WO2021024850A1 - 粘着テープ - Google Patents
粘着テープ Download PDFInfo
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- WO2021024850A1 WO2021024850A1 PCT/JP2020/028837 JP2020028837W WO2021024850A1 WO 2021024850 A1 WO2021024850 A1 WO 2021024850A1 JP 2020028837 W JP2020028837 W JP 2020028837W WO 2021024850 A1 WO2021024850 A1 WO 2021024850A1
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- WIPO (PCT)
- Prior art keywords
- adhesive
- pressure
- adhesive tape
- sensitive adhesive
- adhesive layer
- Prior art date
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Images
Classifications
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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
- C09J201/00—Adhesives based on unspecified macromolecular compounds
- C09J201/02—Adhesives based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups
- C09J201/06—Adhesives based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing oxygen atoms
- C09J201/08—Carboxyl groups
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/18—In situ polymerisation with all reactants being present in the same phase
- B01J13/185—In situ polymerisation with all reactants being present in the same phase in an organic phase
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
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- B32B27/00—Layered products comprising a layer of synthetic resin
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- 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
-
- 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
- C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
- C09J5/08—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers using foamed adhesives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
-
- 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
-
- 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
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- 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
-
- 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
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- 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
-
- 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
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
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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
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- C09J2301/412—Additional features of adhesives in the form of films or foils characterized by the presence of essential components presence of microspheres
-
- 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
- C09J2433/00—Presence of (meth)acrylic polymer
Definitions
- the present invention relates to an adhesive tape. More specifically, it relates to an adhesive tape capable of exhibiting easy peelability in response to a thermal stimulus.
- Adhesive tape As an adhesive tape used for the purpose of temporarily fixing a work piece in the process of manufacturing electronic parts, etc., it is easy to peel off so that it exhibits adhesiveness during temporary fixing and peelability when fixing is not required.
- Adhesive tape is known.
- an adhesive tape having a base material and an adhesive layer, and the adhesive layer containing an adhesive and heat-expandable microspheres typified by a foaming agent is studied. (For example, Patent Document 1).
- This adhesive tape exhibits desired adhesive strength at a relatively low temperature represented by room temperature, while the foaming agent expands when heated to a predetermined temperature (foaming temperature) or higher, and the surface of the adhesive layer Irregularities are generated on the surface, and the adhesive strength is reduced, that is, heat peeling becomes possible.
- foaming temperature a predetermined temperature
- the surface of the adhesive layer Irregularities are generated on the surface, and the adhesive strength is reduced, that is, heat peeling becomes possible.
- the adhesive tape as described above has a problem that the adhesive layer floats from the base material and may be detached in some cases. It is considered that this is because the base material cannot restrain the movement of the pressure-sensitive adhesive layer when the deformation of the pressure-sensitive adhesive layer becomes large. As the temperature rises, the elastic modulus of the pressure-sensitive adhesive layer decreases and the amount of deformation of the pressure-sensitive adhesive layer increases, so that the floating / detaching of the pressure-sensitive adhesive layer during heat peeling becomes a problem.
- the adhesive tape as described above can be used as a temporary fixing tape in a heat treatment step (for example, a heating step, a curing step, etc.).
- the foaming temperature of the temporary fixing adhesive tape in the heating process is set to be higher than the process temperature.
- the heat treatment temperature of the process tends to be high, so that the foaming temperature of the adhesive tape is set high, and as a result, the adhesive layer floats and peels off during heat peeling. It is an easy situation.
- a method of preventing the pressure-sensitive adhesive layer from floating and detaching during heat peeling a method of providing an undercoat layer between the base material and the pressure-sensitive adhesive layer and a method of suppressing deformation of the pressure-sensitive adhesive layer by using a viaduct pressure-sensitive adhesive. Examples thereof include a method and a method for reducing the content of thermally expandable microspheres.
- the effect of the method of providing the undercoat layer between the base material and the pressure-sensitive adhesive layer is limited, and there is selectivity depending on the pressure-sensitive adhesive type, so that it cannot be a fundamental solution.
- the present invention has been made to solve the above-mentioned conventional problems, and an object of the present invention is to provide an adhesive tape in which the adhesive layer is prevented from floating from the base material.
- the adhesive tape of the present invention comprises a base material and a pressure-sensitive adhesive layer arranged on at least one side of the base material, the pressure-sensitive adhesive layer containing a heat-expandable microsphere and an adhesive, and the heat-expandable microsphere.
- the shell is composed of a shell and a volatile substance contained in the shell, and the resin constituting the shell contains a structural unit having a carboxyl group.
- the glass transition temperature (Tg) of the resin constituting the shell is 120 ° C. or higher.
- the content ratio of the structural unit having a carboxyl group is 5 parts by weight to 97 parts by weight with respect to 100 parts by weight of the resin.
- the volatile substance is an organic solvent
- the difference (Tg-bp) between the boiling point (bp) of the organic solvent and the glass transition temperature (Tg) of the resin constituting the shell is 0. It is above °C.
- the pressure-sensitive adhesive is an acrylic pressure-sensitive adhesive.
- the pressure-sensitive adhesive comprises an isocyanate-based crosslinker or an epoxy-based crosslinker.
- the initial adhesive force a when the adhesive surface of the adhesive tape is attached to the polyethylene terephthalate film under an environmental temperature of 25 ° C. is 1.5 N / 20 mm to 20 N / 20 mm.
- the adhesive tape comprises the adhesive layers on both sides of the substrate.
- the pressure-sensitive adhesive layer is provided on one side of the base material, and another pressure-sensitive adhesive layer is provided on the other side of the base material.
- FIGS. 1 (a) and 1 (b) are schematic cross-sectional views of the adhesive tape according to one embodiment of the present invention.
- the adhesive tape 100 includes a base material 10 and an adhesive layer 20 arranged on at least one side of the base material 10.
- FIG. 1 (c) is a schematic cross-sectional view of an adhesive tape according to another embodiment of the present invention.
- the adhesive tape 200 includes a pressure-sensitive adhesive layer 10 and another pressure-sensitive adhesive layer 30 arranged on at least one side of the pressure-sensitive adhesive layer 10.
- the adhesive tape has an elastic layer (described later in item E) capable of imparting elasticity to the adhesive tape and a separator (described later) releasably arranged on the adhesive layer as a layer other than the adhesive layer.
- Item F and the like may be further provided.
- the pressure-sensitive adhesive layer contains heat-expandable microspheres.
- the thermally expandable microspheres can expand at a predetermined temperature.
- the heat-expandable microspheres expand by heating to a predetermined temperature or higher, and the adhesive surface (that is, the surface of the pressure-sensitive adhesive layer) becomes uneven, resulting in increased adhesive strength. Decline or disappear.
- the adhesive tape of the present invention is used as a temporary fixing sheet for a test object or a work piece, for example, during testing or processing of an electronic component (for example, a ceramic capacitor), in a situation where fixing is required. Is exhibited with the required adhesiveness, and then when the adhesive tape is peeled off, the adhesive strength is reduced or eliminated by heating, and good peelability is exhibited.
- the initial adhesive strength a when the adhesive surface of the adhesive tape of the present invention is attached to a polyethylene terephthalate film (for example, 25 ⁇ m in thickness) under an environmental temperature of 25 ° C. is preferably 1.5 N / 20 mm to 20 N / 20 mm. Yes, more preferably 1.5N / 20mm to 18N / 20mm, and even more preferably 2.0N / 20mm to 12N / 20mm. Within such a range, for example, an adhesive tape useful as a temporary fixing sheet used for manufacturing electronic parts can be obtained.
- the initial adhesive strength means the adhesive strength in a state where the heat history of 50 ° C. or higher has not been passed.
- the adhesive strength refers to the adhesive strength measured by a method according to JIS Z 0237: 2000 (bonding conditions: 2 kg roller 1 reciprocation, tensile speed: 300 mm / min, peeling angle 180 °).
- the adhesive strength b when the adhesive surface of the adhesive tape of the present invention, which was heated to 130 ° C. and then cooled to 25 ° C., was attached to a polyethylene terephthalate film (for example, a thickness of 25 ⁇ m) was 0.75 N / 20 mm to 20 N /. It is 20 mm, more preferably 0.75N / 20mm to 18N / 20mm, and even more preferably 1.0N / 20mm to 12N / 20mm.
- the adhesive force b when the adhesive surface of the adhesive tape of the present invention, which was heated to 130 ° C. and then cooled to 25 ° C., was attached to a polyethylene terephthalate film (for example, a thickness of 25 ⁇ m) was higher than the initial adhesive force a. It is preferably 50% or more, more preferably 80% or more, and even more preferably 90% or more.
- a polyethylene terephthalate film for example, a thickness of 25 ⁇ m
- the initial adhesive strength a is preferably 50% or more, more preferably 80% or more, and further preferably 90% or more.
- the thickness of the adhesive tape of the present invention is preferably 30 ⁇ m to 500 ⁇ m, and more preferably 40 ⁇ m to 300 ⁇ m.
- the adhesive layer contains thermally expandable microspheres.
- the pressure-sensitive adhesive layer further comprises a pressure-sensitive adhesive.
- Thermally expandable microspheres are composed of a shell and a volatile substance (typically, an organic solvent) contained in the shell.
- the resin constituting the shell contains a structural unit having a carboxyl group. If the shell is made of a resin having a carboxyl group, the carboxyl group and the base polymer constituting the pressure-sensitive adhesive in the pressure-sensitive adhesive layer interact with each other to impart cohesiveness to the pressure-sensitive adhesive. As a result, in the adhesive tape of the present invention, deformation of the adhesive layer is suppressed, and problems such as the adhesive layer floating or detaching from the base material can be prevented even at a high temperature. By using such an adhesive tape of the present invention, adhesive residue on the adherend at the time of heat peeling can be prevented.
