WO2014156335A1 - Double-sided adhesive sheet - Google Patents
Double-sided adhesive sheet Download PDFInfo
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- WO2014156335A1 WO2014156335A1 PCT/JP2014/052965 JP2014052965W WO2014156335A1 WO 2014156335 A1 WO2014156335 A1 WO 2014156335A1 JP 2014052965 W JP2014052965 W JP 2014052965W WO 2014156335 A1 WO2014156335 A1 WO 2014156335A1
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- WIPO (PCT)
- Prior art keywords
- adhesive layer
- sensitive adhesive
- pressure
- release film
- meth
- Prior art date
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/06—Interconnection of layers permitting easy separation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09J7/10—Adhesives in the form of films or foils without carriers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/40—Properties of the layers or laminate having particular optical properties
- B32B2307/42—Polarizing, birefringent, filtering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/748—Releasability
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
- B32B2457/202—LCD, i.e. liquid crystal displays
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
Definitions
- the present invention relates to a double-sided pressure-sensitive adhesive sheet.
- An optical functional film such as a polarizing plate is fixed using a member such as a liquid crystal cell and a double-sided pressure-sensitive adhesive sheet composed of a pressure-sensitive adhesive.
- a double-sided adhesive sheet forms a coating film by apply
- an adhesive used for fixing an optical functional film such as a polarizing plate For example, an adhesive having a high elastic modulus (a storage elastic modulus at 23 ° C. of 0.3 MPa or more) using an ultraviolet curable resin is used (see, for example, Patent Document 1). This is due to the following reason. Since the manufactured optical functional film such as a polarizing plate easily contracts due to heat or the like, the optical functional film contracts due to thermal history. As a result, the pressure-sensitive adhesive layer on which the optical films are laminated cannot follow the shrinkage stress, and the layer is easily peeled off at the interface. However, the shrinkage can be suppressed by using a high modulus adhesive.
- the second release film is bonded to the second release film on the adhesive coating on the first release film.
- bubbles lamination
- active energy rays such as an ultraviolet-ray
- An object of the present invention is to provide a double-sided pressure-sensitive adhesive sheet that is excellent in durability and in which bubbles (lami bubbles) are prevented from being generated between the second release film and the pressure-sensitive adhesive layer.
- an adhesive layer comprising a first surface and a second surface; A first release film adhered to the first surface of the pressure-sensitive adhesive layer; A second release film adhered to the second surface of the pressure-sensitive adhesive layer,
- the storage elastic modulus of the pressure-sensitive adhesive layer at 23 ° C. is 0.3 MPa or more,
- the peeling force from the pressure-sensitive adhesive layer of the second release film is smaller than the peeling force from the pressure-sensitive adhesive layer of the first release film,
- the second release film is configured such that the arithmetic average roughness Ra 2 of the surface in contact with the pressure-sensitive adhesive layer is 30 nm or less and the maximum protrusion height Rp 2 is 250 nm or less.
- a featured double-sided pressure-sensitive adhesive sheet is configured such that the arithmetic average roughness Ra 2 of the surface in contact with the pressure-sensitive adhesive layer.
- the first release film is configured such that the arithmetic average roughness Ra 1 of the surface in contact with the pressure-sensitive adhesive layer is 40 nm or less and the maximum protrusion height Rp 1 is 700 nm or less.
- the peel force from the pressure-sensitive adhesive layer of the first release film is X [mN / 25 mm]
- the peel force from the pressure-sensitive adhesive layer of the second release film is Y [mN / 25 mm].
- the present invention for example, it is used for adhering an optical functional film such as a polarizing plate, and is excellent in durability, and bubbles (lami bubbles) are present between the second release film and the pressure-sensitive adhesive layer. It is possible to provide a double-sided PSA sheet that is prevented from being generated.
- FIG. 1 is a cross-sectional view of the double-sided pressure-sensitive adhesive sheet of the present invention.
- the double-sided pressure-sensitive adhesive sheet of the present invention is used, for example, for bonding an optical functional film such as a polarizing plate and a member such as a liquid crystal cell.
- FIG. 1 is a cross-sectional view of the double-sided pressure-sensitive adhesive sheet of the present invention.
- the double-sided pressure-sensitive adhesive sheet 1 includes a pressure-sensitive adhesive layer 10 having a first surface 101 and a second surface 102, and a first surface provided on the first surface 101 of the pressure-sensitive adhesive layer 10.
- the release film 11 and the second release film 12 provided on the second surface 102 of the pressure-sensitive adhesive layer 10 are included.
- the storage elastic modulus at 23 ° C. of the pressure-sensitive adhesive layer is 0.3 MPa or more
- the peeling force of the second release film from the pressure-sensitive adhesive layer is that of the first release film. It is comprised so that it may become smaller than the peeling force from the said adhesive layer.
- the second release film has an arithmetic average roughness Ra 2 of the surface in contact with the adhesive layer has a 30nm or less, and the maximum projection height Rp 2 in its plane, characterized in that at 250nm or less.
- the storage elastic modulus of the pressure-sensitive adhesive layer is set to 0.3 MPa or more, it is possible to more surely suppress the change in dimensional dimension of the optical functional film such as a polarizing plate over time.
- the peeling force from an adhesive layer means the peeling force measured as follows.
- the peel force was measured in accordance with JIS-Z0237.
- the double-sided pressure-sensitive adhesive sheet was cut into a width of 25 mm and a length of 200 mm, and the release film was 300 mm / min with the pressure-sensitive adhesive layer fixed using a tensile tester. This is done by pulling in the 180 ° direction at a speed.
- the storage elastic modulus of the pressure-sensitive adhesive layer means that a 30 ⁇ m-thick pressure-sensitive adhesive is laminated, a cylindrical test piece having a thickness of 8 mm ⁇ ⁇ 3 mm is prepared, and the torsional shear method is used under the following conditions. It refers to the measured storage modulus.
- Measuring device Dynamic viscoelasticity measuring device “DYNAMIC ANALYZER RDAII” manufactured by Rheometric, frequency: 1 Hz, temperature: 23 ° C., 80 ° C.
- DYNAMIC ANALYZER RDAII manufactured by Rheometric, frequency: 1 Hz, temperature: 23 ° C., 80 ° C.
- the pressure-sensitive adhesive layer 10 has a first surface 101 and a second surface 102.
- the storage elastic modulus at 23 ° C. of the pressure-sensitive adhesive layer 10 is 0.3 MPa or more. Thereby, the time-dependent change of the dimension of optical functional films, such as a polarizing plate, can be suppressed.
- the storage elastic modulus of the pressure-sensitive adhesive layer 10 at 23 ° C. is 0.3 MPa or more, and more preferably 0.35 to 12 MPa. Thereby, the temporal change of the dimension of the optical functional film such as a polarizing plate can be more reliably suppressed, and the adhesion durability can be increased.
- an adhesive which comprises the adhesive layer 10 Active energy rays are irradiated to the adhesive material containing (A) acrylic copolymer and (B) active energy ray hardening-type compound. It is preferable to use an adhesive. Thereby, the storage elastic modulus of the adhesive layer 10 can be made relatively high, and the durability (heat resistance, low temperature resistance, moisture resistance, etc.) of the adhesive layer 10 can be made higher.
- acrylic copolymer (A) examples include (meth) acrylic acid ester copolymers.
- (meth) acrylic acid ester means both acrylic acid ester and methacrylic acid ester. The same applies to other similar terms.
- the (meth) acrylic acid ester-based copolymer preferably has a crosslinking point that can be crosslinked by various crosslinking methods.
- the (meth) acrylic acid ester copolymer having such a crosslinking point is not particularly limited, and is a conventional (meth) acrylic acid ester copolymer commonly used as a resin component of an adhesive. Any copolymer can be appropriately selected and used.
- Examples of the (meth) acrylic acid ester copolymer having such a crosslinking point include (meth) acrylic acid alkyl ester having an alkyl group of 1 to 20 carbon atoms in the ester moiety, and a crosslinkable functional group in the molecule. It is preferable to use a copolymer of the monomer having and other monomers used as desired.
- examples of the alkyl (meth) acrylate alkyl ester having 1 to 20 carbon atoms in the alkyl group of the ester moiety include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, ( Butyl (meth) acrylate, pentyl (meth) acrylate, hexyl (meth) acrylate, cyclohexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, isooctyl (meth) acrylate, decyl (meth) acrylate, (Meth) acrylic acid dodecyl, (meth) acrylic acid myristyl, (meth) acrylic acid palmityl, (meth) acrylic acid stearyl, etc. may be used, and one or more of these may be used in combination.
