WO2014157445A1 - Double-sided adhesive sheet - Google Patents
Double-sided adhesive sheet Download PDFInfo
- Publication number
- WO2014157445A1 WO2014157445A1 PCT/JP2014/058734 JP2014058734W WO2014157445A1 WO 2014157445 A1 WO2014157445 A1 WO 2014157445A1 JP 2014058734 W JP2014058734 W JP 2014058734W WO 2014157445 A1 WO2014157445 A1 WO 2014157445A1
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- WIPO (PCT)
- Prior art keywords
- sensitive adhesive
- pressure
- adhesive layer
- release film
- film
- Prior art date
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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
- 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
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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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- 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
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)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
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
-
- 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
-
- 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
-
- 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
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
- C09J7/403—Adhesives in the form of films or foils characterised by release liners characterised by the structure of the release feature
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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
- B32B2405/00—Adhesive articles, e.g. adhesive tapes
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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
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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
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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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
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/124—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present on both sides of the carrier, e.g. double-sided adhesive tape
- C09J2301/1242—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present on both sides of the carrier, e.g. double-sided adhesive tape the opposite adhesive layers being different
-
- 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 by using a double-sided pressure-sensitive adhesive sheet composed of a member such as a liquid crystal cell and an adhesive. Moreover, such a double-sided adhesive sheet forms an adhesive layer by apply
- the conventional double-sided pressure-sensitive adhesive sheet has not been able to sufficiently prevent the generation of crushed skin.
- a part of the pressure-sensitive adhesive layer sticks to one release film, and a pressure-sensitive adhesive layer that is smooth and has a good appearance does not remain on the other release film.
- a phenomenon called so-called crying separation occurred.
- the object of the present invention is to prevent both of the generation of wrinkles on the surface of the pressure-sensitive adhesive layer and the transfer phenomenon called so-called crying separation when the roll is wound and stored. It is to provide an adhesive sheet.
- 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 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 arithmetic average roughness Ra of the surface opposite to the surface in contact with the pressure-sensitive adhesive layer of the first release film and the second release film is 5 to 35 nm, and the maximum protrusion height Rp is 50.
- a double-sided pressure-sensitive adhesive sheet characterized by being -400 nm.
- 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 double-sided pressure-sensitive adhesive sheet according to any one of (1) to (4), wherein the double-sided pressure-sensitive adhesive sheet satisfies the relationship of XY ⁇ 5.
- the present invention for example, it is used for sticking an optical functional film such as a polarizing plate, and a plurality of minute irregularities are generated on the surface of the pressure-sensitive adhesive layer when stored in a roll shape. It is possible to provide a double-sided pressure-sensitive adhesive sheet capable of preventing the transfer phenomenon referred to as crying separation. Moreover, it becomes possible to provide the double-sided adhesive sheet which can suppress the electric charging at the time of drawing out a blocking and peeling film from a roll.
- 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 pressure-sensitive adhesive layer 10 does not have anything that becomes a support after the first release film 11 and the second release film 12 have been removed.
- the double-sided pressure-sensitive adhesive sheet of the present invention is the double-sided pressure-sensitive adhesive sheet 1 having the pressure-sensitive adhesive layer 10, the first release film 11, and the second release film 12, and has the following characteristics.
- the peeling force from the adhesive layer 10 of the second release film 12 is configured to be smaller than the peeling force from the adhesive layer 10 of the first release film 11, and the first release film 11 and the first release film 11 2 is characterized in that the arithmetic average roughness Ra of the surface opposite to the surface in contact with the adhesive layer 10 of the release film 12 is 5 to 35 nm, and the maximum protrusion height Rp is 50 to 400 nm.
- the arithmetic average roughness Ra of the surface opposite to the surface in contact with the adhesive layer 10 of the release film 12 is 5 to 35 nm
- the maximum protrusion height Rp is 50 to 400 nm.
- the double-sided pressure-sensitive adhesive sheet 1 is rolled up and stored / conveyed, the first surface 101 and the second surface 102 of the pressure-sensitive adhesive layer 10 have minute irregularities (skin skin). ) Can be prevented.
- the 2nd peeling film 12 is made into the adhesive layer 10 by making the peeling force from the adhesive layer 10 of the 2nd peeling film 12 smaller than the peeling force from the adhesive layer 10 of the 1st peeling film.
- a part of the pressure-sensitive adhesive layer 10 sticks to the second release film 12, and the phenomenon that the pressure-sensitive adhesive layer in a smooth and good appearance does not remain on the first release film, so-called crying It is possible to prevent the occurrence of a so-called transfer phenomenon.
- the peeling force from the adhesive layer 10 means the peeling force measured as follows.
- the peel force was measured in accordance with JIS-Z0237.
- the double-sided pressure-sensitive adhesive sheet 1 was cut into a width of 25 mm and a length of 200 mm, and the release film was 300 mm / mm in a state where the pressure-sensitive adhesive layer 10 was fixed using a tensile tester. It shall be performed by pulling in the direction of 180 ° at a speed of minutes.
- the pressure-sensitive adhesive layer 10 has a first surface 101 and a second surface 102.
- pressure-sensitive adhesives such as acrylic pressure-sensitive adhesives, polyester-based pressure-sensitive adhesives, and urethane-based pressure-sensitive adhesives can be used without limitation, but acrylic pressure-sensitive adhesives are preferred.
- acrylic pressure-sensitive adhesives are preferred.
- examples of the form of the pressure-sensitive adhesive include solvent type and emulsion type.
- acrylic adhesives it is preferable to use a (meth) acrylic acid ester copolymer.
- the acrylic ester copolymer has high transparency and can be suitably used for optical parts. Moreover, the acrylic ester copolymer is excellent in durability.
- the pressure-sensitive adhesive is an acrylic pressure-sensitive adhesive
- a polymer mainly comprising a main monomer component that provides tackiness, a comonomer component that provides adhesiveness and cohesive force, a functional group-containing monomer component for improving crosslinking points and adhesion, or It can be composed of a copolymer.
- main monomer components include ester moieties such as methyl acrylate, ethyl acrylate, butyl acrylate, amyl acrylate, 2-ethylhexyl acrylate, octyl acrylate, cyclohexyl acrylate, benzyl acrylate, and methoxyethyl acrylate.
- ester moieties such as methyl acrylate, ethyl acrylate, butyl acrylate, amyl acrylate, 2-ethylhexyl acrylate, octyl acrylate, cyclohexyl acrylate, benzyl acrylate, and methoxyethyl acrylate.