- the structural unit having a carboxyl group can be, for example, a structural unit derived from a carboxy group-containing monomer such as a carboxy group-containing monomer such as acrylic acid, methacrylic acid, itaconic acid, maleic acid, fumaric acid, and citraconic acid. ..
- the resin constituting the shell may further contain a structural unit derived from a radically polymerizable monomer other than the structural unit having a carboxyl group.
- the monomer include nitrile monomers such as acrylonitrile, methacrylonitrile, ⁇ -chloroacrylonitrile, ⁇ -ethoxyacrylonitrile, and fumaronitrile; vinylidene chloride; vinyl acetate; methyl (meth) acrylate and ethyl (meth) acrylate.
- N-butyl (meth) acrylate N-butyl (meth) acrylate, isobutyl (meth) acrylate, t-butyl (meth) acrylate, isobornyl (meth) acrylate, cyclohexyl (meth) acrylate, benzyl (meth) acrylate, ⁇ -carboxyethyl acrylate and the like (meth).
- Acrylate ester styrene monomer such as styrene, ⁇ -methylstyrene, chlorostyrene; amide monomer such as acrylamide, substituted acrylamide, methacrylicamide, substituted methacrylicamide and the like.
- the resin constituting the shell includes a structural unit having a carboxyl group, a structural unit derived from isobornyl acrylate, a structural unit derived from methacrylonitrile, a structural unit derived from acrylonitrile, and methyl (meth). Includes at least one selected from the group consisting of structural units derived from acrylates and structural units derived from vinylidene chloride.
- the resin constituting the shell contains a structural unit having a carboxyl group and a structural unit derived from methacrylnitrile and / or acrylonitrile.
- the content ratio of the structural unit having a carboxyl group is preferably 5 parts by weight to 97 parts by weight, more preferably 5 parts by weight to 90 parts by weight, based on 100 parts by weight of the resin. It is more preferably 5 parts by weight to 85 parts by weight, particularly preferably 5 parts by weight to 80 parts by weight, and most preferably 10 parts by weight to 75 parts by weight. Within such a range, deformation of the pressure-sensitive adhesive layer is suppressed while controlling the productivity and particle size of the heat-expandable microspheres, and the pressure-sensitive adhesive layer floats or desorbs from the base material even at high temperatures.
- the resin forming the shell may be a crosslinked product.
- cross-linking By cross-linking, the exclusion free volume of the polymer can be adjusted, and thereby the diffusivity of the contained volatile substance, the expandability of the shell, and the like can be controlled.
- the crosslinked product may further contain a monomer-derived structural unit having two or more polymerizable double bonds in the molecule.
- the above radically polymerizable monomer and a monomer having two or more polymerizable double bonds in the molecule are used in combination.
- Examples of the monomer having two or more polymerizable double bonds in the molecule include aromatic divinyl compounds such as divinylbenzene and divinylnaphthalene; allyl methacrylate, triacrylic formal, triallyl isocyanate, and ethylene glycol di (meth).
- the glass transition temperature (Tg) of the resin constituting the shell is preferably 120 ° C. or higher, more preferably 125 ° C. or higher, further preferably 130 ° C. or higher, and particularly preferably 135 ° C. or higher.
- Tg glass transition temperature
- the Fox calculation formula is a homopolymer in which each of the glass transition temperature Tg (° C.) of the copolymer and the monomers constituting the copolymer are homopolymerized. ) is a relational expression between the glass transition temperature Tg i (° C.) of.
- unit weight in the following Fox equation Tg (° C.) represents a glass transition temperature of a copolymer, W i is the weight fraction of monomer i, Tg i (° C.) is formed from monomer i Shows the combined glass transition temperature.
- the glass transition temperature of the homopolymer formed from the monomer is methacrylic acid homopolymer: 228 ° C., acrylonitrile homopolymer: 97 ° C., methyl methacrylate homopolymer: 102 ° C., methacryloylnitrile homopolymer: 120 ° C. ° C., Vinylidene Chloride Monopolymer: 75 ° C., Isobornyl Acrylate Monopolymer: 97 ° C.
- the thickness of the shell is preferably 1 ⁇ m to 15 ⁇ m, more preferably 1 ⁇ m to 7 ⁇ m, and further preferably 1 ⁇ m to 5 ⁇ m.
- the volatile substance contained in the shell is typically an organic solvent.
- the organic solvent include linear aliphatic hydrocarbons having 3 to 8 carbon atoms and their fluorocarbons, branched aliphatic hydrocarbons having 3 to 8 carbon atoms and their fluorocarbons, and 3 to 8 carbon atoms. Linear alicyclic hydrocarbons and fluorides thereof, ether compounds having 2 to 8 carbon atoms, or compounds in which a part of the hydrogen atom of the hydrocarbon group is replaced by a fluorine atom, etc. Can be mentioned.
- the organic solvents are propane, cyclopropane, butane, cyclobutane, isopentane, pentane, cyclopentane, neopentane, isopentane, hexane, cyclohexane, 2-methylpentane, 2,2-dimethylbutane, heptane, cyclo.
- Hydrocarbons composed only of hydrogen atoms and carbon atoms such as heptane, octane, cyclooctane, methylheptanes, trimethylpentanes; C 3 F 7 OCH 3 , C 4 F 9 OCH 3 , C 4 F 9 OC 2 hydrofluoroethers such like H 5 is used.
- the organic solvent has an advantage that it has a low affinity with the resin and / or the pressure-sensitive adhesive forming the shell, it is difficult to dissolve the shell and / or the pressure-sensitive adhesive, and it is difficult to change physical properties such as thermal properties.
- hydrocarbons composed only of hydrogen atoms and carbon atoms are preferable from the viewpoint of industrial use.
- branched hydrocarbons for example, isobutane, isopentane, etc.
- hydrocarbons composed only of hydrogen atoms and carbon atoms.
- Branched hydrocarbons are hard to be charged, and if this solvent is used, accidents such as ignition due to charging can be prevented.
- the boiling point of the organic solvent is preferably ⁇ 50 ° C. to 100 ° C., more preferably ⁇ 20 ° C. to 100 ° C. Within such a range, it is possible to obtain thermally expandable microspheres in which the shell can expand satisfactorily without breaking. If the boiling point of the organic solvent is too low, the operation for suppressing volatilization during the production of thermal expansion microspheres may become complicated.
- the difference (Tg-bp) between the boiling point (bp) of the organic solvent and the glass transition temperature (Tg) of the resin constituting the shell is preferably 0 ° C. or higher, more preferably 0 ° C. to 200 ° C. Yes, more preferably 50 ° C to 150 ° C.
- Tg-bp glass transition temperature
- the shell is destroyed by the pressure generated when the organic solvent is heated, and the adhesive is scattered. And may hinder the effect.
- the "boiling point (bp) of the organic solvent” is calculated by (sum of boiling points of each organic solvent) / (number of kinds of organic solvents). The value.
- the content ratio of the organic solvent is preferably 5% by weight to 35% by weight, more preferably 10% by weight to 30% by weight, based on the weight of the heat-expandable microspheres before heating. Within such a range, it is possible to obtain thermal expandability that allows stable expansion. If the content ratio is less than 5% by weight, the expansion during heating becomes insufficient, it becomes difficult to form the adhesive unevenness, heat peeling failure occurs, and adhesive residue may occur. If the content ratio exceeds 35% by weight, the expansion becomes excessive during heating, and the adhesive layer may be peeled off from the base material.
- the average particle size (number standard) of the heat-expandable microspheres before foaming the heat-expandable microspheres under an ambient temperature of 25 ° C. is preferably 5 ⁇ m to 30 ⁇ m, more preferably 5 ⁇ m to 28 ⁇ m. Yes, more preferably 10 ⁇ m to 25 ⁇ m. Within such a range, thermally expandable microspheres having high dispersibility in the pressure-sensitive adhesive layer can be obtained.
- the pressure-sensitive adhesive layer containing the heat-expandable microspheres in a highly dispersible state has high uniformity of unevenness generated by heating and can exhibit excellent peelability.
- the average particle size of the heat-expandable microspheres can be controlled, for example, by the conditions for polymerizing the heat-expandable microspheres (details will be described later).
- the average particle size can be measured by the particle size distribution measuring method in the laser scattering method. More specifically, the average particle size is determined by dispersing the heat-expandable microspheres to be used in a predetermined solvent (for example, water) and then using a particle size distribution measuring device (for example, product name "SALD-2000J" manufactured by Shimadzu Corporation). ) Can be used for measurement.
- the foaming temperature of the heat-expandable microspheres is preferably 150 ° C. to 280 ° C., more preferably 155 ° C. to 260 ° C.
- the foaming temperature of the heat-expandable microspheres may correspond to a temperature at which the adhesive strength of the adhesive tape is 1.0 N / 20 mm or less and 50% or less of the initial adhesive strength.
- the content ratio of the heat-expandable microspheres is represented by the area ratio of the heat-expandable microspheres measured from the cross section.
- the ratio of the cross-sectional area B of the heat-expandable microspheres is the cross-sectional area A of the pressure-sensitive adhesive layer.
- it is preferably 3% to 75%, and more preferably 3.5% to 70%.
- the ratio of the cross-sectional area B is less than 3%, even if the heat-expanded microspheres are expanded by heating, the unevenness generated on the surface of the adhesive may be insufficient and the desired peelability may not be obtained.
- the ratio of the cross-sectional area B exceeds 75%, the volume change of the pressure-sensitive adhesive layer becomes too large, which may cause floating / peeling between the base material and the pressure-sensitive adhesive layer, and adhesion in the pressure-sensitive adhesive layer.
- the agent content is low, and the desired adhesive strength may not be obtained.
- the ratio of the cross-sectional area B of the heat-expandable microspheres is determined by, for example, observing the cross section of the pressure-sensitive adhesive layer with an electron microscope (for example, manufactured by Hitachi Technologies America, trade name "S-3400N low vacuum scanning electron microscope").