- the monomer having a crosslinkable functional group in the molecule preferably contains at least one of a hydroxyl group, a carboxyl group, and an amino group as a functional group.
- this monomer include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, (Meth) acrylic acid hydroxyalkyl esters such as (meth) acrylic acid 3-hydroxybutyl and (meth) acrylic acid 4-hydroxybutyl; (meth) acrylic acid monomethylaminoethyl, (meth) acrylic acid monoethylaminoethyl, ( (Meth) acrylic acid monomethylaminopropyl, (meth) acrylic acid monoethylaminopropyl and other (meth) acrylic acid monoalkylaminoalkyl; acrylic acid, methacrylic acid, crotonic acid, maleic acid, ita
- the form of copolymerization of the (meth) acrylic acid ester copolymer (A) is not particularly limited, and any of random, block, and graft copolymers may be used.
- the (meth) acrylic acid ester copolymer (A) preferably has a mass average molecular weight of 500,000 or more, more preferably 600,000 to 2,000,000, and 700,000 to 1,800,000. More preferably. Thereby, the adhesiveness and adhesion durability with the adherend are sufficient, and the occurrence of the lifting or peeling of the pressure-sensitive adhesive layer 10 can be more effectively prevented.
- the mass average molecular weight is a standard polystyrene equivalent value obtained by measuring the (meth) acrylic acid ester copolymer (A) by a gel permeation chromatography (GPC) method.
- the content of monomer units having a crosslinkable functional group in the molecule is preferably in the range of 0.01 to 10% by mass.
- the content is 0.01% by mass or more, crosslinking is sufficient due to a reaction between a crosslinking agent and a crosslinkable functional group, which will be described later, and durability is improved.
- the content is 10% by mass or less, the degree of cross-linking becomes too high, and the suitability for bonding to a liquid crystal glass cell or a retardation plate is not deteriorated.
- a more preferable content of the monomer unit having a crosslinkable functional group is 0.05 to 7.0% by mass, A range of 0.2 to 6.0% by mass is preferable.
- the (meth) acrylic acid ester copolymer (A) one type may be used, or two or more types may be used in combination.
- a polyfunctional (meth) acrylate monomer having a molecular weight of less than 1000 can be used as the active energy ray-curable compound (B).
- Examples of the polyfunctional (meth) acrylate monomer having a molecular weight of less than 1000 include 1,4-butanediol di (meth) acrylate, 1,6-hexanediol di (meth) acrylate, neopentyl glycol di (meth) acrylate, Polyethylene glycol di (meth) acrylate, neopentyl glycol adipate di (meth) acrylate, hydroxypivalate neopentyl glycol di (meth) acrylate, dicyclopentanyl di (meth) acrylate, caprolactone modified dicyclopentenyl di (meth) acrylate , Bifunctional types such as ethylene oxide-modified phosphoric acid di (meth) acrylate, di (acryloxyethyl) isocyanurate, allylated cyclohexyl di (meth) acrylate; trimethylolpropane tri (Meth) acrylate, dipent
- the cyclic structure may be a carbocyclic structure or a heterocyclic structure, and may be a monocyclic structure or a polycyclic structure.
- polyfunctional (meth) acrylate monomers include those having an isocyanurate structure such as di (acryloxyethyl) isocyanurate, tris (acryloxyethyl) isocyanurate, dimethylol dicyclopentane diacrylate, Ethylene oxide-modified hexahydrophthalic acid diacrylate, tricyclodecane dimethanol acrylate, neopentyl glycol-modified trimethylolpropane diacrylate, adamantane diacrylate, and the like can be suitably used.
- isocyanurate structure such as di (acryloxyethyl) isocyanurate, tris (acryloxyethyl) isocyanurate, dimethylol dicyclopentane diacrylate, Ethylene oxide-modified hexahydrophthalic acid diacrylate, tricyclodecane dimethanol acrylate, neopentyl glycol-modified trimethylolpropane diacrylate,
- an active energy ray curable acrylate oligomer can be used as the active energy ray curable compound (B).
- the mass average molecular weight of the acrylate oligomer is preferably 50,000 or less.
- examples of such acrylate oligomers include polyester acrylate oligomers, epoxy acrylate oligomers, urethane acrylate oligomers, polyether acrylate oligomers, polybutadiene acrylate oligomers, silicone acrylate oligomers, and the like.
- the polyester acrylate oligomer is obtained by, for example, esterifying hydroxyl groups of a polyester oligomer having hydroxyl groups at both ends with (meth) acrylic acid, obtained by condensation of a polyvalent carboxylic acid and a polyhydric alcohol, or It can be obtained by esterifying the terminal hydroxyl group of an oligomer obtained by adding an alkylene oxide to a polyvalent carboxylic acid with (meth) acrylic acid.
- the epoxy acrylate oligomer can be obtained, for example, by reacting (meth) acrylic acid with an oxirane ring of a relatively low molecular weight bisphenol type epoxy resin or novolak type epoxy resin and esterifying it.
- a carboxyl-modified epoxy acrylate oligomer obtained by partially modifying this epoxy acrylate oligomer with a dibasic carboxylic acid anhydride can also be used.
- the urethane acrylate oligomer can be obtained, for example, by esterifying a polyurethane oligomer obtained by a reaction between a polyether polyol or a polyester polyol and a polyisocyanate with (meth) acrylic acid.
- the polyol acrylate oligomer can be obtained by esterifying the hydroxyl group of the polyether polyol with (meth) acrylic acid.
- the weight average molecular weight of the acrylate oligomer is preferably 50,000 or less, more preferably 500 to 50,000, and still more preferably 3,000 to 40,000 in terms of standard polymethyl methacrylate measured by GPC method. It is selected in the range.
- acrylate oligomers may be used alone or in combination of two or more.
- an adduct acrylate polymer in which a group having a (meth) acryloyl group is introduced into the side chain can also be used.
- Such an adduct acrylate polymer is a copolymer of the (meth) acrylic acid ester described in the (meth) acrylic acid ester copolymer (A) and a monomer having a crosslinkable functional group in the molecule.
- a compound having a (meth) acryloyl group and a group capable of reacting with the crosslinkable functional group is allowed to react with a part of the crosslinkable functional group of the copolymer.
- the mass average molecular weight of the adduct acrylate polymer is usually 500,000 to 2,000,000 in terms of standard polystyrene.
- active energy ray-curable compound (B) one type may be appropriately selected from the above-mentioned polyfunctional acrylate monomers, acrylate oligomers, and adduct acrylate polymers, and two or more types may be used in combination. May be.
- the content ratio of the (meth) acrylic ester copolymer (A) and the active energy ray-curable compound (B) is a mass ratio from the aspect of the performance of the obtained adhesive,
- the ratio is preferably 100: 1 to 100: 100, more preferably 100: 5 to 100: 50, and still more preferably 100: 10 to 100: 40.
- the adhesive material may contain a photopolymerization initiator as necessary.
- the photopolymerization initiator include benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin-n-butyl ether, benzoin isobutyl ether, acetophenone, dimethylaminoacetophenone, 2,2-dimethoxy-2-phenylacetophenone, 2,2-diethoxy-2-phenylacetophenone, 2-hydroxy-2-methyl-1-phenylpropan-1-one, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-1- [4- (methylthio) phenyl]- 2-morpholino-propan-1-one, 4- (2-hydroxyethoxy) phenyl-2- (hydroxy-2-propyl) ketone, benzophenone, p-phenylbenzophenone, 4,4'-diethylamino Benzophenone, dichlorobenzoph
- the blending amount of the photopolymerization initiator in the adhesive material is preferably 0.2 to 20 parts by mass with respect to 100 parts by mass of the active energy ray-curable compound (B).
- the adhesive material may contain a crosslinking agent as required.
- a crosslinking agent Arbitrary acrylic adhesives can be suitably selected and used from the acrylic adhesives conventionally used as a crosslinking agent in the conventional acrylic adhesive.
- crosslinking agents include polyisocyanate compounds, epoxy resins, melamine resins, urea resins, dialdehydes, methylol polymers, aziridine compounds, metal chelate compounds, metal alkoxides, metal salts, and the like. Of these, one or two or more can be used in combination. Among these, it is preferable to use a polyisocyanate compound as a crosslinking agent.
- polyisocyanate compound examples include aromatic polyisocyanates such as tolylene diisocyanate, diphenylmethane diisocyanate, and xylylene diisocyanate, aliphatic polyisocyanates such as hexamethylene diisocyanate, alicyclic polyisocyanates such as isophorone diisocyanate, hydrogenated diphenylmethane diisocyanate, and the like.