- alkyl methacrylates having 1 to 20 carbon atoms in the alkyl group, and methacrylic acid having 1 to 20 carbon atoms in the alkyl portion of the ester moiety such as butyl methacrylate, 2-ethylhex
- Examples include acid alkyl esters.
- Examples of the comonomer component include methyl acrylate, methyl methacrylate, ethyl methacrylate, vinyl acetate, styrene, acrylonitrile, and the like.
- the functional group-containing monomer component preferably contains at least one of a hydroxyl group, a carboxyl group, and an amino group as a functional group.
- a hydroxyl group preferably contains at least one of 2-hydroxyethyl (meth) acrylate, (meth) acrylic acid.
- (Meth) acrylic such as 2-hydroxypropyl, 3-hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, 3-hydroxybutyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate Acid hydroxyalkyl ester; (meth) acrylic acid monomethylaminoethyl, (meth) acrylic acid monoethylaminoethyl, (meth) acrylic acid monomethylaminopropyl, (meth) acrylic acid monoethylaminopropyl, etc.
- Alkylaminoalkyl acrylic acid, Methacrylic acid, crotonic acid, maleic acid, itaconic acid, ethylenically unsaturated carboxylic acids such as citraconic acid.
- the (meth) acrylic acid ester copolymer is not particularly limited with respect to the copolymerization form, and may be any of random, block, and graft copolymers.
- the (meth) acrylic acid ester-based copolymer those having a mass average molecular weight of 500,000 or more are preferable, those having 600,000 to 2,000,000 are more preferable, and 700,000 to 180 are preferable. It is more preferable to use one of many.
- the double-sided pressure-sensitive adhesive sheet 1 has sufficient adhesion to the adherend and adhesion durability, and can more effectively prevent the occurrence of floating and peeling.
- the mass average molecular weight is a value in terms of polystyrene measured by a gel permeation chromatography (GPC) method.
- the content of units derived from the functional group-containing monomer component 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 with a crosslinking agent described later, and durability is improved.
- a more preferable content of the unit derived from the functional group-containing monomer component is 0.05 to 7.0% by mass, and a range of 0.2 to 6.0% by mass is particularly preferable.
- the (meth) acrylic acid ester copolymer (A) one type may be used, or two or more types may be used in combination.
- an acrylic pressure-sensitive adhesive usually does not have an unsaturated bond in the molecule, so that stability to light and oxygen can be improved. Furthermore, a pressure-sensitive adhesive having quality and characteristics according to the application can be obtained by appropriately selecting the type and molecular weight of the monomer.
- the pressure-sensitive adhesive layer 10 is prepared by preparing a pressure-sensitive adhesive solution (pressure-sensitive adhesive composition) in which such a pressure-sensitive adhesive is dissolved in an organic solvent, and applying this onto the first release film 11 or the second release film 12. Can be formed.
- a pressure-sensitive adhesive solution pressure-sensitive adhesive composition
- Such a pressure-sensitive adhesive composition may be either a crosslinked type that undergoes crosslinking treatment or a non-crosslinked type that does not undergo crosslinking treatment, but a crosslinked type is more preferred.
- a cross-linked type is used, a pressure-sensitive adhesive layer with better cohesion can be formed.
- the crosslinking agent used in the crosslinking adhesive composition include isocyanate compounds, epoxy compounds, metal chelate compounds, metal alkoxides, metal salts, amine compounds, hydrazine compounds, and aldehyde compounds.
- Examples of the organic solvent used for preparing the pressure-sensitive adhesive composition include toluene, xylene, methanol, ethanol, isobutanol, n-butanol, acetone, methyl ethyl ketone, tetrahydrofuran, and ethyl acetate.
- the concentration of the pressure-sensitive adhesive composition is adjusted so that the solid content is in the range of about 5 to 60% by mass using these organic solvents for the convenience of coating.
- Coating of the pressure-sensitive adhesive composition to the first release film 11 or the second release film 12 is, for example, a bar coating method, a reverse roll coating method, a knife coating method, a roll knife coating method, a gravure coating method, an air doctor.
- the coating can be performed by a conventionally known coating method such as a coating method or a doctor blade coating method.
- the average thickness of the pressure-sensitive adhesive layer 10 is preferably 3 to 30 ⁇ m, more preferably 5 to 28 ⁇ m. Thereby, it can be set as the thinness suitable for using for a thin display.
- the proportion of the unevenness outside the range of ⁇ 0.2 ⁇ m from the reference surface in the first surface 101 of the pressure-sensitive adhesive layer 10 is preferably 20% or less.
- the proportion of the unevenness outside the range of ⁇ 0.2 ⁇ m from the reference surface in the second surface 102 of the pressure-sensitive adhesive layer 10 is preferably 20% or less.
- 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 film or a multilayer film having two or more layers made of the same or different materials. Such a multilayer film may be obtained by laminating films formed in advance through an adhesive layer as necessary, or by coating a resin film forming composition on a film formed in advance. But you can.
- the resin layer forming composition for forming the resin layer is mainly composed of an epoxy compound, an acrylate compound, a urethane acrylate compound, a polyester compound, etc., and if necessary, a crosslinking agent, a catalyst, and photopolymerization start. And those containing an agent, an ultraviolet absorber and the like.
- These composition for resin layer formation may have sclerosis
- the arithmetic average roughness Ra of the outer surface of the first base film 112 is obtained by using the multilayer film in which the resin layer forming composition is coated on the film formed in advance and the resin layer is formed.
- the maximum protrusion height Rp can be adjusted.
- 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 arithmetic average roughness Ra of the surface of the first release film 11 opposite to the surface in contact with the pressure-sensitive adhesive layer 10 is 5 to 35 nm, and more preferably 13 to 30 nm. Thereby, it is possible to more effectively prevent the skin from being generated on the first surface 101 and the second surface 102 of the pressure-sensitive adhesive layer 10 over time after winding the double-sided pressure-sensitive adhesive sheet 1 into a roll. it can.
- the arithmetic average roughness Ra is less than the lower limit value, the first release film 11 may be blocked over time after the first release film 11 is wound into a roll, or the first release film 11 may be blocked. It is impossible to prevent the release film 11 from being charged when it is fed out from the roll.
- the wound surface of the pressure-sensitive adhesive layer 10 may be damaged over time on the first surface 101 and the second surface 102 after the double-sided pressure-sensitive adhesive sheet 1 is rolled up. Can not be prevented.