- the obtained image can be appropriately processed and obtained.
- the image is output on paper, and the paper weight a of the pressure-sensitive adhesive layer portion (that is, the entire pressure-sensitive adhesive layer containing the heat-expandable microspheres) and the weight b of the paper obtained by cutting out only the heat-expandable microsphere portion. Therefore, it can be obtained by the formula of b / a ⁇ 100.
- the content ratio of the thermally expandable microspheres is preferably 5 parts by weight to 80 parts by weight, more preferably 5 parts by weight to 60 parts by weight, and further preferably 10 parts by weight with respect to 100 parts by weight of the pressure-sensitive adhesive layer. There are parts to 50 parts by weight. Within such a range, it is possible to realize the ratio of the cross-sectional area B of the heat-expandable microspheres as described above.
- the cross-sectional area B of the heat-expandable microsphere can be set in a preferable range.
- the content ratio of the heat-expandable microspheres is calculated by the following formula.
- the heat-expandable microspheres can be produced by any suitable method.
- the heat-expandable microspheres are obtained by a suspension polymerization method.
- Suspension polymerization is usually carried out by dispersing a monomer (shell-forming material) and an organic solvent in an aqueous dispersion medium containing a dispersant and polymerizing the monomer in the presence of the organic solvent.
- a dispersion stabilizer that stabilizes the dispersion may be used.
- the dispersion stabilizer in the aqueous dispersion medium include inorganic fine particles such as silica, magnesium hydroxide, calcium phosphate, and aluminum hydroxide.
- dispersion stabilizing aid for example, a condensation product of diethanolamine and an aliphatic dicarboxylic acid, polyvinylpyrrolidone, methyl cellulose, polyethylene oxide, polyvinyl alcohol, various emulsifiers and the like may be used.
- the characteristics of the thermally expandable microspheres such as the particle size and the content of the organic solvent can be controlled by the polymerization conditions of the suspension polymerization, the type and amount of the mixed components, and the like. For example, heat-expandable microspheres having a large particle size can be obtained by reducing the amount of the dispersant added, slowing down the stirring speed during polymerization, and the like. Further, by increasing the amount of the monomer compounded or slowing down the stirring speed at the time of polymerization, it is possible to obtain thermally expandable microspheres having a thick shell.
- any suitable pressure-sensitive adhesive can be used as long as the effects of the present invention can be obtained.
- the above-mentioned adhesive include acrylic adhesive, silicone adhesive, vinyl alkyl ether adhesive, polyester adhesive, polyamide adhesive, urethane adhesive, fluorine adhesive, and styrene-diene block.
- examples thereof include a polymerization system pressure-sensitive adhesive and an active energy ray-curable pressure-sensitive adhesive.
- an acrylic pressure-sensitive adhesive, a rubber-based pressure-sensitive adhesive or a silicone-based pressure-sensitive adhesive is preferable, and an acrylic-based pressure-sensitive adhesive is more preferable.
- the gel fraction of the pressure-sensitive adhesive is preferably 20% by weight to 100% by weight, more preferably 30% by weight to 99% by weight, and further preferably 50% by weight to 99% by weight.
- the gel fraction is less than 20% by weight, even if the heat-expanded microspheres expand and the surface of the pressure-sensitive adhesive layer becomes uneven, the pressure-sensitive adhesive layer may flow and the unevenness may disappear in a short time.
- the gel fraction exceeds 99% by weight, the thermal expansion microspheres explode and thermally expand even if the thermal expansion of the thermally expandable microspheres is hindered and sufficient unevenness is not generated, or even if unevenness is generated.
- the gel fraction of the pressure-sensitive adhesive can be controlled by adjusting the composition of the base polymer constituting the pressure-sensitive adhesive, the type and content of the cross-linking agent added to the pressure-sensitive adhesive, the type and content of the pressure-sensitive adhesive, and the like. ..
- the method for measuring the gel fraction is as follows. Approximately 0.1 g of the adhesive is sampled and weighed (sample weight), the sample is wrapped in a mesh sheet (trade name "NTF-1122", manufactured by Nitto Denko KK), and then in approximately 50 ml of toluene. Was soaked in room temperature for 1 week.
- the base polymer contained in the pressure-sensitive adhesive preferably has an OH group or a COOH group.
- the effect of the present invention becomes more remarkable.
- the base polymer if used, the gel fraction can be adjusted by using a cross-linking agent.
- the cohesiveness of the base polymer due to intermolecular force such as hydrogen bonding can be adjusted by the amount of OH groups or COOH groups that do not react with the cross-linking agent. Thereby, it is possible to control the uneven shape of the pressure-sensitive adhesive surface caused by the expansion of the heat-expandable microspheres.
- the acid value of the base polymer is preferably 0 to 100, more preferably 10 to 80, and even more preferably 20 to 50.
- the acid value of the polymer in the pressure-sensitive adhesive layer can be measured by extracting the solvent-soluble component in the pressure-sensitive adhesive layer. Specifically, the solvent-soluble component can be extracted by the following method. (I) The pressure-sensitive adhesive layer is put into a solvent to prepare a solution sample in which the solvent-soluble component in the pressure-sensitive adhesive layer is dissolved in the above-mentioned solvent.
- chloroform CHCl 3
- methylene chloride CH 2 Cl 2
- tetrahydrofuran THF
- acetone dimethyl sulfoxide
- DMSO dimethyl sulfoxide
- DMF N-dimethylformamide
- methanol in consideration of polarity and the like.
- Ethanol, toluene, water and the like, or a mixed solvent containing two or more kinds in any ratio can be used.
- about 30 mL of the solvent is added to about 0.2 g of the pressure-sensitive adhesive layer, and the mixture is stirred in a temperature range from room temperature to about the boiling point of the solvent used for about 30 minutes to 12 hours.
- the solution sample may be prepared by repeating the operation of sorting once or a plurality of times.
- the solvent can be removed from the above solution sample by a method such as evaporation, and the solvent-soluble polymer can be taken out.
- the solvent-soluble polymer may contain a solvent-soluble component that cannot be measured, such as a low molecular weight component of the unreacted cross-linking agent.
- the acrylic pressure-sensitive adhesive includes, for example, an acrylic pressure-sensitive adhesive based on an acrylic polymer (homopolymer or copolymer) using one or more (meth) acrylic acid alkyl esters as a monomer component. And so on.
- Specific examples of the (meth) acrylic acid alkyl ester include methyl (meth) acrylic acid, ethyl (meth) acrylic acid, propyl (meth) acrylic acid, isopropyl (meth) acrylic acid, butyl (meth) acrylic acid, and (meth).
- the acrylic polymer contains a unit corresponding to another monomer copolymerizable with the (meth) acrylic acid alkyl ester, if necessary, for the purpose of modifying cohesive force, heat resistance, crosslinkability, etc. You may.
- monomers include carboxyl group-containing monomers such as acrylic acid, methacrylic acid, carboxyethyl acrylate, carboxypentyl acrylate, itaconic acid, maleic acid, fumaric acid, and crotonic acid; acids such as maleic anhydride and icotanic anhydride.
- Anhydrous monomer hydroxyethyl (meth) acrylate, hydroxypropyl (meth) acrylate, hydroxybutyl (meth) acrylate, hydroxyhexyl (meth) acrylate, hydroxyoctyl (meth) acrylate, hydroxy (meth) acrylate Hydroxyl group-containing monomers such as decyl, hydroxylauryl (meth) acrylate, (4-hydroxymethylcyclohexyl) methylmethacrylate; styrene sulfonic acid, allyl sulfonic acid, 2- (meth) acrylamide-2-methylpropane sulfonic acid, (meth).
- Sulfonic acid group-containing monomers such as acrylamide propanesulfonic acid, sulfopropyl (meth) acrylate, (meth) acryloyloxynaphthalene sulfonic acid; (meth) acrylamide, N, N-dimethyl (meth) acrylamide, N-butyl (meth) (N-substituted) amide-based monomers such as acrylamide, N-methylol (meth) acrylamide, N-methylolpropane (meth) acrylamide; aminoethyl (meth) acrylate, N, N-dimethylaminoethyl (meth) acrylate, (Meta) Aminoalkyl Acrylic Acid Monomer such as t-butylaminoethyl (meth) Acrylic Acid; (Meta) Arkoxyalkyl Acrylic Acid Monomer such as methoxyethyl (meth) Acrylic Acid, ethoxyethyl (Meta)
- Acrylic acid ester-based monomers having the above; hexanediol di (meth) acrylate, (poly) ethylene glycol di (meth) acrylate, (poly) propylene glycol di (meth) acrylate, neopentyl glycol di (meth) acrylate, pentaerythritol Polyfunctional monomers such as di (meth) acrylate, trimethylolpropantri (meth) acrylate, pentaerythritol tri (meth) acrylate, dipentaerythritol hexa (meth) acrylate, epoxy acrylate, polyester acrylate, urethane acrylate; isoprene, butadiene, Olefin-based monomers such as isobutylene; vinyl ether-based monomers such as vinyl ether and the like can be mentioned. These monomers may be used alone or in combination of two or more.
- silicone-based pressure-sensitive adhesive any suitable pressure-sensitive adhesive can be used as long as the effects of the present invention can be obtained.
- a silicone-based pressure-sensitive adhesive for example, a silicone-based pressure-sensitive adhesive containing a silicone rubber containing an organopolysiloxane or a silicone resin as a base polymer is preferably used.
- a base polymer constituting the silicone-based pressure-sensitive adhesive a base polymer obtained by cross-linking the above-mentioned silicone rubber or silicone resin may be used.
- sicone rubber means a polymer (for example, viscosity 1000Pa ⁇ s) in which diorganosiloxane (D unit) as a main component is linearly connected, and is "silicone resin”.