- aromatic polyisocyanates such as tolylene diisocyanate, diphenylmethane diisocyanate, and xylylene diisocyanate
- aliphatic polyisocyanates such as hexamethylene diisocyanate
- alicyclic polyisocyanates such as isophorone diisocyanate
- hydrogenated diphenylmethane diisocyanate and the like.
- the addition amount of the crosslinking agent is preferably 0.01 to 20 parts by mass, and preferably 0.1 to 10 parts by mass with respect to 100 parts by mass of the (meth) acrylic ester copolymer (A). More preferred.
- the adhesive material may contain a silane coupling agent as necessary.
- a silane coupling agent is an organosilicon compound having at least one alkoxysilyl group in the molecule, has good compatibility with the pressure-sensitive adhesive component, and has light transmittance, for example, is substantially transparent. Is preferred.
- the addition amount of the silane coupling agent is preferably 0.001 to 10 parts by mass, and more preferably 0.005 to 5 parts by mass with respect to 100 parts by mass of the solid content of the adhesive material.
- silane coupling agent examples include polymerizable unsaturated group-containing silicon compounds such as vinyltrimethoxysilane, vinyltriethoxysilane, and methacryloxypropyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, 2- ( 3,4-epoxycyclohexyl) ethyltrimethoxysilane and other silicon compounds having an epoxy structure, 3-aminopropyltrimethoxysilane, N- (2-aminoethyl) -3-aminopropyltrimethoxysilane, N- (2- And amino group-containing silicon compounds such as aminoethyl) -3-aminopropylmethyldimethoxysilane, and 3-chloropropyltrimethoxysilane. These may be used individually by 1 type and may be used in combination of 2 or more type.
- various additives usually used in acrylic adhesives as desired for example, tackifiers, antistatic agents, antioxidants, ultraviolet absorbers, as long as the object of the present invention is not impaired.
- tackifiers for example, tackifiers, antistatic agents, antioxidants, ultraviolet absorbers, as long as the object of the present invention is not impaired.
- Light stabilizers, softeners, fillers and the like can be added.
- the pressure-sensitive adhesive constituting the pressure-sensitive adhesive layer 10 is obtained by irradiating an adhesive material composed of the above-described components with active energy rays.
- Examples of active energy rays include ultraviolet rays and electron beams.
- the ultraviolet light can be obtained from a high-pressure mercury lamp, an electrodeless lamp, a xenon lamp, or the like.
- the electron beam can be obtained by an electron beam accelerator or the like.
- an adhesive can be formed, without adding a photoinitiator.
- the irradiation amount of the active energy ray for the adhesive material is appropriately selected so as to obtain the adhesive having the storage elastic modulus as described above.
- the illuminance is 50 to 1000 mW / cm 2 and the light amount is 50 to In the case of 1000 mJ / cm 2 and electron beam, the range of 10 to 1000 krad is preferable.
- the average thickness of the pressure-sensitive adhesive layer 10 is preferably 3 to 10 ⁇ m, and more preferably 4 to 8 ⁇ m. By setting the average thickness of the pressure-sensitive adhesive layer 10 in such a range, it is possible to obtain a thickness suitable for use in a thin display.
- the first release film 11 is attached to the first surface 101 of the pressure-sensitive adhesive layer 10.
- the first release film 11 has a function of protecting the pressure-sensitive adhesive layer 10.
- the first release film 11 is a laminate in which a first release agent layer 111 and a first base film 112 are sequentially laminated from the side in contact with the pressure-sensitive adhesive layer 10. It is configured.
- the first base film 112 has a function of imparting physical strength such as rigidity and flexibility to the first release film 11.
- the material constituting the first base film 112 examples include various synthetic resins.
- a polyester resin such as polybutylene terephthalate resin, polyethylene terephthalate resin, polyethylene naphthalate resin, and polyethylene terephthalate. It is more preferable to use a resin.
- the first base film 112 may be a single layer or a multilayer of two or more layers made of the same or different materials.
- the first base film 112 may contain a filler.
- the filler include silica, titanium oxide, calcium carbonate, kaolin, and aluminum oxide.
- the thickness of the first base film 112 is not particularly limited, but is preferably 10 to 300 ⁇ m, and more preferably 15 to 200 ⁇ m.
- the first release agent layer 111 has a function of imparting peelability to the first release film 11.
- the first release agent layer 111 is formed by applying a first release agent layer-forming composition containing the first release agent to the surface of the first base film 112 and drying it.
- the first release agent is not particularly limited, and examples thereof include alkyd compounds, acrylic compounds, silicone compounds, long-chain alkyl group-containing compounds, and fluorine compounds. Among these, as the first release agent, it is preferable to use an alkyd compound, an acrylic compound, a silicone compound, or a long-chain alkyl group-containing compound.
- an alkyd compound having a crosslinked structure is generally used. Formation of the alkyd compound layer having a crosslinked structure can be performed, for example, by a method in which a layer made of a thermosetting composition containing an alkyd compound, a crosslinking agent, and optionally a curing catalyst is heated and cured.
- the alkyd compound may be a modified product such as a long-chain alkyl-modified alkyd compound or a silicone-modified alkyd compound.
- the acrylic compound an acrylic compound having a crosslinked structure is generally used.
- the acrylic compound may be a modified product such as a long-chain alkyl-modified acrylic compound or a silicone-modified acrylic compound.
- silicone compounds include silicone compounds having dimethylpolysiloxane as a basic skeleton.
- the silicone compound includes an addition reaction type silicone compound, a condensation reaction type silicone compound, an ultraviolet curable silicone compound, an electron beam curable silicone compound, and the like.
- the addition reaction type silicone compound has high reactivity and excellent productivity, and has advantages such as little change in peel strength after production and no curing shrinkage compared to the condensation reaction type silicone compound.
- addition reaction type silicone compound examples include two or more alkenyl groups having 2 to 10 carbon atoms such as a vinyl group, an allyl group, a propenyl group, and a hexenyl group at the terminal and / or side chain of the molecule.
- Organopolysiloxane is mentioned.
- crosslinking agent and a catalyst it is preferable to use a crosslinking agent and a catalyst in combination.
- crosslinking agent examples include, for example, organopolysiloxane having hydrogen atoms bonded to at least two silicon atoms in one molecule, specifically, a dimethylhydrogensiloxy group end-capped dimethylsiloxane-methylhydrogensiloxane copolymer. And trimethylsiloxy group end-capped dimethylsiloxane-methylhydrogensiloxane copolymer, trimethylsiloxy group end-capped methylhydrogenpolysiloxane, poly (hydrogensilsesquioxane), and the like.
- the catalyst fine platinum, fine platinum adsorbed on a carbon powder carrier, chloroplatinic acid, alcohol-modified chloroplatinic acid, olefin complexes of chloroplatinic acid, white metal compounds such as palladium and rhodium Etc.
- Examples of the long-chain alkyl group-containing compound include a polyvinyl carbamate obtained by reacting a polyvinyl alcohol polymer with a long-chain alkyl isocyanate having 8 to 30 carbon atoms, or a long-chain alkyl group having 8 to 30 carbon atoms with polyethyleneimine. An alkylurea derivative obtained by reacting isocyanate is used.
- Fluorine compounds include fluorine silicone compounds and fluorine boron compounds.
- An additive may be appropriately added to the first release agent composition.
- the additive include a catalyst, a dye, and a dispersant.
- the material of the first release agent layer forming composition described above so that the release force of the first release film 11 is greater than the release force of the second release film 12. is appropriately selected.
- the first release agent composition may appropriately contain a dispersion medium or a solvent in order to bring the viscosity at the time of application to an appropriate range.
- Preferred examples of the dispersion medium or solvent include aromatic hydrocarbons such as toluene, fatty acid esters such as ethyl acetate, ketones such as methyl ethyl ketone, and organic solvents such as aliphatic hydrocarbons such as hexane and heptane.
- aromatic hydrocarbons such as toluene
- fatty acid esters such as ethyl acetate
- ketones such as methyl ethyl ketone
- organic solvents such as aliphatic hydrocarbons such as hexane and heptane.
- the content of the first release agent in the first release agent composition is not particularly limited, but is preferably 0.3 to 10% by mass.
- gravure coating method for example, gravure coating method, bar coating method, spray coating method, spin coating method, air knife coating method, roll coating method, blade coating method, gate roll coating method, die coating method, etc.
- a gravure coating method and a bar coating method are preferable, and a bar coating method is particularly preferable.
- the drying temperature is not particularly limited, but is preferably 100 to 150 ° C., and the drying time is preferably 10 seconds to 1 minute.