- the maximum protrusion height Rp on the surface opposite to the surface in contact with the pressure-sensitive adhesive layer 10 of the first release film 11 is 50 to 400 nm, and more preferably 90 to 240 nm.
- 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.
- examples of the silicone compound include an addition reaction type, a condensation reaction type, an ultraviolet curable type, and an electron beam curable type.
- 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 cure shrinkage compared to the condensation reaction type.
- 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 first release film 11 has an arithmetic average roughness Ra of 5 to 50 nm on the surface in contact with the pressure-sensitive adhesive layer 10 (the outer surface of the first release agent layer 111), and its maximum protrusion height Rp. Is preferably 50 to 1000 nm, the arithmetic average roughness Ra of the surface in contact with the pressure-sensitive adhesive layer 10 is 13 to 50 nm, and the maximum protrusion height Rp is more preferably 120 to 1000 nm. Thereby, when the adhesive layer 10 is formed on the 1st peeling film 11, the surface shape of the 1st surface 101 of the adhesive layer 10 can be made favorable.
- the proportion of the unevenness outside the range of ⁇ 0.2 ⁇ m from the reference surface on the outer surface of the first release agent layer 111 is 20% or less.
- 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 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 substrate film 112 described in the section of the first release film 11 described above can be used.
- the arithmetic average roughness Ra of the surface of the second release film 12 opposite to the surface in contact with the pressure-sensitive adhesive layer 10 is 5 to 35 nm, and more preferably 12 to 30 nm. Thereby, when the double-sided pressure-sensitive adhesive sheet 1 is wound up in a roll shape, it is possible to more effectively prevent the skin from being generated on the first surface 101 and the second surface 102 of the pressure-sensitive adhesive layer 10. . On the other hand, if the arithmetic average roughness Ra is less than the lower limit value, the second release film 12 may block over time after the second release film 12 is wound into a roll, or the second release film 12 may be blocked. It is impossible to prevent the release film 12 from being charged when it is fed out from the roll.
- the wound surface of the pressure-sensitive adhesive layer 10 may be damaged over time on the first surface 101 and the second surface 102 after the double-sided pressure-sensitive adhesive sheet 1 is rolled up. Can not be prevented.
- the maximum protrusion height Rp on the surface opposite to the surface in contact with the pressure-sensitive adhesive layer 10 of the second release film 12 is 50 to 400 nm, more preferably 120 to 240 nm.
- 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 second release agent it can be appropriately selected from the materials constituting the first release agent described in the section of the first release film.
- 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.
- the second release film 12 has an arithmetic average roughness Ra of 5 to 50 nm on the surface in contact with the pressure-sensitive adhesive layer 10 (the outer surface of the second release agent layer 121), and its maximum protrusion height Rp. Is preferably 50 to 1000 nm, the arithmetic average roughness Ra of the surface in contact with the pressure-sensitive adhesive layer 10 is 13 to 50 nm, and the maximum protrusion height Rp is more preferably 120 to 1000 nm.
- the proportion of the unevenness outside the range of ⁇ 0.2 ⁇ m from the reference surface on the outer surface of the second release agent layer 121 is 20% or less.
- Example 1 Preparation of double-sided PSA sheet (Example 1) 1. Preparation of First Release Film A polyethylene terephthalate (PET) film (thickness 38 ⁇ m, arithmetic average roughness Ra: 20 nm, maximum protrusion height Rp: 203 nm) having the same front and back roughness was prepared as a first base film. .
- PET polyethylene terephthalate
- the first release agent layer-forming composition A having the following composition was applied with a bar coater so that the thickness after drying was 0.1 ⁇ m. And dried at 120 ° C. for 1 minute to provide a first release agent layer. This obtained the 1st peeling film.
- Table 1 shows the projection height Rp and the ratio of the unevenness outside the range of ⁇ 0.2 ⁇ m from the reference surface on the first release agent layer side surface of the first release film.
- first release agent layer-forming composition A Silicone resin solution containing organopolysiloxane with vinyl group and organopolysiloxane with hydrosilyl group (manufactured by Toray Dow Corning Co., Ltd., trade name “BY24-561”, solid content 30% by mass) in terms of solid content 30 parts by mass and 15 parts by mass of solid resin in terms of solid content of MQ resin (made by Toray Dow Corning Co., Ltd., trade name “SD7292”, solid content 71% by mass) having a vinyl group, and solid content concentration in toluene solvent was diluted and mixed so as to be 1.0% by mass.
- 2 parts by mass of a platinum-based catalyst (trade name “SRX-212”, manufactured by Toray Dow Corning Co., Ltd., solid content: 100% by mass) was added to prepare a first release agent layer forming composition A.
- Second Release Film A polyethylene terephthalate (PET) film (thickness 38 ⁇ m, arithmetic average roughness Ra: 19 nm, maximum protrusion height Rp: 194 nm) having the same front and back surface roughness was prepared as a second base film. .
- PET polyethylene terephthalate
- a second release agent layer-forming composition B having the following composition was applied to one surface of the second base film with a bar coater so that the thickness after drying was 0.1 ⁇ m. And dried at 120 ° C. for 1 minute to provide a second release agent layer.
- Table 1 shows the protrusion height Rp and the ratio of the unevenness outside the range of ⁇ 0.2 ⁇ m from the reference surface on the surface of the second release film on the second release agent layer side.
- Second release agent layer-forming composition B 100 parts by mass of silicone resin (manufactured by Shin-Etsu Chemical Co., Ltd .: trade name “KS847H”, solid content concentration 30% by mass) and 1 part by mass of a platinum-based catalyst (manufactured by Shin-Etsu Chemical Co., Ltd .: trade name “CAT-PL50T”, solid content)
- the second release agent layer forming composition B having a solid content concentration of 1% by mass was prepared by diluting with 100% by mass of toluene.
- 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 polymer (A) 0.15 parts by mass of a polyisocyanate-based crosslinking agent (trade name “Takenate D-110N”, solid content concentration 75% by mass, manufactured by Mitsui Chemicals), and silane
- a coupling agent (“KBM-403” manufactured by Shin-Etsu Chemical Co., Ltd., solid content concentration: 100% by mass
- toluene was added as a solvent to adjust the solid content to 15% by mass.
- An adhesive composition A was prepared.
- the mass average molecular weight is a value in terms of polystyrene measured by a gel permeation chromatography (GPC) method.
- Example 2 A double-sided PSA sheet was prepared in the same manner as in Example 1 except that the second release film was obtained as follows.
