying a high temperature during sputtering or further heating the non-crystalline ITO.
前記透明導電層の厚みは、好ましくは０．００５～１０μｍであり、より好ましくは０．０１～３μｍであり、さらに好ましくは０．０１～１μｍである。透明導電層の厚みが、０．００５μｍ未満では、透明導電層の電気抵抗値の変化が大きくなる傾向がある。一方、１０μｍを超える場合は、透明導電層の生産性が低下し、コストも上昇し、さらに、光学特性も低下する傾向がある。
The thickness of the transparent conductive layer is preferably 0.005 to 10 μm, more preferably 0.01 to 3 μm, and further preferably 0.01 to 1 μm. If the thickness of the transparent conductive layer is less than 0.005 μm, the change in the electric resistance value of the transparent conductive layer tends to be large. On the other hand, if it exceeds 10 μm, the productivity of the transparent conductive layer tends to decrease, the cost also increases, and the optical characteristics tend to decrease.
前記透明導電層の全光線透過率は、好ましくは８０％以上であり、より好ましくは８５％以上であり、さらに好ましくは９０％以上である。
The total light transmittance of the transparent conductive layer is preferably 80% or more, more preferably 85% or more, and further preferably 90% or more.
前記透明導電層の密度は、好ましくは１．０～１０．５ｇ／ｃｍ３であり、より好ましくは１．３～３．０ｇ／ｃｍ３である。
The density of the transparent conductive layer is preferably 1.0 to 10.5 g / cm 3 , and more preferably 1.3 to 3.0 g / cm 3 .
前記透明導電層の表面抵抗値は、好ましくは０．１～１０００Ω／□であり、より好ましくは０．５～５００Ω／□であり、さらに好ましくは１～２５０Ω／□である。
The surface resistance value of the transparent conductive layer is preferably 0.1 to 1000 Ω / □, more preferably 0.5 to 500 Ω / □, and further preferably 1 to 250 Ω / □.
前記透明導電層の形成方法としては特に限定されず、従来公知の方法を採用することができる。具体的には、例えば、真空蒸着法、スパッタリング法、イオンプレーティング法を例示できる。また、必要とする膜厚に応じて適宜の方法を採用することもできる。
The method for forming the transparent conductive layer is not particularly limited, and a conventionally known method can be adopted. Specifically, for example, a vacuum deposition method, a sputtering method, and an ion plating method can be exemplified. Further, an appropriate method can be adopted depending on the required film thickness.
また、透明導電層と透明基材との間に、必要に応じて、アンダーコート層、オリゴマー防止層等を設けることができる。
Further, an undercoat layer, an oligomer prevention layer, etc. can be provided between the transparent conductive layer and the transparent base material, if necessary.
前記透明導電層は、タッチセンサを構成し、折り曲げ可能に構成されていることが要求される。
The transparent conductive layer constitutes a touch sensor and is required to be bendable.
本発明のフレキシブル画像表示装置用粘着型光学フィルムは、前記タッチセンサを構成する透明導電層を、前記第２の多層化粘着剤層に対して、前記位相差膜と接している面と反対側に配置することができる（図１参照）。
In the adhesive optical film for a flexible image display device of the present invention, the transparent conductive layer constituting the touch sensor is on the side opposite to the surface in contact with the retardation film with respect to the second multilayer adhesive layer. Can be placed in (see FIG. 1).
本発明のフレキシブル画像表示装置用粘着型光学フィルムは、前記タッチセンサを構成する透明導電層を、前記第１の多層化粘着剤層に対して、前記保護膜と接している面と反対側に配置させることができる（図２参照）。
In the adhesive optical film for a flexible image display device of the present invention, the transparent conductive layer constituting the touch sensor is placed on the side opposite to the surface in contact with the protective film with respect to the first multilayer adhesive layer. It can be arranged (see FIG. 2).
また、本発明のフレキシブル画像表示装置用粘着型光学フィルムは、前記タッチセンサを構成する透明導電層を、前記保護膜とウィンドウフィルム（ＯＣＡ）の間に配置することができる（図２参照）。
Further, in the adhesive optical film for a flexible image display device of the present invention, the transparent conductive layer constituting the touch sensor can be arranged between the protective film and the window film (OCA) (see FIG. 2).
前記透明導電層は、フレキシブル画像表示装置に用いられる場合として、インセル型またはオンセル型といったタッチセンサを内蔵した液晶表示装置に好適に適用することができ、特に、有機ＥＬ表示パネルにタッチセンサが内蔵（組み込まれていても）されてもよい。
The transparent conductive layer can be suitably applied to a liquid crystal display device having a built-in touch sensor such as an in-cell type or an on-cell type when used in a flexible image display device, and in particular, the touch sensor is built in an organic EL display panel. It may be (incorporated).
［導電性層（帯電防止層）］
また、本発明のフレキシブル画像表示装置用粘着型光学フィルムは、導電性を有する層（導電性層、帯電防止層）を有していても構わない。前記フレキシブル画像表示装置用粘着型光学フィルムは、屈曲機能を有し、非常に薄い厚み構成となるため、製造工程等で生じる微弱な静電気に対して反応性が大きく、ダメージを受けやすいが、前記粘着型光学フィルムに導電性層を設けることで、製造工程等での静電気による負荷が大きく軽減され、好ましい態様となる。 [Conductive layer (antistatic layer)]
Further, the adhesive optical film for a flexible image display device of the present invention may have a conductive layer (conductive layer, antistatic layer). Since the adhesive optical film for a flexible image display device has a bending function and has a very thin thickness structure, it is highly responsive to weak static electricity generated in a manufacturing process or the like and is easily damaged. By providing the conductive layer on the adhesive optical film, the load due to static electricity in the manufacturing process or the like is greatly reduced, which is a preferable embodiment.
また、本発明のフレキシブル画像表示装置用粘着型光学フィルムは、導電性を有する層（導電性層、帯電防止層）を有していても構わない。前記フレキシブル画像表示装置用粘着型光学フィルムは、屈曲機能を有し、非常に薄い厚み構成となるため、製造工程等で生じる微弱な静電気に対して反応性が大きく、ダメージを受けやすいが、前記粘着型光学フィルムに導電性層を設けることで、製造工程等での静電気による負荷が大きく軽減され、好ましい態様となる。 [Conductive layer (antistatic layer)]
Further, the adhesive optical film for a flexible image display device of the present invention may have a conductive layer (conductive layer, antistatic layer). Since the adhesive optical film for a flexible image display device has a bending function and has a very thin thickness structure, it is highly responsive to weak static electricity generated in a manufacturing process or the like and is easily damaged. By providing the conductive layer on the adhesive optical film, the load due to static electricity in the manufacturing process or the like is greatly reduced, which is a preferable embodiment.
また、前記粘着型光学フィルムを含むフレキシブル画像表示装置は、屈曲機能を有することが大きな特徴の１つであるが、連続屈曲させた場合に屈曲部のフィルム（基材）間の収縮により、静電気が生じる場合がある。そこで、前記粘着型光学フィルムに導電性を付与した場合、発生した静電気を速やかに取り除くことができ、画像表示装置の静電気によるダメージを軽減させることができ、好ましい態様となる。
Further, one of the major features of the flexible image display device including the adhesive optical film is that it has a bending function, but when it is continuously bent, static electricity is generated due to shrinkage between the films (base materials) of the bent portion. May occur. Therefore, when the adhesive optical film is imparted with conductivity, the generated static electricity can be quickly removed, and the damage caused by the static electricity of the image display device can be reduced, which is a preferable embodiment.
また、前記導電性層は、導電性機能をもつ下塗り層であってもよく、導電成分を含んだ粘着剤であってもよく、さらに導電成分を含んだ表面処理層であってもよい。例えば、ポリチオフェン等の導電性高分子及びバインダーを含有する帯電防止剤組成物を用いて、偏光フィルムと多層化粘着剤層との間に導電性層を形成する方法を採用することができる。更に、帯電防止剤であるイオン性化合物を含む粘着剤も用いることができる。また、前記導電性層は１層以上有することが好ましく、２層以上含んでいてもよい。
Further, the conductive layer may be an undercoat layer having a conductive function, an adhesive containing a conductive component, or a surface treatment layer containing a conductive component. For example, a method of forming a conductive layer between a polarizing film and a multilayer pressure-sensitive adhesive layer by using an antistatic agent composition containing a conductive polymer such as polythiophene and a binder can be adopted. Further, a pressure-sensitive adhesive containing an ionic compound which is an antistatic agent can also be used. Further, the conductive layer preferably has one or more layers, and may include two or more layers.