- D unit diorganosiloxane
- Sicone resin means a polymer composed of triorganosylhemioxane (M unit) and silicate (Q unit) as main components
- silicone rubber examples include organopolysiloxane containing dimethylsiloxane as a constituent unit.
- a functional group for example, a vinyl group
- the weight average molecular weight of the organopolysiloxane is preferably 100,000 to 1,000,000, more preferably 150,000 to 500,000.
- the weight average molecular weight can be measured by GPC (solvent: THF).
- silicone resin examples include an organopolysiloxane containing at least one structural unit selected from R 3 SiO 1/2 structural unit, SiO 2 structural unit, RSiO 3/2 structural unit and R 2 SiO structural unit. (R is a monovalent hydrocarbon group or hydroxyl group).
- the above silicone rubber and silicone resin can be used in combination.
- the weight ratio (rubber: resin) of the silicone rubber to the silicone resin in the silicone adhesive is preferably 100: 0 to 100: 220, more preferably 100: 0 to 100: 180, and further preferably 100: It is 10 to 100: 100.
- the silicone rubber and the silicone resin may be contained in the silicone-based pressure-sensitive adhesive as a mere mixture, or may be contained in the silicone-based pressure-sensitive adhesive in the form of a partial condensation of the silicone rubber and the silicone resin.
- the rubber: resin ratio can also be determined from the ratio of the Q unit (resin) and the D unit (rubber) obtained by measuring the composition of the silicone pressure-sensitive adhesive by 29 Si-NMR.
- any suitable pressure-sensitive adhesive can be used as long as the effects of the present invention can be obtained.
- the rubber-based pressure-sensitive adhesive include natural rubber; polyisoprene rubber, butadiene rubber, styrene-butadiene (SB) rubber, styrene-isoprene (SI) rubber, styrene-isoprene-styrene block copolymer (SIS) rubber, and styrene.
- SBS styrene-ethylene-butylene-styrene block copolymer
- SEBS styrene-ethylene-butylene-styrene block copolymer
- SEPS styrene-ethylene-propylene-styrene block copolymer
- SEP rubber-based pressure-sensitive adhesive based on block copolymer
- recycled rubber butyl rubber, polyisobutylene rubber, or synthetic rubber such as a modified product thereof; is preferably used.
- the pressure-sensitive adhesive may optionally contain any suitable additive.
- suitable additive include a cross-linking agent, a tackifier, a plasticizer, a pigment, a dye, a filler, an antioxidant, a conductive material, an antistatic agent, an ultraviolet absorber, a light stabilizer, a peeling conditioner, and a softening agent. , Surfactants, flame retardants, antioxidants and the like.
- any suitable tackifier is used.
- a tackifier resin is used.
- Specific examples of the tackifier resin include rosin-based tackifier resins (eg, unmodified rosin, modified rosin, rosinphenol-based resins, rosin ester-based resins, etc.) and terpene-based tackifier resins (eg, terpene-based resins, terpene phenols).
- Hydrocarbon-based resin for example, aliphatic hydrocarbon resin, aliphatic cyclic hydrocarbon resin, aromatic-based Hydrocarbon resins (for example, styrene resins, xylene resins, etc.), aliphatic / aromatic petroleum resins, aliphatic / alicyclic petroleum resins, hydrogenated hydrocarbon resins, kumaron resins, kumaron inden resins , Etc.), phenol-based tackifier resins (eg, alkylphenol-based resins, xylene formaldehyde-based resins, resoles, novolak, etc.), ketone-based tackifier resins, polyamide-based tackifier resins, epoxy-based tackifier resins, elastomer-based tackifier resins
- hydrocarbon-based tackifier resin for example, aliphatic hydrocarbon resin, aliphatic cyclic hydrocarbon resin, aromatic-based Hydrocarbon resins (for example, styren
- the amount of the tackifier added is preferably 5 parts by weight to 100 parts by weight, more preferably 5 parts by weight to 50 parts by weight, based on 100 parts by weight of the base polymer.
- cross-linking agent examples include isocyanate-based cross-linking agents, epoxy-based cross-linking agents, melamine-based cross-linking agents, peroxide-based cross-linking agents, urea-based cross-linking agents, metal alkoxide-based cross-linking agents, metal chelate-based cross-linking agents, and metals.
- examples thereof include salt-based cross-linking agents, carbodiimide-based cross-linking agents, oxazoline-based cross-linking agents, aziridine-based cross-linking agents, and amine-based cross-linking agents. Of these, an isocyanate-based cross-linking agent or an epoxy-based cross-linking agent is preferable.
- isocyanate-based cross-linking agent examples include lower aliphatic polyisocyanates such as butylene diisocyanate and hexamethylene diisocyanate; alicyclic isocyanates such as cyclopentylene diisocyanate, cyclohexylene diisocyanate, and isophorone diisocyanate; 2,4- Aromatic isocyanates such as tolylene diisocyanate, 4,4'-diphenylmethane diisocyanate, xylylene diisocyanate; trimethylolpropane / tolylene diisocyanate trimer adduct (manufactured by Nippon Polyurethane Industry Co., Ltd., trade name "Coronate L”), tri Methylolpropane / hexamethylene diisocyanate trimeric adduct (manufactured by Nippon Polyurethane Industry Co., Ltd., trade name "Coronate HL”), is
- the content of the isocyanate-based cross-linking agent can be set to an arbitrary appropriate amount according to the desired adhesive strength, elasticity of the pressure-sensitive adhesive layer, etc., and is typically 0. It is 1 part by weight to 20 parts by weight, more preferably 0.5 part by weight to 10 parts by weight.
- epoxy-based cross-linking agent examples include N, N, N', N'-tetraglycidyl-m-xylene diamine, diglycidyl aniline, and 1,3-bis (N, N-glycidyl aminomethyl) cyclohexane (Mitsubishi Gas).
- the content of the epoxy-based cross-linking agent can be set to an arbitrary appropriate amount according to the desired adhesive strength, elasticity of the pressure-sensitive adhesive layer, etc., and is typically 0. It is 01 parts by weight to 10 parts by weight, more preferably 0.03 parts by weight to 5 parts by weight.
- any suitable plasticizer can be used.
- the plasticizer include trimet acid ester-based plasticizers, pyromellitic acid ester-based plasticizers, polyester-based plasticizers, adipic acid-based plasticizers, and the like.
- a trimellitic acid ester-based plasticizer for example, trimellitic acid tri (n-octyl), trimellitic acid tri (2-ethylhexyl), etc.
- a pyrimellitic acid ester-based plasticizer for example, pyromerit
- the plasticizer may be used alone or in combination of two or more.
- the content of the plasticizer is preferably 1 part by weight to 20 parts by weight, and more preferably 1 part by weight to 5 parts by weight with respect to 100 parts by weight of the base polymer.
- the elastic modulus of the adhesive layer at 23 ° C. by the nanoindentation method is preferably 0.1 MPa to 500 MPa, more preferably 0.5 MPa to 400 MPa.
- the elastic modulus by the nanoindentation method is measured at a location about 3 ⁇ m inside the surface of the adhesive layer and where there are no thermally expanded microspheres (a location 1 ⁇ m or more away from the shell surface of the thermally expanded microspheres).
- the load applied to the indenter and the pressing depth when the indenter is pushed into the pressure-sensitive adhesive layer are continuously measured during loading and unloading, and can be obtained from the obtained load-pushing depth curve.
- the elastic modulus by the nanoindentation method means the elastic modulus measured as described above under the measurement conditions of loading / unloading speed: 1000 nm / s and pushing depth: 800 nm.
- the thickness of the pressure-sensitive adhesive layer is preferably 5 ⁇ m to 300 ⁇ m, more preferably 5 ⁇ m to 250 ⁇ m, further preferably 5 ⁇ m to 100 ⁇ m, and particularly preferably 5 ⁇ m to 60 ⁇ m.
- the pressure-sensitive adhesive layer may further contain any suitable other ingredients as long as the effects of the present invention are obtained.
- examples of other components include beads.
- examples of the beads include glass beads, resin beads and the like. By adding such beads to the pressure-sensitive adhesive layer, the elastic modulus of the pressure-sensitive adhesive layer can be improved, and a pressure-sensitive adhesive tape capable of processing a workpiece with higher accuracy can be obtained.
- the average particle size of the beads is, for example, 0.01 ⁇ m to 50 ⁇ m.
- the amount of beads added is, for example, 10 parts by weight to 200 parts by weight, preferably 20 parts by weight to 100 parts by weight, based on 100 parts by weight of the pressure-sensitive adhesive layer.
- Base material examples include resin sheets, non-woven fabrics, paper, metal foils, woven fabrics, rubber sheets, foam sheets, and laminates thereof (particularly, laminates including resin sheets).
- the resin constituting the resin sheet include polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polybutylene terephthalate (PBT), polyethylene (PE), polypropylene (PP), ethylene-propylene copolymer, and ethylene-.
- EVA Vinyl acetate copolymer
- nylon polyamide
- aramid total aromatic polyamide
- PI polyimide
- PVC polyvinyl chloride
- PPS polyphenylene terephide
- fluororesin polyetheretherketone
- PEEK polyetheretherketone
- Etc. Vinyl acetate copolymer
- the non-woven fabric include non-woven fabrics made of natural fibers having heat resistance such as non-woven fabrics containing Manila hemp; synthetic resin non-woven fabrics such as polypropylene resin non-woven fabrics, polyethylene resin non-woven fabrics and ester resin non-woven fabrics.
- the metal foil include copper foil, stainless steel foil, aluminum foil and the like.
- paper include Japanese paper
- the thickness of the base material can be set to an arbitrary appropriate thickness according to the desired strength or flexibility, the purpose of use, and the like.