- the thickness of the first release agent layer is preferably from 0.01 to 5 ⁇ m, particularly preferably from 0.03 to 3 ⁇ m.
- the arithmetic average roughness Ra 1 of the surface of the first release film 11 in contact with the pressure-sensitive adhesive layer 10 is preferably 40 nm or less, and the maximum protrusion height Rp 1 is preferably 700 nm or less.
- the adhesiveness (adhesiveness) of the 1st surface 101 of the adhesive layer 10 and adherends, such as a liquid crystal cell can be made higher.
- durability of optical products such as liquid crystal panels finally obtained can be further increased.
- corrugation of the 1st surface 101 of the adhesive layer 10 can be prevented.
- the second release film 12 is attached to the second surface 102 of the pressure-sensitive adhesive layer 10.
- the second release film 12 has a function of protecting the pressure-sensitive adhesive layer 10.
- the arithmetic average roughness Ra 2 of the surface in contact with the pressure-sensitive adhesive layer 10 of the second release film 12 is 30 nm or less, and the maximum protrusion height Rp 2 is 250 nm or less.
- the second release film 12 is a laminate in which a second release agent layer 121 and a second base film 122 are sequentially laminated from the side in contact with the pressure-sensitive adhesive layer 10. It is configured.
- the same material as the first base film 112 described in the section of the first release film 11 described above can be used.
- the second release agent layer 121 is formed by applying a second release agent layer-forming composition containing the second release agent to the surface of the second base film 122 and drying it.
- the same material as the first release agent described in the section of the first release film described above can be used.
- the material of the second release agent layer forming composition described above so that the release force of the second release film 12 is smaller than the release force of the first release film 11. is appropriately selected.
- the second release agent layer 121 may be a single layer or a plurality of layers of two or more layers, but one layer is preferable for simplifying the operation.
- the thickness of the second release agent layer 121 is preferably 0.01 to 5 ⁇ m, and more preferably 0.03 to 3 ⁇ m.
- Example 1 Preparation of double-sided PSA sheet (Example 1) 1. Preparation of the first release film After drying the first release agent layer-forming composition A having the following composition on one surface of a polyethylene terephthalate (PET) film (thickness 38 ⁇ m) as the first substrate film The film was coated with a bar coater so that the thickness of the film became 0.1 ⁇ m, and dried at 120 ° C. for 1 minute to provide a first release agent layer. This produced the 1st peeling film.
- Table 1 shows the arithmetic average roughness Ra 1 and the maximum protrusion height Rp 1 of the surface of the first release agent layer of the obtained first release film.
- first release agent layer-forming composition A A silicone resin solution containing organopolysiloxane having a vinyl group and an organopolysiloxane having a hydrosilyl group (trade name “BY24-561” manufactured by Toray Dow Corning Co., Ltd.), 30 parts by mass in terms of solid content, vinyl MQ resin (trade name “SD7292”, manufactured by Toray Dow Corning Co., Ltd.) equipped with a base is diluted and mixed in a toluene solvent so that the solid content concentration is 1.0% by mass in a toluene solvent. did. To this solution was added 2 parts by mass of a platinum-based catalyst (trade name “SRX-212” manufactured by Toray Dow Corning) to prepare a first release agent layer forming composition A.
- SRX-212 platinum-based catalyst manufactured by Toray Dow Corning
- a second release agent layer-forming composition B having the following composition is dried on one surface of a polyethylene terephthalate (PET) film (thickness 38 ⁇ m) as a second substrate film.
- PET polyethylene terephthalate
- a second coater was applied by a bar coater so that the subsequent thickness was 0.1 ⁇ m and dried at 120 ° C. for 1 minute. This produced the 2nd peeling film.
- Table 1 shows the arithmetic average roughness Ra 2 and the maximum protrusion height Rp 2 of the surface of the second release agent layer of the obtained second release film.
- Second release agent layer-forming composition B 100 parts by mass of a silicone resin (manufactured by Shin-Etsu Chemical Co., Ltd .: trade name “KS847H”) and 1 part by mass of a curing agent (manufactured by Shin-Etsu Chemical Co., Ltd .: trade name “CAT-PL50T”) are diluted with toluene to obtain a solid content concentration. 1% by mass of a second release agent layer-forming composition B was prepared.
- a part of the obtained solution was subjected to GPC measurement, and production of a polymer (A) having a mass average molecular weight of 1.6 million was confirmed.
- 100 parts by mass (solid content) of the above polymer (A) 20 parts by mass of tris (acryloxyethyl) isocyanurate (trade name “Aronix M-315”, molecular weight: 423, manufactured by Toagosei Co., Ltd.), photopolymerization initiator (Ciba Specialty Chemicals, trade name “Irgacure 500”) 2.0 parts by mass, polyisocyanate-based crosslinking agent (manufactured by Nippon Polyurethanes, trade name “Coronate L”, 4 parts by mass, and silane coupling agent (Shin-Etsu) 0.1 parts by mass of “KBM-403” manufactured by Kagaku Kogyo Co., Ltd. was added and mixed to obtain a mixed solution, and toluene was further added as a solvent to the
- UV ultraviolet light
- UV irradiation conditions ⁇ Uses an electrodeless lamp H bulb manufactured by Fusion. ⁇ Illuminance 600 mW / cm 2 , light quantity 150 mJ / cm 2 “UVPF-36” manufactured by Eye Graphics Co., Ltd. was used as the UV illuminance / light meter.
- Example 2 A double-sided PSA sheet was prepared in the same manner as in Example 1 except that the average thickness of the PSA layer was 3 ⁇ m.
- Example 3 A double-sided PSA sheet was prepared in the same manner as in Example 1 except that the average thickness of the PSA layer was 10 ⁇ m.
- Example 4 Adhesive as in Example 1 except that 20 parts by mass of tris (acryloxyethyl) isocyanurate (trade name “Aronix M-315”, manufactured by Toagosei Co., Ltd.) of the adhesive composition A was changed to 10 parts by mass.
- Composition B was prepared to produce a double-sided PSA sheet.
- Example 5 Adhesive as in Example 1 except that 20 parts by mass of tris (acryloxyethyl) isocyanurate (trade name “Aronix M-315” manufactured by Toagosei Co., Ltd.) of the adhesive composition A was changed to 40 parts by mass. Composition C was prepared to produce a double-sided PSA sheet.
- Example 6 The second release film was changed so that the arithmetic average roughness Ra 2 and the maximum protrusion height Rp 2 of the surface of the release agent layer of the second release film were changed to the values shown in Table 1.
- a double-sided PSA sheet was prepared in the same manner as in Example 1 except that was prepared.
- Example 8 Except that 20 parts by mass of Tris (acryloxyethyl) isocyanurate (trade name “Aronix M-315”, manufactured by Toagosei Co., Ltd.) of the adhesive composition A was 7.5 parts by mass, the same as in Example 1 above.
- a pressure-sensitive adhesive composition D was prepared to prepare a double-sided pressure-sensitive adhesive sheet.
- Example 9 A double-sided PSA sheet was prepared in the same manner as in Example 1 except that the average thickness of the PSA layer was 2 ⁇ m.
- Example 10 The first release film was changed so that the arithmetic average roughness Ra 1 and the maximum protrusion height Rp 1 of the surface of the release agent layer of the first release film were changed to the values shown in Table 1.
- a double-sided PSA sheet was prepared in the same manner as in Example 1 except that was prepared.
- Example 3 Adhesive as in Example 1 except that 20 parts by mass of tris (acryloxyethyl) isocyanurate (trade name “Aronix M-315” manufactured by Toagosei Co., Ltd.) of the adhesive composition A was changed to 5 parts by mass.
- Composition E was prepared to produce a double-sided PSA sheet.
- Rp 2 was measured in accordance with JIS B 0601-1994 using a surface roughness measuring instrument SV3000S4 (stylus type) manufactured by Mitutoyo Corporation.
- the storage elastic modulus at 23 ° C. of the pressure-sensitive adhesive layer used in the double-sided pressure-sensitive adhesive sheet of each example and comparative example is a viscoelasticity measuring device (trade name “DYNAMIC ANALAYZER” manufactured by REOMETRIC) according to JIS K 7244. Was measured by the torsional shear method under the following conditions.
- the peel force of the first release film and the second release film on the adhesive layer was measured using a tensile tester according to JIS-Z0237. It was done. The measurement was performed by pulling the first release film or the second release film in a 180 ° direction at a speed of 300 mm / min in a state where the double-sided PSA sheet was cut to a width of 25 mm and a length of 200 mm and the PSA layer was fixed. It has been executed.