- PET polyethylene terephthalate
- the resin layer forming composition A is applied to the outer surface of the PET film with a bar coater, heated and dried at 150 ° C. for 40 seconds to cure the resin material, and the thickness is 0.6 ⁇ m.
- a second substrate film was produced by forming a resin layer.
- the thickness after drying the second release agent composition B on the surface (PET film side) opposite to the side on which the resin layer is formed in the second base film is 0.1 ⁇ m.
- a second release film was prepared by coating with a bar coater and drying at 120 ° C. for 1 minute to provide a second release agent layer.
- Table 1 shows the protrusion height Rp and the ratio of the unevenness outside the range of ⁇ 0.2 ⁇ m from the reference surface on the surface of the second release film on the second release agent layer side.
- Example 3 A double-sided PSA sheet was produced in the same manner as in Example 2 except that the thickness of the resin layer of the second base film was 0.8 ⁇ m.
- Example 4 A double-sided PSA sheet was prepared in the same manner as in Example 2 except that the thickness of the resin layer of the second base film was 0.5 ⁇ m.
- Example 5 Except for changing the second base film of the second release film to a polyethylene terephthalate (PET) film (thickness 38 ⁇ m, arithmetic average roughness Ra: 32 nm, maximum protrusion height Rp: 230 nm) with the same roughness on both sides Produced a double-sided PSA sheet as in Example 1.
- PET polyethylene terephthalate
- the second base film of the second release film is a polyethylene terephthalate (PET) film (thickness 38 ⁇ m, surface on the second release agent layer side with different roughness on the front and back surfaces (arithmetic average roughness Ra: 40 nm, maximum (Projection height Rp: 900 nm), except for the surface opposite to the second release agent layer (arithmetic average roughness Ra: 19 nm, maximum projection height Rp: 194 nm)), the same as in Example 1 A double-sided PSA sheet was prepared.
- PET polyethylene terephthalate
- Example 7 The second substrate film of the second release film was changed to a polyethylene terephthalate (PET) film (thickness 38 ⁇ m, arithmetic average roughness Ra: 15 nm, maximum protrusion height Rp: 131 nm) having the same front and back roughness. Except for the above, a double-sided PSA sheet was prepared in the same manner as in Example 1.
- PET polyethylene terephthalate
- the first base film of the first release film and the second base film of the second release film are made of a polyethylene terephthalate (PET) film (thickness: 38 ⁇ m, arithmetic average roughness Ra: 10 nm).
- PET polyethylene terephthalate
- a double-sided PSA sheet was prepared in the same manner as in Example 1 except that the maximum protrusion height Rp was changed to 93 nm.
- the first base film of the first release film and the second base film of the second release film are made of a polyethylene terephthalate (PET) film (thickness: 38 ⁇ m, arithmetic average roughness Ra: 40 nm).
- PET polyethylene terephthalate
- a double-sided PSA sheet was prepared in the same manner as in Example 1 except that the maximum protrusion height Rp was changed to 535 nm.
- PET polyethylene terephthalate
- the resin layer forming composition A is applied to the outer surface of the PET film with a bar coater, heated and dried at 150 ° C. for 40 seconds to cure the resin material, and the thickness is 0.6 ⁇ m.
- a second substrate film was produced by forming a resin layer.
- the thickness of the second release agent composition B after drying is 0.1 ⁇ m on the surface (PET film side) opposite to the surface on which the resin layer is formed in the second base film.
- a second release film was prepared by coating with a bar coater and drying at 120 ° C. for 1 minute to provide a second release agent layer.
- Comparative Example 4 A double-sided PSA sheet was prepared in the same manner as Comparative Example 2 except that the thickness of the release agent layer of the second release film was 0.6 ⁇ m.
- the surface of the adhesive layer side of the first release film and the second release film used in the double-sided adhesive sheet of each example and comparative example and the surface of the base film side (opposite to the surface in contact with the adhesive layer)
- the arithmetic average roughness Ra and the maximum protrusion height Rp of the side surface were measured according to JIS B 0601-1994 using a surface roughness measuring instrument SV3000S4 (stylus type) manufactured by Mitutoyo Corporation.
- the proportion of the unevenness outside the range of ⁇ 0.2 ⁇ m from the reference surface on the surface of the pressure-sensitive adhesive layer side of the first release film and the second release film used in the double-sided pressure-sensitive adhesive sheet of each Example and Comparative Example is Using the optical interference type surface shape observation device “Wyko NT-1100” [Veeco Co., Ltd.], stitching was performed at 2.5 magnifications in the VSI mode, and the obtained surface shape image in the range of 4 ⁇ 4 mm To binarize the image with a portion outside the range of ⁇ 0.2 ⁇ m from the reference surface and a portion within the range of ⁇ 0.2 ⁇ m, and the unevenness of the portion outside the range of ⁇ 0.2 ⁇ m from the reference surface The area ratio was calculated.
- the peel strength of the first release film and the second release film with respect to the PSA layer is in accordance with JIS-Z0237.
- the measurement was performed by pulling the first release film or the second release film in the 180 ° direction at a speed of 300 mm / min with the pressure-sensitive adhesive layer fixed using a tensile tester.
- the double-sided adhesive sheet of each Example and each comparative example is a reference surface about each of the 1st surface (1st peeling film side) and 2nd surface (2nd peeling film side) of an adhesive layer.
- the area occupancy ratio of the irregularities outside the range of ⁇ 0.2 ⁇ m was measured. If the surface of the pressure-sensitive adhesive layer is smooth, the value is close to 0%.
- stitching was performed at 2.5 magnifications in the VSI mode.
- the double-sided pressure-sensitive adhesive sheet of the present invention was free from appearance defects because it was prevented from being crushed. Moreover, the double-sided adhesive sheet of this invention was excellent in the peelability of each peeling film, blocking resistance, and antistatic property. Moreover, the double-sided pressure-sensitive adhesive sheet of the present invention prevents the occurrence of a transfer phenomenon called crying separation. 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.
- a second release sheet adhered to the second surface of the layer, and the release force of the second release film from the adhesive layer is the adhesive of the first release film.
- An arithmetic average roughness Ra of the surface opposite to the surface in contact with the pressure-sensitive adhesive layer of the first release film and the second release film is smaller than the peel force from the layer, and is 5 to 35 nm; and
- the maximum protrusion height Rp is 50 to 400 nm.