［フレキシブル画像表示装置］
本発明のフレキシブル画像表示装置は、上記のフレキシブル画像表示装置用粘着型光学フィルムと、有機ＥＬ表示パネルとを含み、有機ＥＬ表示パネルに対して視認側にフレキシブル画像表示装置用粘着型光学フィルムが配置され、折り曲げ可能に構成されている。任意ではあるが、フレキシブル画像表示装置用粘着型光学フィルムに対して視認側にウインドウを配置することができる（図１～図３参照）。 [Flexible image display device]
The flexible image display device of the present invention includes the above-mentioned adhesive optical film for a flexible image display device and an organic EL display panel, and the adhesive optical film for a flexible image display device is on the visual side with respect to the organic EL display panel. It is arranged and configured to be foldable. Although optional, a window can be arranged on the viewing side with respect to the adhesive optical film for a flexible image display device (see FIGS. 1 to 3).
本発明のフレキシブル画像表示装置は、上記のフレキシブル画像表示装置用粘着型光学フィルムと、有機ＥＬ表示パネルとを含み、有機ＥＬ表示パネルに対して視認側にフレキシブル画像表示装置用粘着型光学フィルムが配置され、折り曲げ可能に構成されている。任意ではあるが、フレキシブル画像表示装置用粘着型光学フィルムに対して視認側にウインドウを配置することができる（図１～図３参照）。 [Flexible image display device]
The flexible image display device of the present invention includes the above-mentioned adhesive optical film for a flexible image display device and an organic EL display panel, and the adhesive optical film for a flexible image display device is on the visual side with respect to the organic EL display panel. It is arranged and configured to be foldable. Although optional, a window can be arranged on the viewing side with respect to the adhesive optical film for a flexible image display device (see FIGS. 1 to 3).
図１は、本発明によるフレキシブル画像表示装置の１つの実施形態を示す断面図である。このフレキシブル画像表示装置１００は、フレキシブル画像表示装置用粘着型光学フィルム１１と、折り曲げ可能に構成された有機ＥＬ表示パネル１０を含む。そして、有機ＥＬ表示パネル１０に対して、視認側にフレキシブル画像表示装置用粘着型光学フィルム１１が配置され、フレキシブル画像表示装置１００は折り曲げ可能に構成されている。また、任意ではあるが、フレキシブル画像表示装置用粘着型光学フィルム１１に対して、視認側に透明なウインドウ４０が第１の多層化粘着剤層１２－１を介して配置させることができる。
FIG. 1 is a cross-sectional view showing one embodiment of the flexible image display device according to the present invention. The flexible image display device 100 includes an adhesive optical film 11 for a flexible image display device and an organic EL display panel 10 configured to be foldable. An adhesive optical film 11 for a flexible image display device is arranged on the visual side with respect to the organic EL display panel 10, and the flexible image display device 100 is configured to be bendable. Further, although optional, a transparent window 40 can be arranged on the visual side of the adhesive optical film 11 for a flexible image display device via the first multilayer adhesive layer 12-1.
フレキシブル画像表示装置用粘着型光学フィルム１１は、光学積層体２０と、更に、第２の多層化粘着剤層１２－２、及び、第３の多層化粘着剤層１２－３を構成する粘着剤層とを含む。
The adhesive optical film 11 for a flexible image display device comprises an optical laminate 20, a second multi-layered pressure-sensitive adhesive layer 12-2, and a third multi-layered pressure-sensitive adhesive layer 12-3. Including layers.
光学積層体２０は、偏光膜１、透明樹脂材料の保護膜２及び位相差膜３を含む。透明樹脂材料の保護膜２は、偏光膜１の視認側の第１面に接合される。位相差膜３は、偏光膜１の第１面とは異なる第２面に接合される。偏光膜１と位相差膜３は、例えば、偏光膜１の視認側から内部に入射した光が内部反射して視認側に射出されることを防止するために円偏光を生成したり、視野角を補償したりするためのものである。
The optical laminate 20 includes a polarizing film 1, a protective film 2 made of a transparent resin material, and a retardation film 3. The protective film 2 made of a transparent resin material is joined to the first surface of the polarizing film 1 on the visible side. The retardation film 3 is joined to a second surface different from the first surface of the polarizing film 1. The polarizing film 1 and the retardation film 3 generate circular polarization or have a viewing angle, for example, in order to prevent light incident on the inside of the polarizing film 1 from the viewing side from being internally reflected and emitted to the viewing side. It is for compensating for.
本実施形態においては、従来偏光膜の両面に保護膜が設けられていたのに対して、片面のみに保護膜が設けられる構成とされ、偏光膜自体も従来の有機ＥＬ表示装置に使用されている偏光膜に比べて、非常に薄い厚み（２０μｍ以下）の偏光膜が使用されることによって、光学積層体２０の厚みが低減することができる。また、偏光膜１は、従来の有機ＥＬ表示装置に使用されている偏光膜に比べて非常に薄いので、温度又は湿度条件で発生する伸縮による応力が極めて小さくなる。したがって、偏光膜の収縮によって生じる応力が隣接する有機ＥＬ表示パネル１０に反り等の変形を生じさせる可能性が大幅に軽減され、変形に起因する表示品質の低下やパネル封止材料の破壊を大幅に抑制することが可能になる。また、厚みの薄い偏光膜の使用により、屈曲を阻害することがなく、好ましい態様となる。
In the present embodiment, the protective film is provided on both sides of the conventional polarizing film, whereas the protective film is provided on only one side, and the polarizing film itself is also used in the conventional organic EL display device. The thickness of the optical laminate 20 can be reduced by using a polarizing film having a thickness very thin (20 μm or less) as compared with the polarizing film. Further, since the polarizing film 1 is much thinner than the polarizing film used in the conventional organic EL display device, the stress due to expansion and contraction generated under temperature or humidity conditions becomes extremely small. Therefore, the possibility that the stress caused by the shrinkage of the polarizing film causes deformation such as warpage in the adjacent organic EL display panel 10 is greatly reduced, and the deterioration of display quality and the destruction of the panel encapsulating material due to the deformation are greatly reduced. It becomes possible to suppress. Further, the use of a thin polarizing film does not hinder bending, which is a preferable embodiment.
光学積層体２０を、保護膜２側を内側として折り曲げる場合、光学積層体２０の厚み（例えば、９２μｍ以下）を薄くし、第１の多層化粘着剤層１２－１を保護膜２に対して位相差膜３とは反対側に配置することによって、光学積層体２０にかかる応力を低減することが可能となり、これにより光学積層体２０が折り曲げ可能となり、また、屈曲部において各層の割れや粘着剤層の剥がれを抑制することができ、最終的にフレキシブル画像表示装置用粘着型光学フィルム１１を折り曲げ可能とすることができる。
When the optical laminate 20 is bent with the protective film 2 side as the inside, the thickness of the optical laminate 20 (for example, 92 μm or less) is reduced, and the first multilayer adhesive layer 12-1 is applied to the protective film 2. By arranging it on the side opposite to the retardation film 3, it is possible to reduce the stress applied to the optical laminate 20, whereby the optical laminate 20 can be bent, and each layer is cracked or adhered at the bent portion. The peeling of the agent layer can be suppressed, and finally the adhesive optical film 11 for a flexible image display device can be bent.
任意ではあるが、位相差膜３に対して、保護膜２とは反対側に、タッチセンサを構成する折り曲げ可能な透明導電層６が更に配置されることができる。透明導電層６は、例えば特開２０１４－２１９６６７号公報に示されるような製造方法によって位相差膜３に直接接合される構成とし、これにより光学積層体２０の厚みが低減され、光学積層体２０を折り曲げた場合の光学積層体２０にかかる応力をより低減することができる。
Although optional, a bendable transparent conductive layer 6 constituting the touch sensor can be further arranged on the side opposite to the protective film 2 with respect to the retardation film 3. The transparent conductive layer 6 is configured to be directly bonded to the retardation film 3 by, for example, a manufacturing method as shown in Japanese Patent Application Laid-Open No. 2014-219667, whereby the thickness of the optical laminate 20 is reduced, and the optical laminate 20 is reduced. The stress applied to the optical laminate 20 when the product is bent can be further reduced.