- the thickness of the base material is preferably 1000 ⁇ m or less, more preferably 1 ⁇ m to 1000 ⁇ m, further preferably 1 ⁇ m to 500 ⁇ m, particularly preferably 3 ⁇ m to 300 ⁇ m, and most preferably 5 ⁇ m to 250 ⁇ m.
- the base material may be surface-treated.
- the surface treatment include corona treatment, chromic acid treatment, ozone exposure, flame exposure, high-voltage impact exposure, ionizing radiation treatment, coating treatment with an undercoat agent, and the like.
- the organic coating material examples include the materials described in Plastic Hard Coat Material II (CMC Publishing, (2004)).
- Urethane-based polymers are preferably used, more preferably polyacrylic urethane, polyester urethane, or precursors thereof. This is because it is easy to apply and apply to the base material, and various types can be industrially selected and obtained at low cost.
- the urethane-based polymer is, for example, a polymer composed of a reaction mixture of an isocyanato monomer and an alcoholic hydroxyl group-containing monomer (for example, a hydroxyl group-containing acrylic compound or a hydroxyl group-containing ester compound).
- the organic coating material may contain a chain extender such as polyamine, an antioxidant, an oxidation stabilizer and the like as optional additives.
- the thickness of the organic coating layer is not particularly limited, but for example, about 0.1 ⁇ m to 10 ⁇ m is suitable, about 0.1 ⁇ m to 5 ⁇ m is preferable, and about 0.5 ⁇ m to 5 ⁇ m is more preferable.
- any suitable adhesive layer can be formed.
- the pressure-sensitive adhesive forming another pressure-sensitive adhesive layer include rubber-based pressure-sensitive adhesives, acrylic-based pressure-sensitive adhesives, vinyl alkyl ether-based pressure-sensitive adhesives, silicone-based pressure-sensitive adhesives, polyester-based pressure-sensitive adhesives, polyamide-based pressure-sensitive adhesives, and urethane-based pressure-sensitive adhesives. Examples thereof include agents, fluorine-based pressure-sensitive adhesives, and styrene-diene block copolymer-based pressure-sensitive adhesives.
- the pressure-sensitive adhesive may contain, for example, known or commonly used additives such as plasticizers, fillers, surfactants, anti-aging agents, and tackifiers.
- the thickness of the other pressure-sensitive adhesive layer is preferably 300 ⁇ m or less, more preferably 1 ⁇ m to 300 ⁇ m, and further preferably 5 ⁇ m to 100 ⁇ m.
- the adhesive tape of the present invention may further include an elastic layer.
- the elastic layer can be placed on one side of the pressure-sensitive adhesive layer. If the adhesive tape comprises a substrate, the elastic layer may be placed between the adhesive layer and the substrate.
- the followability to the adherend is improved. Further, when the adhesive tape provided with the elastic layer is heated at the time of peeling, the deformation (expansion) of the adhesive layer in the surface direction is restrained, and the deformation in the thickness direction is prioritized. As a result, the peelability is improved.
- the elastic layer contains a base polymer, and as the base polymer, a polymer exemplified as a base polymer constituting the pressure-sensitive adhesive layer can be used.
- the elastic layer may include natural rubber, synthetic rubber, synthetic resin, or the like.
- the synthetic rubber and synthetic resin include nitrile-based, diene-based, and acrylic-based synthetic rubber; polyolefin-based, polyester-based thermoplastic elastomers; ethylene-vinyl acetate copolymer; polyurethane; polybutadiene; and soft polyvinyl chloride.
- the base polymer constituting the elastic layer may be the same as or different from the base polymer forming the pressure-sensitive adhesive layer.
- the elastic layer may be a foamed film formed from the base polymer.
- the foamed film can be obtained by any suitable method.
- the elastic layer and the pressure-sensitive adhesive layer can be distinguished by the difference in the base polymer and / or the presence or absence of the foaming agent (the elastic layer does not contain the foaming agent). More specifically, when the interface between the elastic layer and the pressure-sensitive adhesive layer can be identified by cross-sectional observation, such as when the elastic layer and the pressure-sensitive adhesive layer are formed of different base polymers, the elastic layer and the pressure-sensitive adhesive layer are used. The boundary of is defined by the interface. When the interface between the elastic layer and the pressure-sensitive adhesive layer cannot be identified by cross-section observation, the region where the foaming agent is observed by cross-section observation is the pressure-sensitive adhesive layer.
- the elastic layer may contain any suitable additive, if desired.
- the additive include a cross-linking agent, a vulcanizing agent, a tackifier resin, a plasticizer, a softener, a filler, an anti-aging agent and the like.
- a hard resin such as polyvinyl chloride
- the thickness of the elastic layer is preferably 3 ⁇ m to 200 ⁇ m, more preferably 5 ⁇ m to 100 ⁇ m. Within such a range, the above-mentioned function of the elastic layer can be fully exerted.
- the tensile elastic modulus of the elastic layer at 25 ° C. is preferably 0.01 MPa to 500 MPa, more preferably 0.05 MPa to 500 MPa, and further preferably 0.1 MPa to 500 MPa. Within such a range, the above-mentioned function of the elastic layer can be fully exerted.
- the tensile elastic modulus can be measured according to JIS K 7161: 2008.
- the adhesive tape of the present invention may further include a separator, if necessary. At least one surface of the separator is a peeling surface, and the separator may be provided to protect the pressure-sensitive adhesive layer.
- the separator can be composed of any suitable material.
- the adhesive tape of the present invention can be produced by any suitable method.
- the pressure-sensitive adhesive tape of the present invention is, for example, a method of directly applying a pressure-sensitive adhesive layer-forming composition containing a pressure-sensitive adhesive and heat-expandable microspheres onto a substrate, or forming a pressure-sensitive adhesive layer on any suitable substrate. Examples thereof include a method of transferring the coating layer formed by coating the composition to a substrate.
- the composition for forming the pressure-sensitive adhesive layer may contain any suitable solvent.
- the heat-expandable microspheres are sprinkled on the pressure-sensitive adhesive coating layer, and then the heat-expandable microspheres are formed by using a laminator or the like. It may be embedded in the coating layer to form an adhesive layer containing thermally expandable microspheres.
- the content of the heat-expandable microspheres in the pressure-sensitive adhesive layer-forming composition is preferably 5% by weight to 95% by weight, more preferably 10% by weight, based on the solid content weight of the pressure-sensitive adhesive layer-forming composition. It is from% by weight to 70% by weight, more preferably 10% by weight to 50% by weight.
- the elastic layer can be formed by, for example, applying a composition for forming the elastic layer on a base material or a pressure-sensitive adhesive layer.
- each layer can be formed by applying and then drying.
- the coating method include a coating method using a multi-coater, a die coater, a gravure coater, an applicator, and the like.
- the drying method include natural drying and heat drying. The heating temperature for heat-drying can be set to any suitable temperature depending on the characteristics of the substance to be dried.
- the adhesive tape of the present invention can be suitably used as a sheet for temporarily fixing an electronic component material when manufacturing and evaluating an electronic component.
- the adhesive tape of the present invention can be used as an adhesive tape for temporarily fixing an object to be tested in a thermal shock test.
- the adhesive tape of the present invention can be used as an adhesive tape for temporarily fixing the workpiece in the resin sealing step at the time of manufacturing a substrateless semiconductor package.
- the semiconductor package refers to a form of a semiconductor component package that enables surface mounting of a single high-integration semiconductor on a printed circuit board.
- WLCSP wafer level chip size package
- FOWLP fan-out wafer level package
- FIWLP fan-in wafer level package
- the adhesive tape needs to have a function of holding the bare chip in a predetermined position without moving against them. Is.
- a function that can be easily peeled off from the bare chip is required after the sealing process. That is, the adhesive tape disclosed in the present application can be suitably used for manufacturing the above-mentioned package, and can exhibit its function in particular in the resin sealing step.
- the adhesive tape of the present invention can be used as an adhesive tape for temporarily fixing the workpiece in the patterning step of the wiring circuit. In yet another embodiment, the adhesive tape of the present invention can be used as an adhesive tape for temporarily fixing the workpiece in the electrode coating / drying step of the electronic component. In yet another embodiment, the adhesive tape of the present invention is used as an adhesive tape for temporarily fixing an adherend in order to consistently process an electronic component fragmentation step and a heat treatment step on the same tape. Can be. As described above, the adhesive tape of the present invention can be suitably used for a process involving heating.
- the adhesive tape with the adherend was set in a tensile tester with a constant temperature bath (manufactured by Shimadzu Corporation, trade name "Shimadzu Autograph AG-120 kN”) set at 25 ° C., and left for 30 minutes.
- a load when the adherend was peeled off from the adhesive tape under the conditions of peeling angle: 180 ° and tensile speed: 300 mm / min was measured, and the maximum load at that time (excluding the peak top at the initial stage of measurement). The maximum value of the load) was obtained, and this maximum load was defined as the adhesive force (N / 20 mm).
- the feed rate of the dicing blade was 70 mm / S, and the rotation speed of the dicing blade was 50,000 / s.
- the ratio (chip skipping rate) (%) of the number of chips peeled off from the adhesive tape (chip skipping) during the cutting process was determined and used as the evaluation of the cutting processability. If all the chips are attached to the adhesive tape and are not peeled off, the chip skipping rate is 0% (that is, the chip skipping rate is 0%).
- the number of dicing chips was A 0
- the number of chips skipped was A
- Chip skipping rate the rate at which the chips are peeled off
- EP-K-300 a program temperature controller (hot air dryer) (manufactured by Isuzu Motors Ltd., "EP-K-300") was used to heat-treat at a foaming temperature for 5 minutes. After the heat treatment, turn the adhesive tape upside down in the air (so that the chips are on the bottom), peel off the chips from the adhesive tape by free fall, and the percentage of chips remaining on the sheet (chip residue). ) (%) Is calculated. If all the chips are peeled off and do not remain on the adhesive tape, the remaining chips are 0%.