- Lami bubbles were not generated. ⁇ : Lami bubbles were less than 10. ⁇ : There were 10 or more lami bubbles.
- the pressure-sensitive adhesive layer was exposed by peeling off the first release film from the double-sided PSA sheet of each Example and each Comparative Example. Next, the exposed pressure-sensitive adhesive layer was bonded to a polarizing plate in which a polarizing film composed of a polarizing film with a discotic liquid crystal layer and a viewing angle widening film were integrated. The obtained polarizing plate with the pressure-sensitive adhesive layer was cut into a size of 233 mm ⁇ 309 mm using a cutting device (Super cutter manufactured by Hadano Seisakusho, PN1-600). Subsequently, the 2nd peeling film was peeled off and the adhesive layer was exposed.
- a cutting device Super cutter manufactured by Hadano Seisakusho, PN1-600
- the exposed adhesive layer was affixed to non-alkali glass (Corning, Eagle XG) to obtain a sample. Then, the sample was pressurized at 0.5 MPa and 50 ° C. for 20 minutes in an autoclave manufactured by Kurihara Seisakusho. Then, the sample was left still in the environment of the following durability conditions. After 500 hours, the sample was observed using a 10-fold magnifier. Appearance change was based on the following.
- ⁇ There were no defects on the four sides of the sample. ⁇ : On the four sides of the sample, there was no defect at a portion of 0.6 mm or more from the outer peripheral edge. ⁇ : At least one of the four sides of the sample has a pressure-sensitive adhesive float, pressure-sensitive adhesive peeling, pressure-sensitive adhesive foaming, pressure-sensitive adhesive streaks, etc. There was an abnormal appearance defect of the adhesive.
- the double-sided pressure-sensitive adhesive sheet of the present invention prevented the generation of lami bubbles. Moreover, the double-sided adhesive sheet of this invention was excellent in the peelability of each peeling film. Moreover, the double-sided pressure-sensitive adhesive sheet of the present invention was excellent in durability. On the other hand, satisfactory results were not obtained in the comparative example.
- the double-sided pressure-sensitive adhesive sheet of the present invention comprises a pressure-sensitive adhesive layer comprising a first surface and a second surface, a first release film adhered to the first surface of the pressure-sensitive adhesive layer, and the pressure-sensitive adhesive. And a second release film attached to the second surface of the layer.
- the storage elastic modulus of the pressure-sensitive adhesive layer at 23 ° C. is 0.3 MPa or more.
- the peeling force from the pressure-sensitive adhesive layer of the second release film is smaller than the peeling force from the pressure-sensitive adhesive layer of the first release film.
- the second release film is configured such that the arithmetic average roughness Ra 2 of the surface in contact with the pressure-sensitive adhesive layer is 30 nm or less, and the maximum protrusion height Rp 2 is 250 nm or less.
- Such a double-sided PSA sheet is excellent in durability and prevents bubbles (lami bubbles) from being generated between the second release film and the PSA layer. Therefore, the present invention has industrial applicability.
Abstract
Description
(1) 第1の面と第2の面とを備える粘着剤層と、
前記粘着剤層の前記第1の面に貼着された第1の剥離フィルムと、
前記粘着剤層の前記第2の面に貼着された第2の剥離フィルムと、を有し、
23℃における前記粘着剤層の貯蔵弾性率が、0.3MPa以上であり、
前記第2の剥離フィルムの前記粘着剤層からの剥離力は、前記第1の剥離フィルムの前記粘着剤層からの剥離力よりも小さく、
前記第2の剥離フィルムは、前記粘着剤層と接する面の算術平均粗さRa2が30nm以下であり、かつ、その最大突起高さRp2が250nm以下であるように構成されていることを特徴とする両面粘着シート。 Such an object is achieved by the present inventions (1) to (4) below.
(1) an adhesive layer comprising a first surface and a second surface;
A first release film adhered to the first surface of the pressure-sensitive adhesive layer;
A second release film adhered to the second surface of the pressure-sensitive adhesive layer,
The storage elastic modulus of the pressure-sensitive adhesive layer at 23 ° C. is 0.3 MPa or more,
The peeling force from the pressure-sensitive adhesive layer of the second release film is smaller than the peeling force from the pressure-sensitive adhesive layer of the first release film,
The second release film is configured such that the arithmetic average roughness Ra 2 of the surface in contact with the pressure-sensitive adhesive layer is 30 nm or less and the maximum protrusion height Rp 2 is 250 nm or less. A featured double-sided pressure-sensitive adhesive sheet.
《両面粘着シート》
本発明の両面粘着シートは、例えば、偏光板等の光学機能性フィルムと液晶セル等の部材とを貼合するのに用いられるものである。 Hereinafter, the present invention will be described in detail based on preferred embodiments.
《Double-sided adhesive sheet》
The double-sided pressure-sensitive adhesive sheet of the present invention is used, for example, for bonding an optical functional film such as a polarizing plate and a member such as a liquid crystal cell.
図1に示すように、両面粘着シート1は、第1の面101と第2の面102とを有する粘着剤層10と、粘着剤層10の第1の面101上に設けられた第1の剥離フィルム11と、粘着剤層10の第2の面102上に設けられた第2の剥離フィルム12とを有している。 FIG. 1 is a cross-sectional view of the double-sided pressure-sensitive adhesive sheet of the present invention.
As shown in FIG. 1, the double-sided pressure-sensitive adhesive sheet 1 includes a pressure-sensitive
以下、本実施形態に係る両面粘着シート1を構成する各層について詳細に説明する。 Measuring device: Dynamic viscoelasticity measuring device “DYNAMIC ANALYZER RDAII” manufactured by Rheometric, frequency: 1 Hz, temperature: 23 ° C., 80 ° C.
Hereinafter, each layer which comprises the double-sided adhesive sheet 1 which concerns on this embodiment is demonstrated in detail.
粘着剤層10は、第1の面101と第2の面102とを有する。 <
The pressure-sensitive
光重合開始剤としては、例えば、ベンソイン、ベンゾインメチルエーテル、ベンゾインエチルエーテル、ベンゾインイソプロピルエーテル、ベンゾイン-n-ブチルエーテル、ベンゾインイソブチルエーテル、アセトフェノン、ジメチルアミノアセトフェノン、2,2-ジメトキシ-2-フェニルアセトフェノン、2,2-ジエトキシ-2-フェニルアセトフェノン、2-ヒドロキシ-2-メチル-1-フェニルプロパン-1-オン、1-ヒドロキシシクロヘキシルフェニルケトン、2-メチル-1-[4-(メチルチオ)フェニル]-2-モルフォリノ-プロパン-1-オン、4-(2-ヒドロキシエトキシ)フェニル-2-(ヒドロキシ-2-プロピル)ケトン、ベンゾフェノン、p-フェニルベンゾフェノン、4,4’-ジエチルアミノベンゾフェノン、ジクロロベンゾフェノン、2-メチルアントラキノン、2-エチルアントラキノン、2-ターシャリ-ブチルアントラキノン、2-アミノアントラキノン、2-メチルチオキサントン、2-エチルチオキサントン、2-クロロチオキサントン、2,4-ジメチルチオキサントン、2,4-ジエチルチオキサントン、ベンジルジメチルケタール、アセトフェノンジメチルケタール、p-ジメチルアミノ安息香酸エステル、オリゴ[2-ヒドロキシ-2-メチル-1[4-(1-メチルビニル)フェニル]プロパノン]、2,4,6-トリメチルベンゾイル-ジフェニル-フォスフィンオキサイド等が挙げられ、これらのうち、1種または2種以上を組み合わせて用いてもよい。 The adhesive material may contain a photopolymerization initiator as necessary.
Examples of the photopolymerization initiator include benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin-n-butyl ether, benzoin isobutyl ether, acetophenone, dimethylaminoacetophenone, 2,2-dimethoxy-2-phenylacetophenone, 2,2-diethoxy-2-phenylacetophenone, 2-hydroxy-2-methyl-1-phenylpropan-1-one, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-1- [4- (methylthio) phenyl]- 2-morpholino-propan-1-one, 4- (2-hydroxyethoxy) phenyl-2- (hydroxy-2-propyl) ketone, benzophenone, p-phenylbenzophenone, 4,4'-diethylamino Benzophenone, dichlorobenzophenone, 2-methylanthraquinone, 2-ethylanthraquinone, 2-tert-butylanthraquinone, 2-aminoanthraquinone, 2-methylthioxanthone, 2-ethylthioxanthone, 2-chlorothioxanthone, 2,4-dimethylthioxanthone, 2 , 4-diethylthioxanthone, benzyldimethyl ketal, acetophenone dimethyl ketal, p-dimethylaminobenzoate, oligo [2-hydroxy-2-methyl-1 [4- (1-methylvinyl) phenyl] propanone], 2,4 , 6-trimethylbenzoyl-diphenyl-phosphine oxide and the like, and among these, one kind or a combination of two or more kinds may be used.