任意ではあるが、透明導電層６に対して、位相差膜３とは反対側に、第３の多層化粘着剤層１２－３を構成する粘着剤層が更に配置されることができる。本実施形態においては、第２の多層化粘着剤層１２－２は、透明導電層６に直接接合されている。第２の多層化粘着剤層１２－２を設けることにより、光学積層体２０を折り曲げた場合の光学積層体２０にかかる応力をより低減することができる。
Although optional, the pressure-sensitive adhesive layer constituting the third multilayer pressure-sensitive adhesive layer 12-3 can be further arranged on the side opposite to the retardation film 3 with respect to the transparent conductive layer 6. In the present embodiment, the second multilayer pressure-sensitive adhesive layer 12-2 is directly bonded to the transparent conductive layer 6. By providing the second multilayer pressure-sensitive adhesive layer 12-2, the stress applied to the optical laminate 20 when the optical laminate 20 is bent can be further reduced.
図２に示すフレキシブル画像表示装置は、図１に示すものとほぼ同一であるが、図１のフレキシブル画像表示装置においては、位相差膜３に対して保護膜２とは反対側に、タッチセンサを構成する折り曲げ可能な透明導電層６が配置されるのに対して、図２のフレキシブル画像表示装置においては、第１の多層化粘着剤層１２－１に対して、前記保護膜２とは反対側に、タッチセンサを構成する折り曲げ可能な透明導電層６が配置される点で異なる。また、図１のフレキシブル画像表示装置においては、第３の多層化粘着剤層１２－３が、透明導電層６に対して位相差膜３とは反対側に配置されるのに対して、図２のフレキシブル画像表示装置においては、位相差膜３に対して保護膜２とは反対側に第２の多層化粘着剤層１２－２が配置される点で異なる。
The flexible image display device shown in FIG. 2 is almost the same as that shown in FIG. 1, but in the flexible image display device of FIG. 1, a touch sensor is located on the opposite side of the retardation film 3 from the protective film 2. In contrast to the foldable transparent conductive layer 6 that constitutes the above, in the flexible image display device of FIG. 2, the protective film 2 is different from the first multilayer pressure-sensitive adhesive layer 12-1. The difference is that the bendable transparent conductive layer 6 constituting the touch sensor is arranged on the opposite side. Further, in the flexible image display device of FIG. 1, the third multilayer pressure-sensitive adhesive layer 12-3 is arranged on the side opposite to the retardation film 3 with respect to the transparent conductive layer 6, whereas FIG. The flexible image display device of No. 2 is different in that the second multilayer adhesive layer 12-2 is arranged on the side opposite to the protective film 2 with respect to the retardation film 3.
また、任意ではあるが、フレキシブル画像表示装置用粘着型光学フィルム１１に対して、視認側にウインドウ４０が配置される場合に、第３の多層化粘着剤層１２－３を配置することができる。
Further, although optional, when the window 40 is arranged on the viewing side with respect to the adhesive optical film 11 for a flexible image display device, the third multilayer adhesive layer 12-3 can be arranged. ..
本発明のフレキシブル画像表示装置としては、フレキシブルの液晶表示装置、有機ＥＬ（エレクトロルミネッセンス）表示装置、電子ペーパーなどの画像表示装置として好適に用いることができる。また、抵抗膜方式や静電容量方式といったタッチパネル等の方式に関係なく使用することができる。
The flexible image display device of the present invention can be suitably used as a flexible liquid crystal display device, an organic EL (electroluminescence) display device, an image display device such as electronic paper, and the like. Further, it can be used regardless of a method such as a touch panel such as a resistance film method or a capacitance method.
また、本発明のフレキシブル画像表示装置としては、図３に示すように、タッチセンサを構成する透明導電層６が有機ＥＬ表示パネル１０－１に内蔵されたインセル型のフレキシブル画像表示装置としても使用することが可能である。
Further, as the flexible image display device of the present invention, as shown in FIG. 3, it is also used as an in-cell type flexible image display device in which the transparent conductive layer 6 constituting the touch sensor is built in the organic EL display panel 10-1. It is possible to do.
以下に、本発明の実施例を記載するが、本発明の実施形態はこれらに限定されない。
Examples of the present invention will be described below, but the embodiments of the present invention are not limited thereto.
製造例１
＜アクリル系粘着剤（Ａ）の調製＞
冷却管、窒素導入管、温度計及び撹拌装置を備えた反応容器に、アクリル酸ブチル９４．９質量部、アクリル酸５質量部、アクリル酸２－ヒドロキシエチル０．１質量部、及びジベンゾイルパーオキサイドを前記モノマー合計（固形分）１００質量部に対して０．３質量部を酢酸エチルと共に加えて、窒素ガス気流下、６０℃で７時間反応させた後、その反応液に酢酸エチルを加えて、重量平均分子量２２０万、分散比３．９のアクリル系ポリマー（Ａ）を含有する溶液を得た（固形分濃度３０％）。前記アクリル系ポリマー（Ａ）を含有する溶液の固形分１００質量部あたり、０．６質量部のトリメチロールプロパントリレンジイソシアネート（日本ポリウレタン工業（株）製：コロネートＬ）と、０．０７５質量部のγ－グリシドキシプロピルメトキシシラン（信越化学工業（株）製：ＫＢＭ－４０３）を配合して、アクリル系粘着剤（Ａ）を調製した。 Manufacturing example 1
<Preparation of acrylic adhesive (A)>
In a reaction vessel equipped with a cooling tube, a nitrogen introduction tube, a thermometer and a stirrer, 94.9 parts by mass of butyl acrylate, 5 parts by mass of acrylic acid, 0.1 part by mass of 2-hydroxyethyl acrylate, and dibenzoylper. 0.3 parts by mass of oxide was added together with ethyl acetate to 100 parts by mass of the total monomer (solid content), and the mixture was reacted at 60 ° C. for 7 hours under a nitrogen gas stream, and then ethyl acetate was added to the reaction solution. A solution containing an acrylic polymer (A) having a weight average molecular weight of 2.2 million and a dispersion ratio of 3.9 was obtained (solid content concentration: 30%). 0.6 parts by mass of trimethylolpropane tolylene diisocyanate (manufactured by Nippon Polyurethane Industry Co., Ltd .: Coronate L) and 0.075 parts by mass per 100 parts by mass of the solid content of the solution containing the acrylic polymer (A). Gamma-glycidoxypropylmethoxysilane (manufactured by Shin-Etsu Chemical Co., Ltd .: KBM-403) was blended to prepare an acrylic pressure-sensitive adhesive (A).
＜アクリル系粘着剤（Ａ）の調製＞
冷却管、窒素導入管、温度計及び撹拌装置を備えた反応容器に、アクリル酸ブチル９４．９質量部、アクリル酸５質量部、アクリル酸２－ヒドロキシエチル０．１質量部、及びジベンゾイルパーオキサイドを前記モノマー合計（固形分）１００質量部に対して０．３質量部を酢酸エチルと共に加えて、窒素ガス気流下、６０℃で７時間反応させた後、その反応液に酢酸エチルを加えて、重量平均分子量２２０万、分散比３．９のアクリル系ポリマー（Ａ）を含有する溶液を得た（固形分濃度３０％）。前記アクリル系ポリマー（Ａ）を含有する溶液の固形分１００質量部あたり、０．６質量部のトリメチロールプロパントリレンジイソシアネート（日本ポリウレタン工業（株）製：コロネートＬ）と、０．０７５質量部のγ－グリシドキシプロピルメトキシシラン（信越化学工業（株）製：ＫＢＭ－４０３）を配合して、アクリル系粘着剤（Ａ）を調製した。 Manufacturing example 1
<Preparation of acrylic adhesive (A)>
In a reaction vessel equipped with a cooling tube, a nitrogen introduction tube, a thermometer and a stirrer, 94.9 parts by mass of butyl acrylate, 5 parts by mass of acrylic acid, 0.1 part by mass of 2-hydroxyethyl acrylate, and dibenzoylper. 0.3 parts by mass of oxide was added together with ethyl acetate to 100 parts by mass of the total monomer (solid content), and the mixture was reacted at 60 ° C. for 7 hours under a nitrogen gas stream, and then ethyl acetate was added to the reaction solution. A solution containing an acrylic polymer (A) having a weight average molecular weight of 2.2 million and a dispersion ratio of 3.9 was obtained (solid content concentration: 30%). 0.6 parts by mass of trimethylolpropane tolylene diisocyanate (manufactured by Nippon Polyurethane Industry Co., Ltd .: Coronate L) and 0.075 parts by mass per 100 parts by mass of the solid content of the solution containing the acrylic polymer (A). Gamma-glycidoxypropylmethoxysilane (manufactured by Shin-Etsu Chemical Co., Ltd .: KBM-403) was blended to prepare an acrylic pressure-sensitive adhesive (A).