- the fact that the amount of chips remaining after processing after the heat treatment is small means that the heat peelability is good.
- the number of chips before peeling was B 0
- the number of chips remaining on the sheet after the heat peeling treatment was B
- thermally expandable microsphere A 150 g of sodium chloride, 70 g of colloidal silica (manufactured by Nissan Chemical Co., Ltd., trade name "Snowtex") containing 20% by weight of silica active ingredient, 1 g of polyvinylpyrrolidone, and the like. After adding 0.5 g of a condensate of diethanolamine and adipic acid to 600 g of distilled water, the pH of the obtained mixture was adjusted to 2.8 to 3.2 to obtain an aqueous solution. To the above aqueous solution, 125 g of acrylonitrile and 120 g of methacrylic acid were added as an oil-based additive used as a material for the shell.
- reaction solution 1 g of ethylene glycol dimethacrylate as a cross-linking agent was added to obtain a reaction solution.
- the above reaction solution is added to a pressure-resistant reaction vessel with a homomixer (manufactured by Tokushu Kagaku Kogyo Co., Ltd., trade name "TK homomixer"), and isopentane (boiling point: 27.7) is added as an organic solvent intended to be encapsulated in the shell.
- 20 g of (° C.), 55 g of isopentane (boiling point: 99 ° C.), and 5 g of the initiator (diisopropyloxydicarbonate) were added to the pressure-resistant reaction vessel.
- the above reaction solution is added to a pressure-resistant reaction vessel with a homomixer (manufactured by Tokushu Kagaku Kogyo Co., Ltd., trade name "TK homomixer”), and isobutane (boiling point: -11.)
- TK homomixer manufactured by Tokushu Kagaku Kogyo Co., Ltd., trade name "TK homomixer”
- isobutane oiling point: -11.
- 70 g (7 ° C.) and 5 g of the initiator (diisopropyloxydicarbonate) were added to the pressure resistant reaction vessel.
- the homomixer was rotated under predetermined initial stirring conditions (stirring speed: 8000 rpm, stirring time: 2 minutes) to stir the mixture, and then the mixture was heated to 60 ° C. while stirring at 80 rpm to carry out a reaction for 24 hours.
- the solid content obtained by filtering the reaction solution after the reaction was left at room temperature for 1 week under a nitrogen stream to obtain thermally expanding microspheres.
- the obtained thermally expandable microspheres had an average particle size of 25 ⁇ m when measured under the trade name “SALD-2000J” manufactured by Shimadzu Corporation.
- SALD-2000J trade name
- X-ray CT Xradia520versa manufactured by ZEISS Co., Ltd. (measurement conditions: tube voltage 60 KV tube current 83 ⁇ A, pixel size 0.20 ⁇ m / pixel)
- the solvents in the thermally expanded microspheres are isopentane and isooctane, and the thermally expandable microspheres. It was found that 15% by weight was contained with respect to the weight of the above-mentioned X-ray CT, and the thickness of the shell of the heat-expandable microsphere was 2.5 ⁇ m.
- an isocyanate-based cross-linking agent manufactured by Toso Co., Ltd., trade name "Coronate L
- toluene are mixed to form an elastic layer.
- the above composition for forming an elastic layer is applied to a PET film as a base material (manufactured by Toray Industries, Inc., trade name "Lumirror S10", thickness: 100 ⁇ m), dried, and the elastic layer (thickness: 15 ⁇ m) is placed on the base material.
- the above composition for forming an adhesive layer is applied to a polyethylene terephthalate film with a silicone release agent-treated surface (manufactured by Mitsubishi Chemical Polyester Film Co., Ltd., trade name "MRF38”), dried, and the adhesive layer is applied on the polyethylene terephthalate film. (35 ⁇ m) was formed.
- the pressure-sensitive adhesive layer formed on the polyethylene terephthalate film was transferred to the elastic layer to obtain a pressure-sensitive adhesive tape having a base material, an elastic layer, and a pressure-sensitive adhesive layer in this order.
- the obtained adhesive tape was subjected to the above evaluations (1) to (4). The results are shown in Table 3.
- composition of the composition for forming an elastic layer composition of base polymer, amount of cross-linking agent
- composition for forming an adhesive layer composition of base polymer, type of cross-linking agent, amount of cross-linking agent, type of thermally expandable microspheres
- An adhesive tape was obtained in the same manner as in Example 1 except that the composition was set to 1 or Table 2.
- the obtained adhesive tape was subjected to the above evaluations (1) to (4).
- the results are shown in Table 3.
- "crosslinking agent Tetrad C” is an epoxy-based crosslinking agent (trade name "Tetrad C") manufactured by Mitsubishi Gas Chemical Company.
- Example 15 A composition for forming an adhesive layer was prepared in the same manner as in Example 1. The above composition for forming an adhesive layer is applied to a PET film as a base material (manufactured by Toray Industries, Inc., trade name "Lumilar ES-10", thickness: 100 ⁇ m), dried, and the pressure-sensitive adhesive layer is formed on the base material. It was formed and an adhesive tape was obtained. The obtained adhesive tape was subjected to the above evaluations (1) to (4). The results are shown in Table 3.
- Example 16 A composition for forming an elastic layer and a composition for forming an adhesive layer were prepared in the same manner as in Example 1.
- acrylic copolymers (2-ethylhexyl acrylate (2EHA), ethyl acrylate (EA), methyl methacrylate (MMA) and 2-hydroxyethyl acrylate (HEA) copolymers
- 2EHA constituent units EA constituent units: MMA constituent units:
- HEA Constituent unit 30:70: 5: 5 (weight ratio)) 100 parts by weight
- adhesive Yamasuhara Chemical Co., Ltd., trade name "Mighty Ace G125"
- isocyanate-based cross-linking agent manufactured by Toso Co., Ltd., 3 parts by weight of the trade name "Coronate L
- toluene were mixed to prepare another composition for forming an adhesive layer.
- the above composition for forming an elastic layer is applied to a PET film as a base material (manufactured by Toray Industries, Inc., trade name "Lumirror S10", thickness: 100 ⁇ m), dried, and the elastic layer (thickness: 15 ⁇ m) is placed on the base material.
- the above composition for forming an adhesive layer is applied to a polyethylene terephthalate film with a silicone release agent-treated surface (manufactured by Mitsubishi Chemical Polyester Film Co., Ltd., trade name "MRF38”), dried, and the adhesive layer is applied on the polyethylene terephthalate film. (35 ⁇ m) was formed.
- the above-mentioned other composition for forming an adhesive layer is applied to a polyethylene terephthalate film with a silicone release agent-treated surface (manufactured by Mitsubishi Chemical Polyester Film Co., Ltd., trade name "MRF38”), dried, and then on the polyethylene terephthalate film.
- Another pressure-sensitive adhesive layer (10 ⁇ m) was formed on the surface.
- the pressure-sensitive adhesive layer formed on the polyethylene terephthalate film is transferred to the elastic layer, another pressure-sensitive adhesive layer is transferred to a surface on which the elastic layer of the base material is not formed, and another pressure-sensitive adhesive layer and the base material are transferred.
- An adhesive tape having an elastic layer and an adhesive layer in this order was obtained.
- the obtained adhesive tape was subjected to the above evaluations (1) to (4). The results are shown in Table 3.
- Example 17 A PI film (manufactured by Toray Industries, Inc., trade name "Kapton 100H", thickness: 25 ⁇ m) was used instead of the PET film (manufactured by Toray Industries, Inc., trade name “Lumirror S10", thickness: 100 ⁇ m) as a base material.
- An adhesive tape was obtained in the same manner as in Example 1 except for the above. The obtained adhesive tape was subjected to the above evaluations (1) to (4). The results are shown in Table 3.
- Example 18 An adhesive tape was obtained in the same manner as in Example 17, except that the heat-expandable microspheres C produced in Production Example 3 were used instead of the heat-expandable microspheres A produced in Production Example 1. The obtained adhesive tape was subjected to the above evaluations (1) to (4). The results are shown in Table 3.