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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、
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1の剥離フィルムおよび前記第2の剥離フィルムの前記粘着剤層と接する面とは反対側の面の算術平均粗さRaが5~35nmであり、かつ、その最大突起高さRpが50~400nmであることを特徴とする両面粘着シート。 Such an object is achieved by the present invention described in (1) to (5) 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 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 arithmetic average roughness Ra of the surface opposite to the surface in contact with the pressure-sensitive adhesive layer of the first release film and the second release film is 5 to 35 nm, and the maximum protrusion height Rp is 50. A double-sided pressure-sensitive adhesive sheet characterized by being -400 nm.
《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。粘着剤層10には、第1の剥離フィルム11および第2の剥離フィルム12を除いてしまった後には支持体となるものが存在しない。 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
<粘着剤層10>
粘着剤層10は、第1の面101と第2の面102とを有する。 Hereinafter, each layer which comprises the double-sided adhesive sheet 1 which concerns on this embodiment is demonstrated in detail.
<
The pressure-sensitive
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 first release film 11 is attached to the
The first release film 11 has a function of protecting the pressure-
また、第1の剥離剤層111の外表面における基準面から±0.2μmの範囲外の凹凸の占める割合が20%以下であるのが好ましい。これにより、第1の剥離フィルム11上に粘着剤層10を形成した際に、粘着剤層10の第1の面101の表面形状を良好にすることができる。 The first release film 11 has an arithmetic average roughness Ra of 5 to 50 nm on the surface in contact with the pressure-sensitive adhesive layer 10 (the outer surface of the first release agent layer 111), and its maximum protrusion height Rp. Is preferably 50 to 1000 nm, the arithmetic average roughness Ra of the surface in contact with the pressure-
Moreover, it is preferable that the proportion of the unevenness outside the range of ± 0.2 μm from the reference surface on the outer surface of the first
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、表裏同粗度のポリエチレンテレフタレート(PET)フィルム(厚さ38μm、算術平均粗さRa:20nm、最大突起高さRp:203nm)を用意した。 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 First Release Film A polyethylene terephthalate (PET) film (thickness 38 μm, arithmetic average roughness Ra: 20 nm, maximum protrusion height Rp: 203 nm) having the same front and back roughness was prepared as a first base 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」、固形分30質量%)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」、固形分71質量%)を固形分換算で15質量部とを、トルエン溶媒にて固形分濃度が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」、固形分100質量%)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)
Silicone resin solution containing organopolysiloxane with vinyl group and organopolysiloxane with hydrosilyl group (manufactured by Toray Dow Corning Co., Ltd., trade name “BY24-561”, solid content 30% by mass) in terms of solid content 30 parts by mass and 15 parts by mass of solid resin in terms of solid content of MQ resin (made by Toray Dow Corning Co., Ltd., trade name “SD7292”, solid content 71% by mass) having a vinyl group, and solid content concentration in toluene solvent Was diluted and mixed so as to be 1.0% by mass. To this solution, 2 parts by mass of a platinum-based catalyst (trade name “SRX-212”, manufactured by Toray Dow Corning Co., Ltd., solid content: 100% by mass) was added to prepare a first release agent layer forming composition A.
第2の基材フィルムとして、表裏同粗度のポリエチレンテレフタレート(PET)フィルム(厚さ38μm、算術平均粗さRa:19nm、最大突起高さRp:194nm)を用意した。 2. Preparation of Second Release Film A polyethylene terephthalate (PET) film (thickness 38 μm, arithmetic average roughness Ra: 19 nm, maximum protrusion height Rp: 194 nm) having the same front and back surface roughness was prepared as a second base film. .
シリコーン樹脂100質量部(信越化学工業社製:商品名「KS847H」、固形分濃度30質量%)と、白金系触媒1質量部(信越化学工業社製:商品名「CAT-PL50T」、固形分濃度100質量%)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 silicone resin (manufactured by Shin-Etsu Chemical Co., Ltd .: trade name “KS847H”, solid content concentration 30% by mass) and 1 part by mass of a platinum-based catalyst (manufactured by Shin-Etsu Chemical Co., Ltd .: trade name “CAT-PL50T”, solid content) The second release agent layer forming composition B having a solid content concentration of 1% by mass was prepared by diluting with 100% by mass of toluene.
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99.0質量部、アクリル酸4-ヒドロキシエチル1.0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、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で攪拌しながら、反応溶液を60℃に昇温し、16時間反応させた後、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、ポリイソシアネート系架橋剤(三井化学社製、商品名「タケネートD-110N」、固形分濃度75質量%)0.15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」、固形分濃度100質量%)0.1質量部を添加混合したものに、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, 99.0 parts by mass of n-butyl acrylate and 1.0 part by mass of 4-hydroxyethyl acrylate 200 parts by mass of ethyl acetate and 0.08 part by mass of 2,2′-azobisisobutyronitrile were charged, and the air in the reaction vessel was replaced with nitrogen gas. While stirring in this nitrogen atmosphere, the reaction solution was heated to 60 ° C., reacted for 16 hours, and then 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 polymer (A), 0.15 parts by mass of a polyisocyanate-based crosslinking agent (trade name “Takenate D-110N”, solid content concentration 75% by mass, manufactured by Mitsui Chemicals), and silane To a mixture of 0.1 parts by mass of a coupling agent (“KBM-403” manufactured by Shin-Etsu Chemical Co., Ltd., solid content concentration: 100% by mass), toluene was added as a solvent 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25μmの厚さとなるように、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、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挟み込み、常温条件下、速度50m/minで貼合し、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 on the release agent layer of the first release film to a thickness of 25 μm after drying, and dried at 90 ° C. for 1 minute to form a pressure-sensitive adhesive layer. did. Next, on the formed pressure-sensitive adhesive layer, a silicone rubber roll (rubber hardness: 80) and a metal roll whose laminating pressure is adjusted to 0.5 MPa so that the release agent layer of the second release film is in contact with the pressure-sensitive adhesive layer, And bonded at a speed of 50 m / min under normal temperature conditions to prepare 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%.
第2の剥離フィルムとして、以下のようにして得られたものを用いた以外は、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 second release film was obtained as follows.