製造例２
＜アクリル系粘着剤（Ｂ）の調製＞
冷却管、窒素導入管、温度計及び撹拌装置を備えた反応容器に、アクリル酸ブチル９９質量部、アクリル酸４－ヒドロキシブチル１質量部、及び２，２－アゾビスイソブチロニトリルを前記モノマー合計（固形分）１００質量部に対して０．３質量部を酢酸エチルと共に加えて、窒素ガス気流下、６０℃で４時間反応させた後、その反応液に酢酸エチルを加えて、重量平均分子量１７０万、分散比４．１のアクリル系ポリマー（Ｂ）を含有する溶液を得た（固形分濃度３０％）。前記アクリル系ポリマー（Ｂ）を含有する溶液の固形分１００質量部あたり、０．１５質量部のトリメチロールプロパンキシリレンジイソシアネート（三井武田ケミカル（株）：タケネートＤ１１０Ｎ）と、０．２質量部のシランカップリング剤（綜研化学（株）製：Ａ－１００、アセトアセチル基含有シランカップリング剤）を配合して、アクリル系粘着剤（Ｂ）を調製した。 Manufacturing example 2
<Preparation of acrylic adhesive (B)>
In a reaction vessel equipped with a cooling tube, a nitrogen introduction tube, a thermometer and a stirrer, 99 parts by mass of butyl acrylate, 1 part by mass of 4-hydroxybutyl acrylate, and 2,2-azobisisobutyronitrile were added to the monomer. 0.3 parts by mass is added together with ethyl acetate to 100 parts by mass of the total (solid content), and the mixture is reacted at 60 ° C. for 4 hours under a nitrogen gas stream, and then ethyl acetate is added to the reaction solution and weight averaged. A solution containing an acrylic polymer (B) having a molecular weight of 1.7 million and a dispersion ratio of 4.1 was obtained (solid content concentration: 30%). 0.15 parts by mass of trimethylolpropane xylylene diisocyanate (Mitsui Takeda Pharmaceutical Co., Ltd .: Takeda D110N) and 0.2 parts by mass of trimethylolpropane xylylene diisocyanate per 100 parts by mass of the solid content of the solution containing the acrylic polymer (B). An acrylic pressure-sensitive adhesive (B) was prepared by blending a silane coupling agent (manufactured by Soken Kagaku Co., Ltd .: A-100, an acetoacetyl group-containing silane coupling agent).
＜アクリル系粘着剤（Ｂ）の調製＞
冷却管、窒素導入管、温度計及び撹拌装置を備えた反応容器に、アクリル酸ブチル９９質量部、アクリル酸４－ヒドロキシブチル１質量部、及び２，２－アゾビスイソブチロニトリルを前記モノマー合計（固形分）１００質量部に対して０．３質量部を酢酸エチルと共に加えて、窒素ガス気流下、６０℃で４時間反応させた後、その反応液に酢酸エチルを加えて、重量平均分子量１７０万、分散比４．１のアクリル系ポリマー（Ｂ）を含有する溶液を得た（固形分濃度３０％）。前記アクリル系ポリマー（Ｂ）を含有する溶液の固形分１００質量部あたり、０．１５質量部のトリメチロールプロパンキシリレンジイソシアネート（三井武田ケミカル（株）：タケネートＤ１１０Ｎ）と、０．２質量部のシランカップリング剤（綜研化学（株）製：Ａ－１００、アセトアセチル基含有シランカップリング剤）を配合して、アクリル系粘着剤（Ｂ）を調製した。 Manufacturing example 2
<Preparation of acrylic adhesive (B)>
In a reaction vessel equipped with a cooling tube, a nitrogen introduction tube, a thermometer and a stirrer, 99 parts by mass of butyl acrylate, 1 part by mass of 4-hydroxybutyl acrylate, and 2,2-azobisisobutyronitrile were added to the monomer. 0.3 parts by mass is added together with ethyl acetate to 100 parts by mass of the total (solid content), and the mixture is reacted at 60 ° C. for 4 hours under a nitrogen gas stream, and then ethyl acetate is added to the reaction solution and weight averaged. A solution containing an acrylic polymer (B) having a molecular weight of 1.7 million and a dispersion ratio of 4.1 was obtained (solid content concentration: 30%). 0.15 parts by mass of trimethylolpropane xylylene diisocyanate (Mitsui Takeda Pharmaceutical Co., Ltd .: Takeda D110N) and 0.2 parts by mass of trimethylolpropane xylylene diisocyanate per 100 parts by mass of the solid content of the solution containing the acrylic polymer (B). An acrylic pressure-sensitive adhesive (B) was prepared by blending a silane coupling agent (manufactured by Soken Kagaku Co., Ltd .: A-100, an acetoacetyl group-containing silane coupling agent).
実施例１
＜セパレータ／第１粘着剤層／第２粘着剤層／セパレータからなるセパレータ付き多層化粘着剤層の作製＞
離型処理を施したポリエステルフィルム（セパレータ、三菱化学ポリエステル社製、商品名：ダイヤホイルＭＲＦ＃３８、厚さ３８μｍ）の離型処理面上に、製造例１で調製したアクリル系粘着剤（Ａ）を、乾燥厚さが１５μｍになるようにダイコーターで塗工した。その後、９５℃のオーブン中にて、風速５ｍ／秒の風を１５秒間送ることにより第１乾燥工程を施した。次いで、７５℃のオーブン中にて、風速５ｍ／秒の風を６０秒間送ることにより第２乾燥工程を施した。さらに、１５５℃のオーブン中にて、風速２０ｍ／秒の風を４５秒間送ることにより第３乾燥工程を施し、セパレータ上に第１粘着剤層を形成した。同様の方法で、セパレータ上に第２粘着剤層を形成した。そして、セパレータ上の第１粘着剤層とセパレータ上の第２粘着剤層を互いに貼り合わせて、セパレータ／第１粘着剤層／第２粘着剤層／セパレータからなるセパレータ付き多層化粘着剤層を作製した。 Example 1
<Preparation of a multilayer pressure-sensitive adhesive layer with a separator consisting of a separator / first pressure-sensitive adhesive layer / second pressure-sensitive adhesive layer / separator>
The acrylic adhesive (A) prepared in Production Example 1 on the release-treated surface of a release-treated polyester film (separator, manufactured by Mitsubishi Chemical Polyester, trade name: diamond foil MRF # 38, thickness 38 μm). ) Was coated with a die coater so that the dry thickness was 15 μm. Then, the first drying step was performed by sending a wind having a wind speed of 5 m / sec for 15 seconds in an oven at 95 ° C. Then, in an oven at 75 ° C., a second drying step was performed by sending a wind having a wind speed of 5 m / sec for 60 seconds. Further, in an oven at 155 ° C., a third drying step was performed by sending a wind having a wind speed of 20 m / sec for 45 seconds to form a first pressure-sensitive adhesive layer on the separator. A second pressure-sensitive adhesive layer was formed on the separator in the same manner. Then, the first pressure-sensitive adhesive layer on the separator and the second pressure-sensitive adhesive layer on the separator are bonded to each other to form a multilayer pressure-sensitive adhesive layer with a separator composed of a separator / first pressure-sensitive adhesive layer / second pressure-sensitive adhesive layer / separator. Made.
＜セパレータ／第１粘着剤層／第２粘着剤層／セパレータからなるセパレータ付き多層化粘着剤層の作製＞
離型処理を施したポリエステルフィルム（セパレータ、三菱化学ポリエステル社製、商品名：ダイヤホイルＭＲＦ＃３８、厚さ３８μｍ）の離型処理面上に、製造例１で調製したアクリル系粘着剤（Ａ）を、乾燥厚さが１５μｍになるようにダイコーターで塗工した。その後、９５℃のオーブン中にて、風速５ｍ／秒の風を１５秒間送ることにより第１乾燥工程を施した。次いで、７５℃のオーブン中にて、風速５ｍ／秒の風を６０秒間送ることにより第２乾燥工程を施した。さらに、１５５℃のオーブン中にて、風速２０ｍ／秒の風を４５秒間送ることにより第３乾燥工程を施し、セパレータ上に第１粘着剤層を形成した。同様の方法で、セパレータ上に第２粘着剤層を形成した。そして、セパレータ上の第１粘着剤層とセパレータ上の第２粘着剤層を互いに貼り合わせて、セパレータ／第１粘着剤層／第２粘着剤層／セパレータからなるセパレータ付き多層化粘着剤層を作製した。 Example 1
<Preparation of a multilayer pressure-sensitive adhesive layer with a separator consisting of a separator / first pressure-sensitive adhesive layer / second pressure-sensitive adhesive layer / separator>
The acrylic adhesive (A) prepared in Production Example 1 on the release-treated surface of a release-treated polyester film (separator, manufactured by Mitsubishi Chemical Polyester, trade name: diamond foil MRF # 38, thickness 38 μm). ) Was coated with a die coater so that the dry thickness was 15 μm. Then, the first drying step was performed by sending a wind having a wind speed of 5 m / sec for 15 seconds in an oven at 95 ° C. Then, in an oven at 75 ° C., a second drying step was performed by sending a wind having a wind speed of 5 m / sec for 60 seconds. Further, in an oven at 155 ° C., a third drying step was performed by sending a wind having a wind speed of 20 m / sec for 45 seconds to form a first pressure-sensitive adhesive layer on the separator. A second pressure-sensitive adhesive layer was formed on the separator in the same manner. Then, the first pressure-sensitive adhesive layer on the separator and the second pressure-sensitive adhesive layer on the separator are bonded to each other to form a multilayer pressure-sensitive adhesive layer with a separator composed of a separator / first pressure-sensitive adhesive layer / second pressure-sensitive adhesive layer / separator. Made.