- Adhesive layer 20 Base material 100 Adhesive tape
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Abstract
Description
1つの実施形態においては、上記シェルを構成する樹脂のガラス転移温度(Tg)が120℃以上である。
1つの実施形態においては、上記カルボキシル基を有する構成単位の含有割合が、上記樹脂100重量部に対して、5重量部~97重量部である。
1つの実施形態においては、上記揮発性物質が有機溶媒であり、該有機溶媒の沸点(bp)と上記シェルを構成する樹脂のガラス転移温度(Tg)との差(Tg-bp)が、0℃以上である。
1つの実施形態においては、上記粘着剤が、アクリル系粘着剤である。
1つの実施形態においては、上記粘着材が、イソシアネート系架橋剤またはエポキシ系架橋剤を含む。
1つの実施形態においては、25℃の環境温度下、上記粘着テープの粘着面をポリエチレンテレフタレートフィルムに貼着した際の初期粘着力aが、1.5N/20mm~20N/20mmである。
1つの実施形態においては、130℃まで加熱した後25℃にまで冷却した上記粘着テープの粘着面をポリエチレンテレフタレートフィルムに貼着した際の粘着力bが、25℃の環境温度下で上記粘着テープの粘着面をポリエチレンテレフタレートフィルムに貼着した際の初期粘着力aに対して、50%以上である。
1つの実施形態においては、130℃まで加熱した後25℃にまで冷却するというサイクルを2回行った後の本発明の粘着テープの粘着面をポリエチレンテレフタレートフィルムに貼着した際の粘着力cが、25℃の環境温度下で上記粘着テープの粘着面をポリエチレンテレフタレートフィルムに貼着した際の初期粘着力aに対して、50%以上である。
1つの実施形態においては、上記粘着テープは、上記基材の両側に上記粘着剤層を備える。
1つの実施形態においては、上記基材の一方の側に上記粘着剤層を備え、該基材の他方の側に別の粘着剤層を備える。
図1(a)および(b)は、本発明の1つの実施形態による粘着テープの概略断面図である。粘着テープ100は、基材10と、基材10の少なくとも片側に配置された粘着剤層20とを備える。図1(c)は本発明の別の実施形態による粘着テープの概略断面図である。粘着テープ200は、粘着剤層10と、粘着剤層10の少なくとも片側に配置された別の粘着剤層30とを備える。図示していないが、上記粘着テープは、粘着剤層以外の層として、上記粘着テープに弾性を付与しうる弾性層(後述E項)、粘着剤層上に剥離可能に配置されたセパレータ(後述F項)等をさらに備え得る。
上記のとおり、上記粘着剤層は、熱膨張性微小球を含む。実用的には、粘着剤層は、粘着剤をさらに含む。
熱膨張性微小球は、シェル(殻)と、当該シェル内に含まれる揮発性物質(代表的には、有機溶媒)とから構成される。
1/(273+Tg)=Σ(Wi/(273+Tgi))
単量体から形成される単重合体のガラス転移温度としては、メタクリル酸単重合体:228℃、アクリロニトリル単重合体:97℃、メチルメタクリレート単重合体:102℃、メタクリロイルニトリル単重合体:120℃、塩化ビニリデン単重合体:75℃、イソボルニルアクリレート単重合体:97℃である。また、これら以外の単重合体のガラス転移温度としては、「Polymer Handbook」(第4版、John Wiley & Sons,Inc、1999年)に記載された値を使用することができる。なお、この文献中、複数のTgの値が記載されている場合は、「conventional」の値を採用する。
熱膨張性微小球の含有割合(重量%)=熱膨張性微小球の重量/粘着剤層の重量×100
上記粘着剤層を構成する粘着剤としては、本発明の効果が得られる限りにおいて、任意の適切な粘着剤が用いられ得る。上記粘着剤としては、例えば、アクリル系粘着剤、シリコーン系粘着剤、ビニルアルキルエーテル系粘着剤、ポリエステル系粘着剤、ポリアミド系粘着剤、ウレタン系粘着剤、フッ素系粘着剤、スチレン-ジエンブロック共重合体系粘着剤、活性エネルギー線硬化型粘着剤等が挙げられる。中でも好ましくは、アクリル系粘着剤、ゴム系粘着剤またはシリコーン系粘着剤であり、より好ましくはアクリル系粘着剤である。
粘着剤約0.1gをサンプリングして精秤し(試料の重量)、該サンプルをメッシュ状シート(商品名「NTF-1122」、日東電工株式会社製)で包んだ後、約50mlのトルエン中に室温で1週間浸漬させた。その後、溶剤不溶分(メッシュ状シートの内容物)をトルエンから取り出し、70℃で約5時間乾燥させ、乾燥後の溶剤不溶分を秤量し(浸漬・乾燥後の重量)、下記式(a)よりゲル分率(重量%)を算出する。
ゲル分率(重量%)=[(浸漬・乾燥後の重量)/(試料の重量)]×100 (a)
(i)粘着剤層を、溶媒に投入し、粘着剤層中の溶媒可溶分を上記溶媒に溶解させる溶液試料を調製する。
溶媒としては、極性等を考慮して、クロロホルム(CHCl3)、塩化メチレン(CH2Cl2)、テトラヒドロフラン(THF)、アセトン、ジメチルスルホキシド(DMSO)、N,N-ジメチルホルムアミド(DMF)、メタノール、エタノール、トルエンおよび水等から選択されるいずれか1種の溶媒または2種以上を任意の比率で含む混合溶媒を用いることができる。
典型的には、粘着剤層0.2g程度に溶媒30mL程度を加え、室温から用いる溶媒の沸点程度までの温度域で30分~12時間程度撹拌する。必要に応じて、例えば分析対象成分の抽出効率が低い場合等には、上記溶液を分取した後の試料に、分取した溶液と概ね同量の溶媒を新たに加えて撹拌し、その溶液を分取する操作を1回または複数回繰り返して溶液試料を調製してもよい。
(ii)上記溶液試料から溶媒を、蒸発等の方法により、溶媒を除去し、溶媒可溶性ポリマーを取り出すことができる。
なお溶媒可溶性ポリマーには未反応架橋剤の低分子量分など測定対象とならない溶媒可溶分が含まれることがある。その際には、上記溶液試料をポリマー成分のみ不溶な溶媒に投入する方法(再沈殿法)や、上記溶液試料を用いたゲル濾過クロマトグラフィーで分子量分画(分取液体クロマトグラフィ法)するなどして測定対象のみからなる溶媒可溶性ポリマーを調整する。
上記アクリル系粘着剤としては、例えば、(メタ)アクリル酸アルキルエステルの1種または2種以上を単量体成分として用いたアクリル系ポリマー(ホモポリマーまたはコポリマー)をベースポリマーとするアクリル系粘着剤等が挙げられる。(メタ)アクリル酸アルキルエステルの具体例としては、(メタ)アクリル酸メチル、(メタ)アクリル酸エチル、(メタ)アクリル酸プロピル、(メタ)アクリル酸イソプロピル、(メタ)アクリル酸ブチル、(メタ)アクリル酸イソブチル、(メタ)アクリル酸s-ブチル、(メタ)アクリル酸t-ブチル、(メタ)アクリル酸ペンチル、(メタ)アクリル酸ヘキシル、(メタ)アクリル酸ヘプチル、(メタ)アクリル酸オクチル、(メタ)アクリル酸2-エチルヘキシル、(メタ)アクリル酸イソオクチル、(メタ)アクリル酸ノニル、(メタ)アクリル酸イソノニル、(メタ)アクリル酸デシル、(メタ)アクリル酸イソデシル、(メタ)アクリル酸ウンデシル、(メタ)アクリル酸ドデシル、(メタ)アクリル酸トリデシル、(メタ)アクリル酸テトラデシル、(メタ)アクリル酸ペンタデシル、(メタ)アクリル酸ヘキサデシル、(メタ)アクリル酸ヘプタデシル、(メタ)アクリル酸オクタデシル、(メタ)アクリル酸ノナデシル、(メタ)アクリル酸エイコシル等の(メタ)アクリル酸C1-20アルキルエステルが挙げられる。なかでも、炭素数が4~18の直鎖状もしくは分岐状のアルキル基を有する(メタ)アクリル酸アルキルエステルが好ましく用いられ得る。
上記シリコーン系粘着剤としては、本発明の効果が得られる限り、任意の適切な粘着剤が用いられ得る。上記シリコーン系粘着剤として、例えば、オルガノポリシロキサンを含むシリコーンゴムまたはシリコーンレジン等をベースポリマーとするシリコーン系粘着剤が好ましく用いられる。シリコーン系粘着剤を構成するベースポリマーとして、上記シリコーンゴムまたはシリコーンレジンを、架橋して得られたベースポリマーを用いてもよい。なお、本明細書において、「シリコーンゴム」とは、主成分としてのジオルガノシロキサン(D単位)が直鎖状に連なった重合体(例えば、粘度1000Pa・s)を意味し、「シリコーンレジン」とは、主成分としてのトリオルガノシルヘミオキサン(M単位)とシリケート(Q単位)から構成される重合体を意味する(「粘着剤(フィルム・テープ)の材料設計と機能性付与」、技術情報協会、2009年9月30日発刊)。
上記ゴム系粘着剤としては、本発明の効果が得られる限り、任意の適切な粘着剤が用いられ得る。上記ゴム系粘着剤として、例えば、天然ゴム;ポリイソプレンゴム、ブタジエンゴム、スチレン・ブタジエン(SB)ゴム、スチレン・イソプレン(SI)ゴム、スチレン・イソプレン・スチレンブロック共重合体(SIS)ゴム、スチレン・ブタジエン・スチレンブロック共重合体(SBS)ゴム、スチレン・エチレン・ブチレン・スチレンブロック共重合体(SEBS)ゴム、スチレン・エチレン・プロピレン・スチレンブロック共重合体(SEPS)ゴム、スチレン・エチレン・プロピレンブロック共重合体(SEP)ゴム、再生ゴム、ブチルゴム、ポリイソブチレンゴム、またはこれらの変性体等の合成ゴム;等をベースポリマーとするゴム系粘着剤が好ましく用いられる。
上記粘着剤は、必要に応じて、任意の適切な添加剤を含み得る。該添加剤としては、例えば、架橋剤、粘着付与剤、可塑剤、顔料、染料、充填剤、老化防止剤、導電材、帯電防止剤、紫外線吸収剤、光安定剤、剥離調整剤、軟化剤、界面活性剤、難燃剤、酸化防止剤等が挙げられる。