架橋剤としては、特に制限はなく、従来のアクリル系粘着剤において、架橋剤として慣用されているアクリル系粘着剤の中から、任意のアクリル系粘着剤を適宜選択して用いることができる。このような架橋剤としては、例えば、ポリイソシアネート化合物、エポキシ樹脂、メラミン樹脂、尿素樹脂、ジアルデヒド類、メチロールポリマー、アジリジン系化合物、金属キレート化合物、金属アルコキシド、金属塩などが挙げられ、これらのうち、1種または2種以上を組み合わせて用いることができる。これらの中でも、架橋剤として、ポリイソシアネート化合物を用いるのが好ましい。 Moreover, the adhesive material may contain a crosslinking agent as required.
There is no restriction | limiting in particular as a crosslinking agent, Arbitrary acrylic adhesives can be suitably selected and used from the acrylic adhesives conventionally used as a crosslinking agent in the conventional acrylic adhesive. Examples of such crosslinking agents include polyisocyanate compounds, epoxy resins, melamine resins, urea resins, dialdehydes, methylol polymers, aziridine compounds, metal chelate compounds, metal alkoxides, metal salts, and the like. Of these, one or two or more can be used in combination. Among these, it is preferable to use a polyisocyanate compound as a crosslinking agent.
第1の剥離フィルム11は、粘着剤層10の第1の面101に貼着されている。
当該第1の剥離フィルム11は、粘着剤層10を保護する機能を有している。 [First release film]
The
The
第2の剥離フィルム12は、粘着剤層10の第2の面102に貼着されている。
当該第2の剥離フィルム12は、粘着剤層10を保護する機能を有している。 [Second release film]
The second release film 12 is attached to the
The second release film 12 has a function of protecting the pressure-
[1]両面粘着シートの作製
(実施例1)
1.第1の剥離フィルムの作製
第1の基材フィルムとしてのポリエチレンテレフタレート(PET)フィルム(厚さ38μm)の一方の面に、下記組成の第1の剥離剤層形成用組成物Aを、乾燥後の厚みが0.1μmとなるようにバーコーターにて塗布し、120℃で1分間乾燥して第1の剥離剤層を設けた。これにより第1の剥離フィルムを作製した。得られた第1の剥離フィルムの第1の剥離剤層の表面の算術平均粗さRa1および最大突起高さRp1を表1に記載した。 Next, specific examples of the release film of the present invention will be described.
[1] Preparation of double-sided PSA sheet (Example 1)
1. Preparation of the first release film After drying the first release agent layer-forming composition A having the following composition on one surface of a polyethylene terephthalate (PET) film (thickness 38 μm) as the first substrate film The film was coated with a bar coater so that the thickness of the film became 0.1 μm, and dried at 120 ° C. for 1 minute to provide a first release agent layer. This produced the 1st peeling film. Table 1 shows the arithmetic average roughness Ra 1 and the maximum protrusion height Rp 1 of the surface of the first release agent layer of the obtained first release film.
ビニル基を備えたオルガノポリシロキサンおよびヒドロシリル基を備えたオルガノポリシロキサンを含有するシリコーン樹脂溶液(東レ・ダウコーニング社製、商品名「BY24-561」)を固形分換算で30質量部と、ビニル基を備えたMQレジン(東レ・ダウコーニング社製、商品名「SD7292」)を固形分換算で15質量部とを、トルエン溶媒に、固形分濃度が1.0質量%となるように希釈混合した。この溶液に白金系触媒(東レ・ダウコーニング社製、商品名「SRX-212」)を2質量部添加し、第1の剥離剤層形成用組成物Aを調製した。 (Preparation of first release agent layer-forming composition A)
A silicone resin solution containing organopolysiloxane having a vinyl group and an organopolysiloxane having a hydrosilyl group (trade name “BY24-561” manufactured by Toray Dow Corning Co., Ltd.), 30 parts by mass in terms of solid content, vinyl MQ resin (trade name “SD7292”, manufactured by Toray Dow Corning Co., Ltd.) equipped with a base is diluted and mixed in a toluene solvent so that the solid content concentration is 1.0% by mass in a toluene solvent. did. To this solution was added 2 parts by mass of a platinum-based catalyst (trade name “SRX-212” manufactured by Toray Dow Corning) to prepare a first release agent layer forming composition A.
第2の基材フィルムとしてのポリエチレンテレフタレート(PET)フィルム(厚さ38μm)の1方の面に、下記組成の第2の剥離剤層形成用組成物Bを、乾燥後の厚みが0.1μmとなるようにバーコーターにて塗布し、120℃で1分間乾燥して第2の剥離剤層を設けた。これにより第2の剥離フィルムを作製した。得られた第2の剥離フィルムの第2の剥離剤層の表面の算術平均粗さRa2および最大突起高さRp2を表1に記載した。 2. Production of Second Release Film A second release agent layer-forming composition B having the following composition is dried on one surface of a polyethylene terephthalate (PET) film (thickness 38 μm) as a second substrate film. A second coater was applied by a bar coater so that the subsequent thickness was 0.1 μm and dried at 120 ° C. for 1 minute. This produced the 2nd peeling film. Table 1 shows the arithmetic average roughness Ra 2 and the maximum protrusion height Rp 2 of the surface of the second release agent layer of the obtained second release film.
シリコーン樹脂100質量部(信越化学工業社製:商品名「KS847H」)と、硬化剤1質量部(信越化学工業社製:商品名「CAT-PL50T」)とをトルエンで希釈し、固形分濃度1質量%の第2の剥離剤層形成用組成物Bを調製した。 (Preparation of second release agent layer-forming composition B)
100 parts by mass of a silicone resin (manufactured by Shin-Etsu Chemical Co., Ltd .: trade name “KS847H”) and 1 part by mass of a curing agent (manufactured by Shin-Etsu Chemical Co., Ltd .: trade name “CAT-PL50T”) are diluted with toluene to obtain a solid content concentration. 1% by mass of a second release agent layer-forming composition B was prepared.
攪拌機、温度計、還流冷却器、滴下装置および窒素導入管を備えた反応容器に、アクリル酸n-ブチル95.0質量部、アクリル酸2-ヒドロキシエチル5.0質量部、酢酸エチル200質量部、および、2,2’-アゾビスイソブチロニトリル0.08質量部を仕込み、反応液を得た。次に、上記反応容器内の空気を窒素ガスで置換した。この窒素雰囲気下中、反応液を攪拌しながら、反応溶液を60℃に昇温し、16時間反応させた後、反応液を室温まで冷却した。ここで、得られた溶液の一部をGPC測定し、質量平均分子量160万の重合体(A)の生成を確認した。上記重合体(A)100質量部(固形分)に、トリス(アクリロキシエチル)イソシアヌレート(東亜合成社製、商品名「アロニックスM-315」、分子量:423)20質量部、光重合開始剤(チバ・スペシャルティ・ケミカルズ社製、商品名「イルガキュア500」)2.0質量部、ポリイソシアネート系架橋剤(日本ポリウレタン社製、商品名「コロネートL」4質量部、およびシランカップリング剤(信越化学工業社製「KBM-403」)0.1質量部を添加し、混合して混合液を得た。この混合液に、さらに溶剤としてトルエンを加えて固形分を15質量%に調整し、粘着剤組成物Aを調製した。 3. Preparation of pressure-sensitive adhesive composition In a reaction vessel equipped with a stirrer, a thermometer, a reflux condenser, a dropping device and a nitrogen introduction tube, 95.0 parts by mass of n-butyl acrylate and 5.0 parts by mass of 2-hydroxyethyl acrylate 200 parts by mass of ethyl acetate and 0.08 part by mass of 2,2′-azobisisobutyronitrile were charged to obtain a reaction solution. Next, the air in the reaction vessel was replaced with nitrogen gas. In this nitrogen atmosphere, stirring the reaction solution, the reaction solution was heated to 60 ° C. and reacted for 16 hours, and then the reaction solution was cooled to room temperature. Here, a part of the obtained solution was subjected to GPC measurement, and production of a polymer (A) having a mass average molecular weight of 1.6 million was confirmed. 100 parts by mass (solid content) of the above polymer (A), 20 parts by mass of tris (acryloxyethyl) isocyanurate (trade name “Aronix M-315”, molecular weight: 423, manufactured by Toagosei Co., Ltd.), photopolymerization initiator (Ciba Specialty Chemicals, trade name “Irgacure 500”) 2.0 parts by mass, polyisocyanate-based crosslinking agent (manufactured by Nippon Polyurethanes, trade name “Coronate L”, 4 parts by mass, and silane coupling agent (Shin-Etsu) 0.1 parts by mass of “KBM-403” manufactured by Kagaku Kogyo Co., Ltd. was added and mixed to obtain a mixed solution, and toluene was further added as a solvent to the mixed solution to adjust the solid content to 15% by mass. An adhesive composition A was prepared.