なお、樹脂層形成用組成物Aとしては、主剤としての水酸基を有するビスフェノールA型エポキシ樹脂エステル樹脂溶液(固形分濃度60質量%):100質量部に、架橋剤としてのメチル化メラミン樹脂(固形分濃度100質量%):40質量部と、触媒としてのp-トルエンスルホン酸メタノール溶液(固形分濃度50質量%)5質量部とを添加し、トルエン/メチルエチルケトン(MEK)混合溶媒(トルエン:MEK(質量比)=50:50)で希釈混合して得たものを用いた。 Next, the resin layer forming composition A is applied to the outer surface of the PET film with a bar coater, heated and dried at 150 ° C. for 40 seconds to cure the resin material, and the thickness is 0.6 μm. A second substrate film was produced by forming a resin layer.
In addition, as composition A for resin layer formation, the bisphenol A type epoxy resin ester resin solution which has a hydroxyl group as a main ingredient (solid content concentration of 60 mass%): 100 mass parts, methylated melamine resin (solid) as a crosslinking agent 40 parts by mass and 5 parts by mass of a p-toluenesulfonic acid methanol solution (solid content of 50% by mass) as a catalyst, and a toluene / methyl ethyl ketone (MEK) mixed solvent (toluene: MEK). What was obtained by diluting and mixing at (mass ratio) = 50: 50) was used.
第2の基材フィルムの樹脂層の厚さを0.8μmとした以外は、前記実施例2と同様に両面粘着シートを作製した。 (Example 3)
A double-sided PSA sheet was produced in the same manner as in Example 2 except that the thickness of the resin layer of the second base film was 0.8 μm.
第2の基材フィルムの樹脂層の厚さを0.5μmとした以外は、前記実施例2と同様に両面粘着シートを作製した。 Example 4
A double-sided PSA sheet was prepared in the same manner as in Example 2 except that the thickness of the resin layer of the second base film was 0.5 μm.
第2の剥離フィルムの第2の基材フィルムを、表裏同粗度のポリエチレンテレフタレート(PET)フィルム(厚さ38μm、算術平均粗さRa:32nm、最大突起高さRp:230nm)に変更した以外は、前記実施例1と同様に両面粘着シートを作製した。 (Example 5)
Except for changing the second base film of the second release film to a polyethylene terephthalate (PET) film (thickness 38 μm, arithmetic average roughness Ra: 32 nm, maximum protrusion height Rp: 230 nm) with the same roughness on both sides Produced a double-sided PSA sheet as in Example 1.
第2の剥離フィルムの第2の基材フィルムを、表裏で粗さの異なるポリエチレンテレフタレート(PET)フィルム(厚さ38μm、第2の剥離剤層側の面(算術平均粗さRa:40nm、最大突起高さRp:900nm)、第2の剥離剤層とは反対側の面(算術平均粗さRa:19nm、最大突起高さRp:194nm))に変更した以外は、前記実施例1と同様に両面粘着シートを作製した。 (Example 6)
The second base film of the second release film is a polyethylene terephthalate (PET) film (thickness 38 μm, surface on the second release agent layer side with different roughness on the front and back surfaces (arithmetic average roughness Ra: 40 nm, maximum (Projection height Rp: 900 nm), except for the surface opposite to the second release agent layer (arithmetic average roughness Ra: 19 nm, maximum projection height Rp: 194 nm)), the same as in Example 1 A double-sided PSA sheet was prepared.
第2の剥離フィルムの第2の基材フィルムを、表裏の粗さが同じポリエチレンテレフタレート(PET)フィルム(厚さ38μm、算術平均粗さRa:15nm、最大突起高さRp:131nm)に変更した以外は、前記実施例1と同様に両面粘着シートを作製した。 (Example 7)
The second substrate film of the second release film was changed to a polyethylene terephthalate (PET) film (thickness 38 μm, arithmetic average roughness Ra: 15 nm, maximum protrusion height Rp: 131 nm) having the same front and back roughness. Except for the above, a double-sided PSA sheet was prepared in the same manner as in Example 1.
第1の剥離フィルムの第1の基材フィルムおよび第2の剥離フィルムの第2の基材フィルムを、表裏同粗度のポリエチレンテレフタレート(PET)フィルム(厚さ38μm、算術平均粗さRa:10nm、最大突起高さRp:93nm)に変更した以外は、前記実施例1と同様に両面粘着シートを作製した。 (Example 8)
The first base film of the first release film and the second base film of the second release film are made of a polyethylene terephthalate (PET) film (thickness: 38 μm, arithmetic average roughness Ra: 10 nm). A double-sided PSA sheet was prepared in the same manner as in Example 1 except that the maximum protrusion height Rp was changed to 93 nm.
第2の剥離フィルムの第2の基材フィルムを、表裏同粗度のポリエチレンテレフタレート(PET)フィルム(厚さ38μm、算術平均粗さRa:40nm、最大突起高さRp:535nm)に変更した以外は、前記実施例1と同様に両面粘着シートを作製した。 (Comparative Example 1)
Except for changing the second base film of the second release film to a polyethylene terephthalate (PET) film (thickness 38 μm, arithmetic average roughness Ra: 40 nm, maximum protrusion height Rp: 535 nm) having the same roughness on both sides. Produced a double-sided PSA sheet as in Example 1.
第1の剥離フィルムの第1の基材フィルムおよび第2の剥離フィルムの第2の基材フィルムを、表裏同粗度のポリエチレンテレフタレート(PET)フィルム(厚さ38μm、算術平均粗さRa:40nm、最大突起高さRp:535nm)に変更した以外は、前記実施例1と同様に両面粘着シートを作製した。 (Comparative Example 2)
The first base film of the first release film and the second base film of the second release film are made of a polyethylene terephthalate (PET) film (thickness: 38 μm, arithmetic average roughness Ra: 40 nm). A double-sided PSA sheet was prepared in the same manner as in Example 1 except that the maximum protrusion height Rp was changed to 535 nm.
第2の剥離フィルムとして、以下のようにして得られたものを用いた以外は、前記実施例1と同様に両面粘着シートを作製した。 (Comparative Example 3)
A double-sided PSA sheet was prepared in the same manner as in Example 1 except that the second release film was obtained as follows.
なお、樹脂層形成用組成物Aとしては、主剤としての水酸基を有するビスフェノールA型エポキシ樹脂エステル樹脂溶液(固形分濃度60質量%):100質量部に、架橋剤としてのメチル化メラミン樹脂(固形分濃度100質量%):40質量部と、触媒としてのp-トルエンスルホン酸メタノール溶液(固形分濃度50質量%)5質量部とを添加し、トルエン/メチルエチルケトン(MEK)混合溶媒(トルエン:MEK(質量比)=50:50)で希釈混合して得たものを用いた。 Next, the resin layer forming composition A is applied to the outer surface of the PET film with a bar coater, heated and dried at 150 ° C. for 40 seconds to cure the resin material, and the thickness is 0.6 μm. A second substrate film was produced by forming a resin layer.