実施例２～８
表１に記載のアクリル系粘着剤、第１粘着剤層及び第２粘着剤層の厚み、及び乾燥工程における乾燥条件を採用した以外は、実施例１と同様の方法で、セパレータ付き多層化粘着剤層を作製した。 Examples 2-8
Multi-layer adhesive with separator in the same manner as in Example 1 except that the acrylic pressure-sensitive adhesive shown in Table 1, the thicknesses of the first pressure-sensitive adhesive layer and the second pressure-sensitive adhesive layer, and the drying conditions in the drying step were adopted. An agent layer was prepared.
表１に記載のアクリル系粘着剤、第１粘着剤層及び第２粘着剤層の厚み、及び乾燥工程における乾燥条件を採用した以外は、実施例１と同様の方法で、セパレータ付き多層化粘着剤層を作製した。 Examples 2-8
Multi-layer adhesive with separator in the same manner as in Example 1 except that the acrylic pressure-sensitive adhesive shown in Table 1, the thicknesses of the first pressure-sensitive adhesive layer and the second pressure-sensitive adhesive layer, and the drying conditions in the drying step were adopted. An agent layer was prepared.
比較例１
＜セパレータ／粘着剤層からなるセパレータ付き粘着剤層の作製＞
離型処理を施したポリエステルフィルム（セパレータ、三菱化学ポリエステル社製、商品名：ダイヤホイルＭＲＦ＃３８、厚さ３８μｍ）の離型処理面上に、製造例１で調製したアクリル系粘着剤（Ａ）を、乾燥厚さが３０μｍになるようにダイコーターで塗工した。その後、１１５℃のオーブン中にて、風速８ｍ／秒の風を１５秒間送ることにより第１乾燥工程を施した。次いで、９０℃のオーブン中にて、風速８ｍ／秒の風を６０秒間送ることにより第２乾燥工程を施した。さらに、１５５℃のオーブン中にて、風速２０ｍ／秒の風を４５秒間送ることにより第３乾燥工程を施し、セパレータ上に粘着剤層を形成し、セパレータ／粘着剤層からなるセパレータ付き粘着剤層を作製した。 Comparative Example 1
<Preparation of a pressure-sensitive adhesive layer with a separator consisting of a separator / pressure-sensitive adhesive layer>
The acrylic adhesive (A) prepared in Production Example 1 on the release-treated surface of a release-treated polyester film (separator, manufactured by Mitsubishi Chemical Polyester, trade name: diamond foil MRF # 38, thickness 38 μm). ) Was coated with a die coater so that the dry thickness was 30 μm. Then, the first drying step was performed by sending a wind having a wind speed of 8 m / sec for 15 seconds in an oven at 115 ° C. Then, in an oven at 90 ° C., a second drying step was performed by sending a wind having a wind speed of 8 m / sec for 60 seconds. Further, in an oven at 155 ° C., a third drying step is performed by sending a wind at a wind speed of 20 m / sec for 45 seconds to form an adhesive layer on the separator, and the adhesive having a separator composed of the separator / adhesive layer. Layers were made.
＜セパレータ／粘着剤層からなるセパレータ付き粘着剤層の作製＞
離型処理を施したポリエステルフィルム（セパレータ、三菱化学ポリエステル社製、商品名：ダイヤホイルＭＲＦ＃３８、厚さ３８μｍ）の離型処理面上に、製造例１で調製したアクリル系粘着剤（Ａ）を、乾燥厚さが３０μｍになるようにダイコーターで塗工した。その後、１１５℃のオーブン中にて、風速８ｍ／秒の風を１５秒間送ることにより第１乾燥工程を施した。次いで、９０℃のオーブン中にて、風速８ｍ／秒の風を６０秒間送ることにより第２乾燥工程を施した。さらに、１５５℃のオーブン中にて、風速２０ｍ／秒の風を４５秒間送ることにより第３乾燥工程を施し、セパレータ上に粘着剤層を形成し、セパレータ／粘着剤層からなるセパレータ付き粘着剤層を作製した。 Comparative Example 1
<Preparation of a pressure-sensitive adhesive layer with a separator consisting of a separator / pressure-sensitive adhesive layer>
The acrylic adhesive (A) prepared in Production Example 1 on the release-treated surface of a release-treated polyester film (separator, manufactured by Mitsubishi Chemical Polyester, trade name: diamond foil MRF # 38, thickness 38 μm). ) Was coated with a die coater so that the dry thickness was 30 μm. Then, the first drying step was performed by sending a wind having a wind speed of 8 m / sec for 15 seconds in an oven at 115 ° C. Then, in an oven at 90 ° C., a second drying step was performed by sending a wind having a wind speed of 8 m / sec for 60 seconds. Further, in an oven at 155 ° C., a third drying step is performed by sending a wind at a wind speed of 20 m / sec for 45 seconds to form an adhesive layer on the separator, and the adhesive having a separator composed of the separator / adhesive layer. Layers were made.
比較例２～４
表１に記載のアクリル系粘着剤、粘着剤層の厚み、及び乾燥工程における乾燥条件を採用した以外は、比較例１と同様の方法で、セパレータ付き粘着剤層を作製した。 Comparative Examples 2-4
A pressure-sensitive adhesive layer with a separator was prepared in the same manner as in Comparative Example 1 except that the acrylic pressure-sensitive adhesive shown in Table 1, the thickness of the pressure-sensitive adhesive layer, and the drying conditions in the drying step were adopted.
表１に記載のアクリル系粘着剤、粘着剤層の厚み、及び乾燥工程における乾燥条件を採用した以外は、比較例１と同様の方法で、セパレータ付き粘着剤層を作製した。 Comparative Examples 2-4
A pressure-sensitive adhesive layer with a separator was prepared in the same manner as in Comparative Example 1 except that the acrylic pressure-sensitive adhesive shown in Table 1, the thickness of the pressure-sensitive adhesive layer, and the drying conditions in the drying step were adopted.
〔評価方法〕
＜ＩＳＣ－Ｓ値＞
（株）アイ・システム製のＥｙｅＳｃａｌｅ－４Ｗを用いて、当該装置の仕様に基づいて、３ＣＣＤイメージセンサーのＩＳＣ－Ｓ測定モードにて、粘着剤層の面内のムラのレベルをＩＳＣ－Ｓ値として算出した。
（測定条件）
実施例１～８で作製したセパレータ付き多層化粘着剤層の一方のセパレータを剥離し、粘着面に無アルカリガラス板（コーニング社製、１７３７）を貼り合わせた後、他方のセパレータを剥離した。そして、他方のセパレータを剥離した粘着面を専用治具に貼り付けた状態のものをサンプルとして用いた。また、比較例１～４で作製したセパレータ付き粘着剤層の粘着面に無アルカリガラス板（コーニング社製、１７３７）を貼り合わせた後、セパレータを剥離した。そして、セパレータを剥離した粘着面を専用治具に貼り付けた状態のものをサンプルとして用いた。なお、使用した前記無アルカリガラス板は、ＩＳＣ－Ｓ値に影響を与えないものである。
光源、サンプル(光源が粘着面側)、スクリーンをこの順で設置して、スクリーンに投影された、サンプルの透過画像をＣＣＤカメラにより測定した。光源およびＣＣＤカメラからサンプル（無アルカリガラス板に貼り付けた粘着剤層）までの距離は３０ｃｍになるように配置した。また光源およびＣＣＤカメラからスクリーンまで距離は１００ｃｍになるように配置した。光源およびＣＣＤカメラは、サンプル、スクリーンからの距離が同じになるように２０ｃｍ離して設置した。ＩＳＣ－Ｓ値は、スジムラの評価に係わり、ＩＳＣ－Ｓ値が５０以下であればムラを小さく制御できていると判断できる。 〔Evaluation method〕
<ISC-S value>
Using EyeScale-4W manufactured by Eye System Co., Ltd., the level of in-plane unevenness of the adhesive layer is set to the ISC-S value in the ISC-S measurement mode of the 3CCD image sensor based on the specifications of the device. It was calculated as.