第1の剥離フィルムの剥離剤層上に、粘着剤組成物Aを乾燥後に5μmとなるように、塗布し、90℃で1分間、乾燥させて粘着剤層を形成した。次いで、形成した粘着剤層上に、第2の剥離フィルムの剥離剤層が当該粘着剤層に接するように、第2の剥離フィルムを貼合して、積層体を得た。貼合は、ラミネート圧力を0.5MPaに調整したシリコーンゴムロール(ゴム硬度:80)と金属ロールとの間に積層体を挟み込み、常温条件下、速度50m/minで実行された。次いで、第1の剥離フィルムの下から紫外線(UV)を下記の条件で照射し、両面粘着シートを作製した。その後、温度23℃、相対湿度50%の条件で10日間養生した。 4). Preparation of double-sided pressure-sensitive adhesive sheet The pressure-sensitive adhesive composition A was applied onto the release agent layer of the first release film so as to be 5 μm after drying, and dried at 90 ° C. for 1 minute to form a pressure-sensitive adhesive layer. Subsequently, the 2nd peeling film was bonded on the formed adhesive layer so that the peeling agent layer of a 2nd peeling film might contact the said adhesive layer, and the laminated body was obtained. The lamination was carried out at a speed of 50 m / min under normal temperature conditions by sandwiching the laminate between a silicone rubber roll (rubber hardness: 80) whose laminating pressure was adjusted to 0.5 MPa and a metal roll. Next, ultraviolet light (UV) was irradiated from under the first release film under the following conditions to produce a double-sided PSA sheet. Then, it was cured for 10 days under the conditions of a temperature of 23 ° C. and a relative humidity of 50%.
・フュージョン社製無電極ランプ H バルブ使用。
・照度600mW/cm2、光量150mJ/cm2
UV照度・光量計は、アイグラフィックス社製「UVPF-36」を使用した。 <UV irradiation conditions>
・ Uses an electrodeless lamp H bulb manufactured by Fusion.
・ Illuminance 600 mW / cm 2 , light quantity 150 mJ / cm 2
“UVPF-36” manufactured by Eye Graphics Co., Ltd. was used as the UV illuminance / light meter.
粘着剤層の平均厚さが3μmとなるようにした以外は、前記実施例1と同様に両面粘着シートを作製した。 (Example 2)
A double-sided PSA sheet was prepared in the same manner as in Example 1 except that the average thickness of the PSA layer was 3 μm.
粘着剤層の平均厚さが10μmとなるようにした以外は、前記実施例1と同様に両面粘着シートを作製した。 (Example 3)
A double-sided PSA sheet was prepared in the same manner as in Example 1 except that the average thickness of the PSA layer was 10 μm.
粘着剤組成物Aのトリス(アクリロキシエチル)イソシアヌレート(東亜合成社製、商品名「アロニックスM-315」)20質量部を10質量部とした以外は、前記実施例1同様にして粘着剤組成物Bを調製し、両面粘着シートを作製した。 Example 4
Adhesive as in Example 1 except that 20 parts by mass of tris (acryloxyethyl) isocyanurate (trade name “Aronix M-315”, manufactured by Toagosei Co., Ltd.) of the adhesive composition A was changed to 10 parts by mass. Composition B was prepared to produce a double-sided PSA sheet.
粘着剤組成物Aのトリス(アクリロキシエチル)イソシアヌレート(東亜合成社製、商品名「アロニックスM-315」)20質量部を40質量部とした以外は、前記実施例1同様にして粘着剤組成物Cを調製し、両面粘着シートを作製した。 (Example 5)
Adhesive as in Example 1 except that 20 parts by mass of tris (acryloxyethyl) isocyanurate (trade name “Aronix M-315” manufactured by Toagosei Co., Ltd.) of the adhesive composition A was changed to 40 parts by mass. Composition C was prepared to produce a double-sided PSA sheet.
第2の基材フィルムを変更し、第2の剥離フィルムの剥離剤層の表面の算術平均粗さRa2および最大突起高さRp2を表1に示す値となるように第2の剥離フィルムを作製した以外は、前記実施例1と同様に両面粘着シートを作製した。 (Examples 6 and 7)
The second release film was changed so that the arithmetic average roughness Ra 2 and the maximum protrusion height Rp 2 of the surface of the release agent layer of the second release film were changed to the values shown in Table 1. A double-sided PSA sheet was prepared in the same manner as in Example 1 except that was prepared.
粘着剤組成物Aのトリス(アクリロキシエチル)イソシアヌレート(東亜合成社製、商品名「アロニックスM-315」)20質量部を7.5質量部とした以外は、前記実施例1同様にして粘着剤組成物Dを調製し、両面粘着シートを作製した。 (Example 8)
Except that 20 parts by mass of Tris (acryloxyethyl) isocyanurate (trade name “Aronix M-315”, manufactured by Toagosei Co., Ltd.) of the adhesive composition A was 7.5 parts by mass, the same as in Example 1 above. A pressure-sensitive adhesive composition D was prepared to prepare a double-sided pressure-sensitive adhesive sheet.
粘着剤層の平均厚さが2μmとなるようにした以外は、前記実施例1と同様に両面粘着シートを作製した。 Example 9
A double-sided PSA sheet was prepared in the same manner as in Example 1 except that the average thickness of the PSA layer was 2 μm.
第1の基材フィルムを変更し、第1の剥離フィルムの剥離剤層の表面の算術平均粗さRa1および最大突起高さRp1を表1に示す値となるように第1の剥離フィルムを作製した以外は、前記実施例1と同様に両面粘着シートを作製した。 (Example 10)
The first release film was changed so that the arithmetic average roughness Ra 1 and the maximum protrusion height Rp 1 of the surface of the release agent layer of the first release film were changed to the values shown in Table 1. A double-sided PSA sheet was prepared in the same manner as in Example 1 except that was prepared.
第2の基材フィルムを変更し、第2の剥離フィルムの剥離剤層の表面の算術平均粗さRa2および最大突起高さRp2を表1に示す値となるように第2の剥離フィルムを作製した以外は、前記実施例1と同様に両面粘着シートを作製した。 (Comparative Examples 1 and 2)
The second release film was changed so that the arithmetic average roughness Ra 2 and the maximum protrusion height Rp 2 of the surface of the release agent layer of the second release film were changed to the values shown in Table 1. A double-sided PSA sheet was prepared in the same manner as in Example 1 except that was prepared.
粘着剤組成物Aのトリス(アクリロキシエチル)イソシアヌレート(東亜合成社製、商品名「アロニックスM-315」)20質量部を5質量部とした以外は、前記実施例1同様にして粘着剤組成物Eを調製し、両面粘着シートを作製した。 (Comparative Example 3)
Adhesive as in Example 1 except that 20 parts by mass of tris (acryloxyethyl) isocyanurate (trade name “Aronix M-315” manufactured by Toagosei Co., Ltd.) of the adhesive composition A was changed to 5 parts by mass. Composition E was prepared to produce a double-sided PSA sheet.
・測定周波数:1Hz
・測定温度:23℃ Sample form: 8 mmφ × 3 mm cylinder (produced by laminating an adhesive layer and then cutting it into a cylinder)
・ Measurement frequency: 1Hz
・ Measurement temperature: 23 ℃
以上のようにして得られた両面粘着シートに関して、以下のような評価を行った。 [2] Evaluation The following evaluation was performed on the double-sided PSA sheet obtained as described above.
各実施例および各比較例の両面粘着シートについて、KEYENCE製デジタル顕微鏡を用いて、700μm×500μmの視野範囲内に発生していたラミ気泡(3μm以上)の数をカウントし、下記判定基準に従い評価した。
・判定基準 [2.1] Evaluation of Lami Bubbles Using the KEYENCE digital microscope, the number of Lami bubbles (3 μm or more) generated in the field of view of 700 μm × 500 μm was measured for the double-sided pressure-sensitive adhesive sheets of each Example and each Comparative Example. Counted and evaluated according to the following criteria.