In addition, as composition A for resin layer formation, the bisphenol A type epoxy resin ester resin solution which has a hydroxyl group as a main ingredient (solid content concentration of 60 mass%): 100 mass parts, methylated melamine resin as a crosslinking agent (solid 40 parts by mass and 5 parts by mass of a p-toluenesulfonic acid methanol solution (solid content of 50% by mass) as a catalyst, and a toluene / methyl ethyl ketone (MEK) mixed solvent (toluene: MEK). What was obtained by diluting and mixing at (mass ratio) = 50: 50) was used.
第2の剥離フィルムの剥離剤層の厚さを0.6μmとした以外は、前記比較例2と同様に両面粘着シートを作製した。 (Comparative Example 4)
A double-sided PSA sheet was prepared in the same manner as Comparative Example 2 except that the thickness of the release agent layer of the second release film was 0.6 μm.
第2の剥離フィルムの第2の基材フィルムを、表裏同粗度のポリエチレンテレフタレート(PET)フィルム(厚さ38μm、算術平均粗さRa:4nm、最大突起高さRp:35nm)に変更した以外は、前記実施例1と同様に両面粘着シートを作製した。 (Comparative Example 5)
Except for changing the second base film of the second release film to a polyethylene terephthalate (PET) film (thickness 38 μm, arithmetic average roughness Ra: 4 nm, maximum protrusion height Rp: 35 nm) with the same roughness on both sides Produced a double-sided PSA sheet as in Example 1.
これらの結果を表1に示した。 Moreover, about the double-sided adhesive sheet of each Example and each comparative example, it is a reference surface about each of the 1st surface (1st peeling film side) and 2nd surface (2nd peeling film side) of an adhesive layer. The area occupancy ratio of the irregularities outside the range of ± 0.2 μm was measured. If the surface of the pressure-sensitive adhesive layer is smooth, the value is close to 0%. Using an optical interference surface shape observation apparatus “Wyko NT-1100” [manufactured by Veeco Co., Ltd.], stitching was performed at 2.5 magnifications in the VSI mode. From the obtained surface shape image in the range of 4 × 4 mm, the image is binarized with a portion outside the range of ± 0.2 μm from the reference plane and a portion within the range of ± 0.2 μm, and from the reference plane The area ratio occupied by the unevenness in the portion outside the range of ± 0.2 μm was calculated.
These results are shown in Table 1.
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を、第2の剥離フィルムを剥がし、露出した粘着剤層を黒アクリル板(三菱レイヨン社製)に貼合した。その後、第1の剥離フィルムを剥がし、蛍光灯の光を反射させて観察し、写り込んだ蛍光灯の像が歪まずに見える場合は外観良好(A)、歪んで見える場合には外観不良(B)と判断した。 [2.1] Surface state appearance evaluation of first surface of adhesive layer (visual observation)
The double-sided pressure-sensitive adhesive sheet of each example and each comparative example was peeled off the second release film, and the exposed pressure-sensitive adhesive layer was bonded to a black acrylic plate (manufactured by Mitsubishi Rayon Co., Ltd.). Thereafter, the first release film is peeled off, and the fluorescent lamp light is reflected and observed. When the reflected fluorescent lamp image looks undistorted, the appearance is good (A), and when it appears distorted, the appearance is poor ( B).
各実施例および各比較例の両面粘着シートを、第2の剥離フィルムを剥がし、露出した粘着剤層が上になるようにして黒アクリル板(三菱レイヨン社製)の上に乗せ、蛍光灯の光を反射させて観察し、写り込んだ蛍光灯の像が歪まずに見える場合は外観良好(A)、歪んで見える場合には外観不良(B)と判断した。 [2.2] Surface state appearance evaluation of the second surface of the pressure-sensitive adhesive layer (visual observation)
The double-sided PSA sheet of each Example and each Comparative Example was peeled off the second release film and placed on a black acrylic plate (Mitsubishi Rayon Co., Ltd.) with the exposed PSA layer facing up. When the reflected fluorescent light image was seen without distortion, it was judged that the appearance was good (A), and when it looked distorted, the appearance was bad (B).
各実施例および各比較例における各剥離フィルムをロール状に巻き取ったロールから各剥離フィルムを繰り出す際の帯電量を、春日電機社製「防爆型静電気電位測定器 KSD-0108」を使用して測定した。5kV未満を「A」、5以上10kV未満を「B」、10kV以上を「C」とした。
なお、評価は、条件1:「各剥離フィルムを作製後、23℃50%RH環境下で10日間保管」と条件2:「各剥離フィルムを作製後、40℃環境下で10日間保管」の2つの条件下で行った。 [2.3] Evaluation of unwinding charge amount of release film roll The charge amount when unwinding each release film from a roll obtained by winding each release film in each example and each comparative example in a roll shape was manufactured by Kasuga Electric Co., Ltd. Measurement was performed using an explosion-proof electrostatic potential measuring device KSD-0108. Less than 5 kV was designated as “A”, 5 to less than 10 kV as “B”, and 10 kV or more as “C”.
Evaluation is as follows: Condition 1: “After each release film is prepared and stored for 10 days in an environment of 23 ° C. and 50% RH” and Condition 2: “After each release film is prepared and stored for 10 days in an environment of 40 ° C.” Performed under two conditions.
各実施例および各比較例の両面粘着シートを幅500mmのロール形態とし、第2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2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、以下の評価基準で判定した。
なお、評価は、条件1:「各剥離フィルムを作製後、23℃50%RH環境下で10日間保管」と条件2:「各剥離フィルムを作製後、40℃環境下で10日間保管」の2つの条件下で行った。
A :第2の剥離フィルムへの転着無し
B :第2の剥離フィルムへの転着発生 [2.4] Evaluation of transfer phenomenon called crying separation The double-sided PSA sheet of each Example and each Comparative Example was formed into a roll having a width of 500 mm, the second release film was peeled at a speed of 10 m / min, and the peel angle was 90 °. When 10 m was peeled, the presence or absence of transfer of the pressure-sensitive adhesive to the second peeled film was visually confirmed and judged according to the following evaluation criteria.
Evaluation is as follows: Condition 1: “After each release film is prepared and stored for 10 days in an environment of 23 ° C. and 50% RH” and Condition 2: “After each release film is prepared and stored for 10 days in an environment of 40 ° C.” Performed under two conditions.