(Measurement condition)
One separator of the multilayer pressure-sensitive adhesive layer with a separator prepared in Examples 1 to 8 was peeled off, a non-alkali glass plate (1737 manufactured by Corning Inc.) was attached to the adhesive surface, and then the other separator was peeled off. Then, the one in which the adhesive surface from which the other separator was peeled off was attached to a special jig was used as a sample. Further, a non-alkali glass plate (1737 manufactured by Corning Inc.) was attached to the adhesive surface of the adhesive layer with a separator prepared in Comparative Examples 1 to 4, and then the separator was peeled off. Then, the one in which the adhesive surface from which the separator was peeled off was attached to a special jig was used as a sample. The non-alkali glass plate used does not affect the ISC-S value.
A light source, a sample (the light source is on the adhesive side), and a screen were installed in this order, and a transmitted image of the sample projected on the screen was measured by a CCD camera. The distance from the light source and the CCD camera to the sample (adhesive layer attached to the non-alkali glass plate) was 30 cm. The distance from the light source and the CCD camera to the screen was 100 cm. The light source and the CCD camera were installed 20 cm apart so that the distance from the sample and the screen was the same. The ISC-S value is related to the evaluation of Sujimura, and if the ISC-S value is 50 or less, it can be determined that the unevenness can be controlled to be small.
＜ＩＳＣ－Ｓ値＞
（株）アイ・システム製のＥｙｅＳｃａｌｅ－４Ｗを用いて、当該装置の仕様に基づいて、３ＣＣＤイメージセンサーのＩＳＣ－Ｓ測定モードにて、粘着剤層の面内のムラのレベルをＩＳＣ－Ｓ値として算出した。
（測定条件）
実施例１～８で作製したセパレータ付き多層化粘着剤層の一方のセパレータを剥離し、粘着面に無アルカリガラス板（コーニング社製、１７３７）を貼り合わせた後、他方のセパレータを剥離した。そして、他方のセパレータを剥離した粘着面を専用治具に貼り付けた状態のものをサンプルとして用いた。また、比較例１～４で作製したセパレータ付き粘着剤層の粘着面に無アルカリガラス板（コーニング社製、１７３７）を貼り合わせた後、セパレータを剥離した。そして、セパレータを剥離した粘着面を専用治具に貼り付けた状態のものをサンプルとして用いた。なお、使用した前記無アルカリガラス板は、ＩＳＣ－Ｓ値に影響を与えないものである。
光源、サンプル(光源が粘着面側)、スクリーンをこの順で設置して、スクリーンに投影された、サンプルの透過画像をＣＣＤカメラにより測定した。光源およびＣＣＤカメラからサンプル（無アルカリガラス板に貼り付けた粘着剤層）までの距離は３０ｃｍになるように配置した。また光源およびＣＣＤカメラからスクリーンまで距離は１００ｃｍになるように配置した。光源およびＣＣＤカメラは、サンプル、スクリーンからの距離が同じになるように２０ｃｍ離して設置した。ＩＳＣ－Ｓ値は、スジムラの評価に係わり、ＩＳＣ－Ｓ値が５０以下であればムラを小さく制御できていると判断できる。 〔Evaluation method〕
<ISC-S value>
Using EyeScale-4W manufactured by Eye System Co., Ltd., the level of in-plane unevenness of the adhesive layer is set to the ISC-S value in the ISC-S measurement mode of the 3CCD image sensor based on the specifications of the device. It was calculated as.
(Measurement condition)
One separator of the multilayer pressure-sensitive adhesive layer with a separator prepared in Examples 1 to 8 was peeled off, a non-alkali glass plate (1737 manufactured by Corning Inc.) was attached to the adhesive surface, and then the other separator was peeled off. Then, the one in which the adhesive surface from which the other separator was peeled off was attached to a special jig was used as a sample. Further, a non-alkali glass plate (1737 manufactured by Corning Inc.) was attached to the adhesive surface of the adhesive layer with a separator prepared in Comparative Examples 1 to 4, and then the separator was peeled off. Then, the one in which the adhesive surface from which the separator was peeled off was attached to a special jig was used as a sample. The non-alkali glass plate used does not affect the ISC-S value.
A light source, a sample (the light source is on the adhesive side), and a screen were installed in this order, and a transmitted image of the sample projected on the screen was measured by a CCD camera. The distance from the light source and the CCD camera to the sample (adhesive layer attached to the non-alkali glass plate) was 30 cm. The distance from the light source and the CCD camera to the screen was 100 cm. The light source and the CCD camera were installed 20 cm apart so that the distance from the sample and the screen was the same. The ISC-S value is related to the evaluation of Sujimura, and if the ISC-S value is 50 or less, it can be determined that the unevenness can be controlled to be small.
＜セパレータ剥離力＞
実施例１～８で作製したセパレータ付き多層化粘着剤層の一方のセパレータを剥離し、粘着面に光学フィルム（特開２０１９－１９１２８２号公報の実施例１に記載の位相差層付き偏光板）を貼り合わせて、セパレータ／多層化粘着剤層／光学フィルムからなるセパレータ付き粘着型光学フィルムを作製した。また、比較例１～４で作製したセパレータ付き粘着剤層の粘着面に前記光学フィルムを貼り合わせて、セパレータ／粘着剤層／光学フィルムからなるセパレータ付き粘着型光学フィルムを作製した。
作製したセパレータ付き粘着型光学フィルムを５０ｍｍ×１００ｍｍの大きさに切断して測定用サンプルとした。測定用サンプルを、光学フィルム側を下にして、両面テープを介して平板状の剥離治具に貼り合せた。次いで、測定用サンプルの短辺からセパレータと粘着剤層を剥離し、セパレータをチャックし、引張り試験機を用いて引張り、剥離力（Ｎ／５０ｍｍ）の測定を行った（引張方向：光学フィルムの表面に対して１８０°、引張速度：３００ｍｍ／ｍｉｎ）。５個の測定用サンプルについて剥離力を測定し、各測定用サンプルの測定値の平均値をセパレータ剥離力（Ｎ／５０ｍｍ）として採用した。 <Separator peeling force>
One of the separators of the multilayer pressure-sensitive adhesive layer with a separator prepared in Examples 1 to 8 is peeled off, and an optical film is formed on the adhesive surface (the polarizing plate with a retardation layer according to Example 1 of JP-A-2019-191282). To prepare an adhesive optical film with a separator composed of a separator / a multilayer adhesive layer / an optical film. Further, the optical film was attached to the adhesive surface of the adhesive layer with a separator prepared in Comparative Examples 1 to 4 to prepare an adhesive optical film with a separator composed of a separator / an adhesive layer / an optical film.
The produced adhesive optical film with a separator was cut into a size of 50 mm × 100 mm to prepare a measurement sample. The measurement sample was attached to a flat plate-shaped peeling jig via a double-sided tape with the optical film side facing down. Next, the separator and the pressure-sensitive adhesive layer were peeled off from the short side of the measurement sample, the separator was chucked, pulled by a tensile tester, and the peeling force (N / 50 mm) was measured (tensile direction: optical film). 180 ° to the surface, tensile speed: 300 mm / min). The peeling force was measured for five measuring samples, and the average value of the measured values of each measuring sample was adopted as the separator peeling force (N / 50 mm).
実施例１～８で作製したセパレータ付き多層化粘着剤層の一方のセパレータを剥離し、粘着面に光学フィルム（特開２０１９－１９１２８２号公報の実施例１に記載の位相差層付き偏光板）を貼り合わせて、セパレータ／多層化粘着剤層／光学フィルムからなるセパレータ付き粘着型光学フィルムを作製した。また、比較例１～４で作製したセパレータ付き粘着剤層の粘着面に前記光学フィルムを貼り合わせて、セパレータ／粘着剤層／光学フィルムからなるセパレータ付き粘着型光学フィルムを作製した。
作製したセパレータ付き粘着型光学フィルムを５０ｍｍ×１００ｍｍの大きさに切断して測定用サンプルとした。測定用サンプルを、光学フィルム側を下にして、両面テープを介して平板状の剥離治具に貼り合せた。次いで、測定用サンプルの短辺からセパレータと粘着剤層を剥離し、セパレータをチャックし、引張り試験機を用いて引張り、剥離力（Ｎ／５０ｍｍ）の測定を行った（引張方向：光学フィルムの表面に対して１８０°、引張速度：３００ｍｍ／ｍｉｎ）。５個の測定用サンプルについて剥離力を測定し、各測定用サンプルの測定値の平均値をセパレータ剥離力（Ｎ／５０ｍｍ）として採用した。 <Separator peeling force>
One of the separators of the multilayer pressure-sensitive adhesive layer with a separator prepared in Examples 1 to 8 is peeled off, and an optical film is formed on the adhesive surface (the polarizing plate with a retardation layer according to Example 1 of JP-A-2019-191282). To prepare an adhesive optical film with a separator composed of a separator / a multilayer adhesive layer / an optical film. Further, the optical film was attached to the adhesive surface of the adhesive layer with a separator prepared in Comparative Examples 1 to 4 to prepare an adhesive optical film with a separator composed of a separator / an adhesive layer / an optical film.