・ Criteria
△ :ラミ気泡が10個未満だった。
× :ラミ気泡が10個以上だった。 ○: Lami bubbles were not generated.
Δ: Lami bubbles were less than 10.
×: There were 10 or more lami bubbles.
各実施例および各比較例の両面粘着シートを幅500mmのロール形態に巻取った。次に第1の剥離フィルムを剥離速度10m/分、剥離角度90°の条件で、10m剥離したとき、第1の剥離フィルムへの粘着剤の転着の有無を目視にて確認した。その結果を、以下の評価基準で判定した。 [2.2] Evaluation of transfer phenomenon (crying separation) The double-sided PSA sheet of each Example and each Comparative Example was wound into a roll having a width of 500 mm. Next, when the first release film was peeled for 10 m under the conditions of a peeling speed of 10 m / min and a peeling angle of 90 °, the presence or absence of transfer of the adhesive to the first release film was visually confirmed. The result was determined according to the following evaluation criteria.
× :第1の剥離フィルムへの転着が発生した。 ○: There was no transfer to the first release film.
X: Transfer to the first release film occurred.
各実施例および各比較例の両面粘着シートから第1の剥離フィルムを引き剥がして粘着剤層を露出させた。次に、露出した粘着剤層を、ディスコティック液晶層付偏光フィルムからなる偏光フィルムと視野角拡大フィルムとが一体化した偏光板に貼合した。得られた粘着剤層付き偏光板を、裁断装置(荻野製作所社製スーパーカッター、PN1-600)を用いて233mm×309mmサイズに裁断した。次いで、第2の剥離フィルムを引き剥がして粘着剤層を露出させた。次に、露出した粘着剤層を無アルカリガラス(コーニング社製,イーグルXG)に貼付してサンプルを得た。その後、サンプルを栗原製作所製オートクレーブにて0.5MPa、50℃で、20分加圧した。その後、サンプルを下記の耐久条件の環境下に静置した。500時間後に、10倍ルーペを用いてサンプルの観察を行った。
外観変化は以下を基準とした。 [2.3] Durability Evaluation The pressure-sensitive adhesive layer was exposed by peeling off the first release film from the double-sided PSA sheet of each Example and each Comparative Example. Next, the exposed pressure-sensitive adhesive layer was bonded to a polarizing plate in which a polarizing film composed of a polarizing film with a discotic liquid crystal layer and a viewing angle widening film were integrated. The obtained polarizing plate with the pressure-sensitive adhesive layer was cut into a size of 233 mm × 309 mm using a cutting device (Super cutter manufactured by Hadano Seisakusho, PN1-600). Subsequently, the 2nd peeling film was peeled off and the adhesive layer was exposed. Next, the exposed adhesive layer was affixed to non-alkali glass (Corning, Eagle XG) to obtain a sample. Then, the sample was pressurized at 0.5 MPa and 50 ° C. for 20 minutes in an autoclave manufactured by Kurihara Seisakusho. Then, the sample was left still in the environment of the following durability conditions. After 500 hours, the sample was observed using a 10-fold magnifier.
Appearance change was based on the following.
△ :サンプルの4辺において、外周端部から0.6mm以上の部位に欠点が無かった。
× :サンプルの4辺の少なくとも1辺において、外周端部から0.6mm以上の部位に、粘着剤の浮き、粘着剤の剥がれ、粘着剤に発泡、粘着剤にスジなどの0.1mm以上の粘着剤の外観異常欠点があった。 ○: There were no defects on the four sides of the sample.
Δ: On the four sides of the sample, there was no defect at a portion of 0.6 mm or more from the outer peripheral edge.
×: At least one of the four sides of the sample has a pressure-sensitive adhesive float, pressure-sensitive adhesive peeling, pressure-sensitive adhesive foaming, pressure-sensitive adhesive streaks, etc. There was an abnormal appearance defect of the adhesive.
・80℃ドライ
・60℃90%RH
・HS(-35℃と70℃で各1時間サイクル)環境
これらの結果を表1に合わせて示した。 <Durability conditions>
・ 80 ℃ dry ・ 60 ℃ 90% RH
HS (1 hour cycle at −35 ° C. and 70 ° C.) environment These results are shown in Table 1.
10 粘着剤層
101 第1の面
102 第2の面
11 第1の剥離フィルム
111 第1の剥離剤層
112 第1の基材フィルム
12 第2の剥離フィルム
121 第2の剥離剤層
122 第2の基材フィルム DESCRIPTION OF SYMBOLS 1 Double-
Claims (4)
- 第1の面と第2の面とを備える粘着剤層と、
前記粘着剤層の前記第1の面に貼着された第1の剥離フィルムと、
前記粘着剤層の前記第2の面に貼着された第2の剥離フィルムと、を有し、
23℃における前記粘着剤層の貯蔵弾性率が、0.3MPa以上であり、
前記第2の剥離フィルムの前記粘着剤層からの剥離力は、前記第1の剥離フィルムの前記粘着剤層からの剥離力よりも小さく、
前記第2の剥離フィルムは、前記粘着剤層と接する面の算術平均粗さRa2が30nm以下であり、かつ、その最大突起高さRp2が250nm以下であるように構成されていることを特徴とする両面粘着シート。 An adhesive layer comprising a first surface and a second surface;
A first release film adhered to the first surface of the pressure-sensitive adhesive layer;
A second release film adhered to the second surface of the pressure-sensitive adhesive layer,
The storage elastic modulus of the pressure-sensitive adhesive layer at 23 ° C. is 0.3 MPa or more,
The peeling force from the pressure-sensitive adhesive layer of the second release film is smaller than the peeling force from the pressure-sensitive adhesive layer of the first release film,
The second release film is configured such that the arithmetic average roughness Ra 2 of the surface in contact with the pressure-sensitive adhesive layer is 30 nm or less and the maximum protrusion height Rp 2 is 250 nm or less. A featured double-sided pressure-sensitive adhesive sheet. - 前記第1の剥離フィルムは、前記粘着剤層と接する面の算術平均粗さRa1が40nm以下であり、かつ、その最大突起高さRp1が700nm以下であるように構成されている請求項1に記載の両面粘着シート。 The first release film, the is the arithmetic average roughness Ra 1 of the surface in contact with the adhesive layer is 40nm or less, and claim its maximum projection height Rp 1 is configured to be 700nm or less 2. The double-sided pressure-sensitive adhesive sheet according to 1.
- 前記粘着剤層の平均厚さは、3~10μmである請求項1または2に記載の両面粘着シート。 The double-sided pressure-sensitive adhesive sheet according to claim 1 or 2, wherein the average thickness of the pressure-sensitive adhesive layer is 3 to 10 µm.
- 前記第1の剥離フィルムの前記粘着剤層からの剥離力をX[mN/25mm]、前記第2の剥離フィルムの前記粘着剤層からの剥離力をY[mN/25mm]としたとき、X-Y≧5の関係を満足する請求項1ないし3のいずれか1項に記載の両面粘着シート。 When the peel force from the pressure-sensitive adhesive layer of the first release film is X [mN / 25 mm] and the peel force from the pressure-sensitive adhesive layer of the second release film is Y [mN / 25 mm], X The double-sided pressure-sensitive adhesive sheet according to any one of claims 1 to 3, which satisfies a relationship of -Y≥5.
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JP2019123813A (en) * | 2018-01-17 | 2019-07-25 | リンテック株式会社 | Adhesive sheet |
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EP3173451A1 (en) | 2015-11-27 | 2017-05-31 | Nitto Denko Corporation | Pressure-sensitive adhesive sheet and release film-supported pressure-sensitive adhesive sheet |
US10836932B2 (en) | 2015-11-27 | 2020-11-17 | Nitto Denko Corporation | Pressure-sensitive adhesive sheet and release film-supported pressure-sensitive adhesive sheet |
JP2019123813A (en) * | 2018-01-17 | 2019-07-25 | リンテック株式会社 | Adhesive sheet |
JP7009226B2 (en) | 2018-01-17 | 2022-01-25 | リンテック株式会社 | Adhesive sheet |
Also Published As
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TW201437319A (en) | 2014-10-01 |
CN105008477B (en) | 2016-08-17 |
TWI532817B (en) | 2016-05-11 |
KR20150138241A (en) | 2015-12-09 |
KR102041228B1 (en) | 2019-11-06 |
JPWO2014156335A1 (en) | 2017-02-16 |
JP6246791B2 (en) | 2017-12-13 |
CN105008477A (en) | 2015-10-28 |
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