A: No transfer to the second release film B: Transfer occurrence to the second release film
各実施例および各比較例で得られた各剥離フィルムを、幅1290mm、長さ6000mのロール状に巻き上げた。この剥離フィルムロールを23℃、50%RHの環境下に10日間保管し、剥離フィルムロールの外観を目視にて観察した。ロール状に巻き上げたときから変化がなかったものをブロッキング無し(A)、半分以下の領域の色目が異なった場合をブロッキング若干有り(B)、過半の領域にわたって色目が異なった場合をブロッキング有り(C)とした。
なお、評価は、条件1:「各剥離フィルムを作製後、23℃50%RH環境下で10日間保管」と条件2:「各剥離フィルムを作製後、40℃環境下で10日間保管」の2つの条件下で行った。 [2.5] Blocking evaluation Each release film obtained in each Example and each Comparative Example was wound into a roll having a width of 1290 mm and a length of 6000 m. This release film roll was stored for 10 days in an environment of 23 ° C. and 50% RH, and the appearance of the release film roll was visually observed. There was no blocking when the roll was rolled up (A), there was a little blocking when the color of less than half the area was different (B), and there was blocking when the color was different over the majority of the area ( C).
Evaluation is as follows: Condition 1: “After each release film is prepared and stored for 10 days in an environment of 23 ° C. and 50% RH” and Condition 2: “After each release film is prepared and stored for 10 days in an environment of 40 ° C.” Performed under two conditions.
各実施例および各比較例で得られた各剥離フィルムを、幅1290mm、長さ6000mのロール状に巻き上げた。
この剥離フィルムロールを下記条件1、2で保管し、剥離フィルムロールの表層部と芯部の剥離力(上述の試験方法)を測定し、芯部/表層部で数値化した。
なお、評価は、条件1:「各剥離フィルムを作製後、23℃50%RH環境下で10日間保管」と条件2:「各剥離フィルムを作製後、40℃環境下で10日間保管」の2つの条件下で行った。
A :1.1よりも小さい
B :1.1以上1.3未満
C :1.3以上
これらの結果を表2に示した。 [2.6] Increasing Peeling Force of Release Film Core Each release film obtained in each Example and each Comparative Example was wound into a roll having a width of 1290 mm and a length of 6000 m.
The release film roll was stored under the following conditions 1 and 2, and the peel force (the test method described above) between the surface layer portion and the core portion of the release film roll was measured, and was quantified by the core portion / surface layer portion.
Evaluation is as follows: Condition 1: “After each release film is prepared and stored for 10 days in an environment of 23 ° C. and 50% RH” and Condition 2: “After each release film is prepared and stored for 10 days in an environment of 40 ° C.” Performed under two conditions.
A: Smaller than 1.1 B: 1.1 or more and less than 1.3 C: 1.3 or more These results are shown in Table 2.
これに対して、比較例では満足な結果が得られなかった。 As is clear from Table 2, the double-sided pressure-sensitive adhesive sheet of the present invention was free from appearance defects because it was prevented from being crushed. Moreover, the double-sided adhesive sheet of this invention was excellent in the peelability of each peeling film, blocking resistance, and antistatic property. Moreover, the double-sided pressure-sensitive adhesive sheet of the present invention prevents the occurrence of a transfer phenomenon called crying separation.
On the other hand, satisfactory results were not obtained in the comparative example.
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 (5)
- 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、
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1の剥離フィルムおよび前記第2の剥離フィルムの前記粘着剤層と接する面とは反対側の面の算術平均粗さRaが5~35nmであり、かつ、その最大突起高さRpが50~400nmであ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 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 arithmetic average roughness Ra of the surface opposite to the surface in contact with the pressure-sensitive adhesive layer of the first release film and the second release film is 5 to 35 nm, and the maximum protrusion height Rp is 50. A double-sided pressure-sensitive adhesive sheet characterized by being -400 nm. - 前記粘着剤層の前記第1の面における、基準面から±0.2μmの範囲外の凹凸の占める割合は、20%以下である請求項1に記載の両面粘着シート。 2. The double-sided pressure-sensitive adhesive sheet according to claim 1, wherein the proportion of the unevenness outside the range of ± 0.2 μm from the reference surface in the first surface of the pressure-sensitive adhesive layer is 20% or less.
- 前記粘着剤層の前記第2の面における、基準面から±0.2μmの範囲外の凹凸の占める割合は、20%以下である請求項1または2に記載の両面粘着シート。 3. The double-sided pressure-sensitive adhesive sheet according to claim 1, wherein a proportion of the unevenness outside the range of ± 0.2 μm from the reference surface in the second surface of the pressure-sensitive adhesive layer is 20% or less.
- 前記粘着剤層を構成する粘着剤は、(メタ)アクリル酸エステル共重合体である請求項1ないし3のいずれか1項に記載の両面粘着シート。 The double-sided pressure-sensitive adhesive sheet according to any one of claims 1 to 3, wherein the pressure-sensitive adhesive constituting the pressure-sensitive adhesive layer is a (meth) acrylic acid ester copolymer.
- 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4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 4, which satisfies a relationship of -Y≥5.
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CN108271381A (en) * | 2016-03-04 | 2018-07-10 | 琳得科株式会社 | Sheet for processing semiconductor |
JP2019059203A (en) * | 2017-09-28 | 2019-04-18 | 東レフィルム加工株式会社 | Release film and laminate using the same |
JP2020132811A (en) * | 2019-02-25 | 2020-08-31 | 日東電工株式会社 | Roll body of laminate sheet |
EP3708627A1 (en) * | 2019-02-25 | 2020-09-16 | Nitto Denko Corporation | Roll of laminate sheet |
JP7271219B2 (en) | 2019-02-25 | 2023-05-11 | 日東電工株式会社 | Laminated sheet roll |
EP3798279A1 (en) * | 2019-09-30 | 2021-03-31 | Nitto Denko Corporation | Laminate sheet |
Also Published As
Publication number | Publication date |
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KR102069612B1 (en) | 2020-01-23 |
TW201437320A (en) | 2014-10-01 |
JP6300788B2 (en) | 2018-03-28 |
TWI579364B (en) | 2017-04-21 |
JPWO2014157445A1 (en) | 2017-02-16 |
KR20150135356A (en) | 2015-12-02 |
CN105008478A (en) | 2015-10-28 |
CN105008478B (en) | 2018-06-05 |
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