The produced adhesive optical film with a separator was cut into a size of 50 mm × 100 mm to prepare a measurement sample. The measurement sample was attached to a flat plate-shaped peeling jig via a double-sided tape with the optical film side facing down. Next, the separator and the pressure-sensitive adhesive layer were peeled off from the short side of the measurement sample, the separator was chucked, pulled by a tensile tester, and the peeling force (N / 50 mm) was measured (tensile direction: optical film). 180 ° to the surface, tensile speed: 300 mm / min). The peeling force was measured for five measuring samples, and the average value of the measured values of each measuring sample was adopted as the separator peeling force (N / 50 mm).
表１から、実施例１～８で作製したセパレータ付き多層化粘着剤層の多層化粘着剤層は、厚手化されているにもかかわらず、ＩＳＣ－Ｓ値が５０以下であり、視認性に影響を与える表面ムラが抑制されていることがわかる。一方、比較例１～４で作製したセパレータ付き粘着剤層は、厚手化されているが、ＩＳＣ－Ｓ値が５０を大きく超えており、視認性に影響を与える表面ムラが多く生じていることがわかる。
From Table 1, the multi-layered pressure-sensitive adhesive layer of the multi-layered pressure-sensitive adhesive layer with a separator produced in Examples 1 to 8 has an ISC-S value of 50 or less even though it is thickened, and has high visibility. It can be seen that the affecting surface unevenness is suppressed. On the other hand, the pressure-sensitive adhesive layers with separators produced in Comparative Examples 1 to 4 are thickened, but the ISC-S value greatly exceeds 50, and many surface irregularities that affect visibility occur. I understand.
本発明の多層化粘着剤層等は、液晶表示装置（ＬＣＤ）、有機ＥＬ表示装置、ＣＲＴ、及びＰＤＰなどの画像表示装置の構成部材として有用である。
The multi-layered pressure-sensitive adhesive layer of the present invention is useful as a constituent member of an image display device such as a liquid crystal display device (LCD), an organic EL display device, a CRT, and a PDP.
１ 偏光膜
２ 保護膜
３ 位相差層
６ 透明導電層
８ 透明基材
１０ 有機ＥＬ表示パネル
１０－１ 有機ＥＬ表示パネル（タッチセンサ付き）
１１ フレキシブル画像表示装置用粘着型光学フィルム（有機ＥＬ表示装置用粘着型光学フィルム）
１２－１ 第１の多層化粘着剤層
１２－２ 第２の多層化粘着剤層
１２－３ 第３の多層化粘着剤層
１３ 加飾印刷フィルム
２０ 光学積層体
４０ ウインドウ
１００ フレキシブル画像表示装置（有機ＥＬ表示装置） 1 Polarizingfilm 2 Protective film 3 Phase difference layer 6 Transparent conductive layer 8 Transparent base material 10 Organic EL display panel 10-1 Organic EL display panel (with touch sensor)
11 Adhesive optical film for flexible image display device (Adhesive optical film for organic EL display device)
12-1 First Multilayer Adhesive Layer 12-2 Second Multilayer Adhesive Layer 12-3 ThirdMultilayer Adhesive Layer 13 Decorative Printing Film 20 Optical Laminate 40 Window 100 Flexible Image Display Device ( Organic EL display device)
２ 保護膜
３ 位相差層
６ 透明導電層
８ 透明基材
１０ 有機ＥＬ表示パネル
１０－１ 有機ＥＬ表示パネル（タッチセンサ付き）
１１ フレキシブル画像表示装置用粘着型光学フィルム（有機ＥＬ表示装置用粘着型光学フィルム）
１２－１ 第１の多層化粘着剤層
１２－２ 第２の多層化粘着剤層
１２－３ 第３の多層化粘着剤層
１３ 加飾印刷フィルム
２０ 光学積層体
４０ ウインドウ
１００ フレキシブル画像表示装置（有機ＥＬ表示装置） 1 Polarizing
11 Adhesive optical film for flexible image display device (Adhesive optical film for organic EL display device)
12-1 First Multilayer Adhesive Layer 12-2 Second Multilayer Adhesive Layer 12-3 Third
Claims (13)
- ２層以上の粘着剤層が直接積層されている多層化粘着剤層であって、
前記粘着剤層は、それぞれ厚みが１０～２０μｍであり、
前記多層化粘着剤層は、総厚みが２０～１００μｍであり、かつ
前記多層化粘着剤層は、ＩＳＣ－Ｓ値が５０以下であることを特徴とする多層化粘着剤層。 A multi-layered pressure-sensitive adhesive layer in which two or more pressure-sensitive adhesive layers are directly laminated.
Each of the pressure-sensitive adhesive layers has a thickness of 10 to 20 μm, and has a thickness of 10 to 20 μm.
The multi-layered pressure-sensitive adhesive layer has a total thickness of 20 to 100 μm, and the multi-layered pressure-sensitive adhesive layer has an ISC-S value of 50 or less. - 前記多層化粘着剤層は、少なくとも直接積層されている第１粘着剤層と第２粘着剤層を含み、
前記第１粘着剤層の形成材料である粘着剤組成物は、（メタ）アクリル系ポリマーＡを含み、
前記第２粘着剤層の形成材料である粘着剤組成物は、（メタ）アクリル系ポリマーＢを含み、
前記（メタ）アクリル系ポリマーＡの形成材料であるモノマー組成物と前記（メタ）アクリル系ポリマーＢの形成材料であるモノマー組成物は、炭素数１～１８のアルキル基を有するアルキル（メタ）アクリレートを５０質量％以上含む、請求項１に記載の多層化粘着剤層。 The multilayered pressure-sensitive adhesive layer includes at least a first pressure-sensitive adhesive layer and a second pressure-sensitive adhesive layer that are directly laminated.
The pressure-sensitive adhesive composition, which is a material for forming the first pressure-sensitive adhesive layer, contains a (meth) acrylic polymer A and contains.
The pressure-sensitive adhesive composition, which is a material for forming the second pressure-sensitive adhesive layer, contains a (meth) acrylic polymer B and contains.
The monomer composition which is the material for forming the (meth) acrylic polymer A and the monomer composition which is the material for forming the (meth) acrylic polymer B are alkyl (meth) acrylates having an alkyl group having 1 to 18 carbon atoms. The multilayer pressure-sensitive adhesive layer according to claim 1, which contains 50% by mass or more of. - 前記（メタ）アクリル系ポリマーＡの形成材料であるモノマー組成物と前記（メタ）アクリル系ポリマーＢの形成材料であるモノマー組成物は、同じアルキル（メタ）アクリレートを５０質量％以上含む、請求項２に記載の多層化粘着剤層。 The claim that the monomer composition which is a material for forming the (meth) acrylic polymer A and the monomer composition which is a material for forming the (meth) acrylic polymer B contain the same alkyl (meth) acrylate in an amount of 50% by mass or more. 2. The multi-layered pressure-sensitive adhesive layer according to 2.
- 有機ＥＬ表示装置用多層化粘着剤層である、請求項１～３のいずれかに記載の多層化粘着剤層。 The multi-layered pressure-sensitive adhesive layer according to any one of claims 1 to 3, which is a multi-layered pressure-sensitive adhesive layer for an organic EL display device.
- 請求項１～４のいずれかに記載の多層化粘着剤層の片面又は両面にセパレータを有するセパレータ付き多層化粘着剤層。 A multi-layered pressure-sensitive adhesive layer with a separator having separators on one side or both sides of the multi-layered pressure-sensitive adhesive layer according to any one of claims 1 to 4.
- 引張速度３００ｍｍ／分、剥離角度１８０度の条件で測定されるセパレータ剥離力が０．１５Ｎ／５０ｍｍ以下である、請求項５に記載のセパレータ付き多層化粘着剤層。 The multilayer adhesive layer with a separator according to claim 5, wherein the separator peeling force measured under the conditions of a tensile speed of 300 mm / min and a peeling angle of 180 degrees is 0.15 N / 50 mm or less.
- 請求項１～４のいずれかに記載の多層化粘着剤層と、光学フィルムとを有する粘着型光学フィルム。 An adhesive optical film having the multilayer adhesive layer according to any one of claims 1 to 4 and an optical film.
- フレキシブル画像表示装置用粘着型光学フィルムである、請求項７に記載の粘着型光学フィルム。 The adhesive optical film according to claim 7, which is an adhesive optical film for a flexible image display device.
- 請求項５又は６に記載のセパレータ付き多層化粘着剤層と、光学フィルムとを有するセパレータ付き粘着型光学フィルム。 An adhesive optical film with a separator having the multilayer adhesive layer with a separator according to claim 5 or 6 and an optical film.
- 請求項１～４のいずれかに記載の多層化粘着剤層、又は請求項７又は８に記載の粘着型光学フィルムを有する画像表示装置。 An image display device having the multilayer pressure-sensitive adhesive layer according to any one of claims 1 to 4 or the pressure-sensitive optical film according to claim 7 or 8.
- セパレータ上に粘着剤組成物を塗布する工程、及び温度３０～１０５℃、風速０．５～７ｍ／秒、及び乾燥時間５～３０秒間の条件で塗布した粘着剤組成物を乾燥する第１乾燥工程、前記第１乾燥工程後、温度３０～８５℃、風速０．５～７ｍ／秒、及び乾燥時間１０～１２０秒間の条件で塗布した粘着剤組成物を乾燥する第２乾燥工程、前記第２乾燥工程後、温度９０～１６０℃、風速０．１～２５ｍ／秒、及び乾燥時間１０～１８０秒間の条件で塗布した粘着剤組成物を乾燥する第３乾燥工程を含む乾燥工程により、セパレータ上に粘着剤層を形成する工程、
さらに、前記粘着剤層上に別の粘着剤組成物を塗布する工程、及び前記乾燥工程を繰り返し行うことにより、前記粘着剤層上に別の粘着剤層を順次積層する工程を含む、請求項５又は６に記載のセパレータ付き多層化粘着剤層の製造方法。 First drying to dry the pressure-sensitive adhesive composition applied on the separator, and under the conditions of a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 to 30 seconds. The second drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 85 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 10 to 120 seconds after the first drying step. 2 After the drying step, the separator is subjected to a drying step including a third drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds. The process of forming an adhesive layer on top,
Further, the claim includes a step of applying another pressure-sensitive adhesive composition on the pressure-sensitive adhesive layer and a step of sequentially laminating another pressure-sensitive adhesive layer on the pressure-sensitive adhesive layer by repeating the drying step. 5. The method for producing a multilayer pressure-sensitive adhesive layer with a separator according to 5 or 6. - 一方のセパレータ上に粘着剤組成物を塗布する工程、及び温度３０～１０５℃、風速０．５～７ｍ／秒、及び乾燥時間５～３０秒間の条件で塗布した粘着剤組成物を乾燥する第１乾燥工程、前記第１乾燥工程後、温度３０～８５℃、風速０．５～７ｍ／秒、及び乾燥時間１０～１２０秒間の条件で塗布した粘着剤組成物を乾燥する第２乾燥工程、前記第２乾燥工程後、温度９０～１６０℃、風速０．１～２５ｍ／秒、及び乾燥時間１０～１８０秒間の条件で塗布した粘着剤組成物を乾燥する第３乾燥工程を含む乾燥工程を少なくとも１回行うことにより、一方のセパレータ上に粘着剤層を１層以上形成する工程、
他方のセパレータ上に粘着剤組成物を塗布する工程、及び前記乾燥工程を少なくとも１回行うことにより、他方のセパレータ上に粘着剤層を１層以上形成する工程、
さらに、前記一方のセパレータ上の粘着剤層と前記他方のセパレータ上の粘着剤層とを積層する工程を含む、請求項５又は６に記載のセパレータ付き多層化粘着剤層の製造方法。 A step of applying the pressure-sensitive adhesive composition on one of the separators, and drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 to 30 seconds. 1 drying step, after the first drying step, a second drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 85 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 10 to 120 seconds. After the second drying step, a drying step including a third drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds is performed. A step of forming one or more pressure-sensitive adhesive layers on one separator by performing at least once.
A step of applying the pressure-sensitive adhesive composition on the other separator and a step of forming one or more pressure-sensitive adhesive layers on the other separator by performing the drying step at least once.
The method for producing a multilayer pressure-sensitive adhesive layer with a separator according to claim 5, further comprising a step of laminating the pressure-sensitive adhesive layer on the one separator and the pressure-sensitive adhesive layer on the other separator. - 一方のセパレータ上に粘着剤組成物を塗布する工程、及び温度３０～１０５℃、風速０．５～７ｍ／秒、及び乾燥時間５～３０秒間の条件で塗布した粘着剤組成物を乾燥する第１乾燥工程、前記第１乾燥工程後、温度３０～８５℃、風速０．５～７ｍ／秒、及び乾燥時間１０～１２０秒間の条件で塗布した粘着剤組成物を乾燥する第２乾燥工程、前記第２乾燥工程後、温度９０～１６０℃、風速０．１～２５ｍ／秒、及び乾燥時間１０～１８０秒間の条件で塗布した粘着剤組成物を乾燥する第３乾燥工程を含む乾燥工程を少なくとも１回行うことにより、一方のセパレータ上に粘着剤層を１層以上形成する工程、
前記粘着剤層の前記セパレータを有しない面に光学フィルムを積層し、前記セパレータを剥離する工程、
他方のセパレータ上に粘着剤組成物を塗布する工程、及び前記乾燥工程を少なくとも１回行うことにより、他方のセパレータ上に粘着剤層を１層以上形成する工程、
さらに、前記光学フィルム上の粘着剤層と前記他方のセパレータ上の粘着剤層とを積層する工程を含む、請求項９に記載のセパレータ付き粘着型光学フィルムの製造方法。 A step of applying the pressure-sensitive adhesive composition on one of the separators, and drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 105 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 5 to 30 seconds. 1 drying step, after the first drying step, a second drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 30 to 85 ° C., a wind speed of 0.5 to 7 m / sec, and a drying time of 10 to 120 seconds. After the second drying step, a drying step including a third drying step of drying the pressure-sensitive adhesive composition applied under the conditions of a temperature of 90 to 160 ° C., a wind speed of 0.1 to 25 m / sec, and a drying time of 10 to 180 seconds is performed. A step of forming one or more pressure-sensitive adhesive layers on one separator by performing at least once.
A step of laminating an optical film on a surface of the pressure-sensitive adhesive layer that does not have the separator and peeling the separator.
A step of applying the pressure-sensitive adhesive composition on the other separator and a step of forming one or more pressure-sensitive adhesive layers on the other separator by performing the drying step at least once.
The method for producing an adhesive optical film with a separator according to claim 9, further comprising a step of laminating the pressure-sensitive adhesive layer on the optical film and the pressure-sensitive adhesive layer on the other separator.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202180014294.1A CN115087716A (en) | 2020-03-11 | 2021-03-05 | Multilayered pressure-sensitive adhesive layer, multilayered pressure-sensitive adhesive layer with separator and method for producing same, pressure-sensitive adhesive optical film with separator and method for producing same, and image display device |
| KR1020227024084A KR20220148800A (en) | 2020-03-11 | 2021-03-05 | Multi-layered pressure-sensitive adhesive layer, multi-layered pressure-sensitive adhesive layer with separator and manufacturing method thereof, pressure-sensitive adhesive optical film, pressure-sensitive adhesive optical film with separator and method for manufacturing the same, and image display device |
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| JP2020042417A JP2021143271A (en) | 2020-03-11 | 2020-03-11 | Multilayered adhesive layer, multilayered adhesive layer having separator and manufacturing method thereof, adhesive-type optical film, adhesive-type optical film having separator and manufacturing method thereof, and picture display unit |
| JP2020-042417 | 2020-03-11 |
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| WO2021182340A1 true WO2021182340A1 (en) | 2021-09-16 |
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| JP (1) | JP2021143271A (en) |
| KR (1) | KR20220148800A (en) |
| CN (1) | CN115087716A (en) |
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| CN115087716A (en) | 2022-09-20 |
| JP2021143271A (en) | 2021-09-24 |
| TW202141089A (en) | 2021-11-01 |
| KR20220148800A (en) | 2022-11-07 |
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