23℃における上記粘着剤層のナノインデンテーション法による弾性率は、好ましくは0.1MPa~500MPaであり、より好ましくは0.5MPa~400MPaである。ナノインデンテーション法による弾性率とは、粘着剤層表面から3μm程度内側で、かつ、熱膨張微小球の存在しない箇所(熱膨張微小球のシェル表面から1μm以上離れた箇所)を測定対象として、圧子を粘着剤層に押し込んだときの、圧子への負荷荷重と押し込み深さとを負荷時、除荷時にわたり連続的に測定し、得られた負荷荷重-押し込み深さ曲線から求められる。本明細書において、ナノインデンテーション法による弾性率とは、測定条件を負荷・除荷速度:1000nm/s、押し込み深さ:800nmとして上記のように測定した弾性率をいう。
上記粘着剤層は、本発明の効果が得られる限りにおいて、任意の適切なその他の成分をさらに含み得る。その他の成分としては、例えば、ビーズが挙げられる。該ビーズとしては、例えば、ガラスビーズ、樹脂ビーズ等が挙げられる。粘着剤層にこのようなビーズを添加すれば、粘着剤層の弾性率を向上させることができ、より精度良く被加工物を加工することができる粘着テープが得られ得る。ビーズの平均粒子径は、例えば0.01μm~50μmである。ビーズの添加量は、粘着剤層100重量部に対して、例えば10重量部~200重量部、好ましくは20重量部~100重量部である。
上記基材としては、例えば、樹脂シート、不織布、紙、金属箔、織布、ゴムシート、発泡シート、これらの積層体(特に、樹脂シートを含む積層体)等が挙げられる。樹脂シートを構成する樹脂としては、例えば、ポリエチレンテレフタレート(PET)、ポリエチレンナフタレート(PEN)、ポリブチレンテレフタレート(PBT)、ポリエチレン(PE)、ポリプロピレン(PP)、エチレン-プロピレン共重合体、エチレン-酢酸ビニル共重合体(EVA)、ポリアミド(ナイロン)、全芳香族ポリアミド(アラミド)、ポリイミド(PI)、ポリ塩化ビニル(PVC)、ポリフェニレンサルファイド(PPS)、フッ素系樹脂、ポリエーテルエーテルケトン(PEEK)等が挙げられる。不織布としては、マニラ麻を含む不織布等の耐熱性を有する天然繊維による不織布;ポリプロピレン樹脂不織布、ポリエチレン樹脂不織布、エステル系樹脂不織布等の合成樹脂不織布等が挙げられる。金属箔としては、銅箔、ステンレス箔、アルミニウム箔等が挙げられる。紙としては、和紙、クラフト紙等が挙げられる。
上記別の粘着剤層としては、任意の適切な粘着剤層が形成され得る。別の粘着剤層を形成する粘着剤としては、例えば、ゴム系粘着剤、アクリル系粘着剤、ビニルアルキルエーテル系粘着剤、シリコーン系粘着剤、ポリエステル系粘着剤、ポリアミド系粘着剤、ウレタン系粘着剤、フッ素系粘着剤、スチレン-ジエンブロック共重合体系粘着剤等が挙げられる。粘着剤には、例えば、可塑剤、充填剤、界面活性剤、老化防止剤、粘着性付与剤などの公知乃至慣用の添加剤が配合されていてもよい。
本発明の粘着テープは、弾性層をさらに備えていてもよい。弾性層は、粘着剤層の片面に配置され得る。粘着テープが基材を備える場合、弾性層は、粘着剤層と基材との間に配置され得る。弾性層を備えることにより、被着体に対する追従性が向上する。また、弾性層を備える粘着テープは、剥離時に加熱した際には、粘着剤層の面方向の変形(膨張)が拘束され、厚み方向の変形が優先される。その結果、剥離性が向上する。
本発明の粘着テープは、必要に応じて、セパレータをさらに備え得る。該セパレータは少なくとも一方の面が剥離面となっており、上記粘着剤層を保護するために設けられ得る。セパレータは、任意の適切な材料から構成され得る。
本発明の粘着テープは、任意の適切な方法により製造することができる。本発明の粘着テープは、例えば、基材上に直接、粘着剤および熱膨張性微小球を含む粘着剤層形成用組成物を塗工する方法、または任意の適切な基体上に粘着剤層形成用組成物を塗工し形成された塗工層を基材に転写する方法等が挙げられる。粘着剤層形成用組成物は、任意の適切な溶媒を含み得る。また、粘着剤を含む組成物により粘着剤塗工層を形成した後、該粘着剤塗工層に熱膨張性微小球を振りかけた後、ラミネーター等を用いて、該熱膨張性微小球を該塗工層中に埋め込んで、熱膨張性微小球を含む粘着剤層を形成してもよい。
本発明の粘着テープは、電子部品を製造・評価する際に、電子部品材料を仮固定するためのシートとして、好適に用いられ得る。1つの実施形態においては、本発明の粘着テープは、冷熱衝撃試験において被試験体を仮固定するための粘着テープとして用いられ得る。別の実施形態においては、本発明の粘着テープは、基板レス半導体パッケージ製造時の樹脂封止工程において被加工体を仮固定するための粘着テープとして用いられ得る。ここで、半導体パッケージとは、プリント基板上に単体の高集積度半導体を表面実装可能にする半導体部品のパッケージの形態を指す。具体的には、ウエハーレベルチップサイズパッケージ(WLCSP)やファンアウトウェハレベルパッケージ(FOWLP)やファンインウェハレベルパッケージ(FIWLP)などを指す。これらパッケージの製造での樹脂封止工程では、樹脂硬化のための加熱や樹脂注入圧力が生じるが、粘着テープはこれらに抗ってベアチップが移動することなく所定の位置に保持される機能が必要である。また、封止工程後にはベアチップから簡単に剥がせる機能が必要である。すなわち、本願に開示する粘着テープは、前述したパッケージの製造に好適に用いられ得るものであり、特に樹脂封止工程ではその機能をいかんなく発揮しうるものである。さらに別の実施形態においては、本発明の粘着テープは、配線回路のパターンニング工程において被加工体を仮固定するための粘着テープとして用いられ得る。さらに別の実施形態においては、本発明の粘着テープは、電子部品の電極塗布・乾燥工程において被加工体を仮固定するための粘着テープとして用いられ得る。さらに別の実施形態においては、本発明の粘着テープは、電子部品の小片化工程と熱処理工程とを同じテープ上で一貫して加工するために被着体を仮固定するための粘着テープとして用いられ得る。このように本発明の粘着テープは、加熱を伴う工程に好適に用いられ得る。
(1)初期粘着力
粘着テープを幅:20mm、長さ:140mmのサイズに切断し、粘着剤層上に、被着体としてのポリエチレンテレフタレートフィルム(商品名「ルミラーS-10」東レ社製;厚さ:25μm、幅:25mm)を、JIS Z 0237(2000年)に準じ、温度:25℃および湿度:65%RHの雰囲気下で、2kgのローラーを1往復させて圧着して貼り合わせた。次いで、被着体付きの粘着テープを、25℃に設定された恒温槽付き引張試験機(島津製作所社製、商品名「島津オートグラフAG-120kN」)にセットし、30分間放置した。その後、被着体を、剥離角度:180°、引張速度:300mm/minの条件で、粘着テープから引き剥がした時の荷重を測定し、その際の最大荷重(測定初期のピークトップを除いた荷重の最大値)を求め、この最大荷重を粘着力(N/20mm)とした。
(チップ飛び)
各粘着テープの粘着剤層上に、エポキシ樹脂(日立化成社製、商品名「CEL-9200HF9」)で封止されたQFNリードフレーム(サイズ:125mm×65mm;粘着シートとの貼り合せ面は樹脂面)を貼着させ、それを6インチのダイシングリングに装着固定してダイサーを介し、5mm×5mmのサイズのチップにフルカットした(ダイシングによる切断加工処理を施した)。このカットの際に、チップ飛びの発生の個数を算出した。この時ダイシングブレードにはDISCO社製ZH05-SD2000-N1-110-DDを用いた。ダイシングブレードの送り速度は70mm/S、ダイシングブレードの回転数を50000/sとした。
切断加工中のチップが粘着テープから剥がれた(チップ飛びした)個数の割合(チップ飛び率)(%)を求め、切断加工性の評価とした。なお、すべてのチップが粘着テープに貼着しており剥がれていない場合は、チップ飛び率は0%(すなわち、チップ飛び率は0%)となる。ダイシングしたチップの数をA0、チップが飛んだ数をAとし、チップ飛び率Xは式(1)に従い求めた。
X=(A/A0)×100 ・・・(1)
チップが剥がれている割合(チップ飛び率)が小さいほど、チップ飛び防止性が良好であることを意味している。
(チップ残り)
前記カット後、プログラム温度調節器(熱風乾燥器)(株式会社いすゞ製作所製、「EP-K-300」)を用いて、発泡温度で5分間加熱処理を施した。加熱処理後、粘着テープを空中で上下が反対になるように裏返しにし(チップが下になる様に)、粘着テープからチップを自然落下により剥離させ、シート上に残存したチップの割合(チップ残り)(%)を求める。なお、すべてのチップが剥離して粘着テープに残存していない場合は、チップ残りは0%となる。従って、加熱処理後に加工後のチップが残存する量が少ない(チップ残りが少ない)であることが、加熱剥離性が良好であることを意味している。剥離する前のチップ数をB0、加熱剥離処理後のシート上に残ったチップの数をBとし、チップ残りYは式(2)に従い求めた。
Y=(B/B0)×100 ・・・(2)
各粘着テープを幅:50mm、長さ:100mmのサイズに切断し、セパレーターを剥離後、熱膨張微小球を含む粘着剤面にカッターで碁盤目状(5mm間隔でX-Y方向に5本ずつ)の切り込みを入れ、再びセパレーターをハンドローラーで貼り合せる。このとき、粘着剤層部分はフルカットし、基材にも切りこまれている状態とした。
熱源の天板上に10mm厚の耐熱ガラスを置いた状態で、発泡温度+20℃に予熱したホットプレート(シャマルホットプレート「HHP-411」)を用いて、上記碁盤目状の切り込みを入れた試験片(加熱部分は50mm×50mm)を5分間加熱し、取り出したサンプルの粘着剤層浮き個数をカウントした。
上記(2)におけるカット後、プログラム温度調節器(熱風乾燥器)(株式会社いすゞ製作所製、「EP-K-300」)を用いて、発泡温度で5分間加熱処理を施した。加熱処理後、粘着テープを空中で上下が反対になるように裏返しにし(チップが下になる様に)、粘着テープからチップを自然落下により剥離させ、回収されたチップに粘着剤異物が付着している割合(糊付着)(%)を目視により確認した。なお、すべてのチップに粘着剤異物が付着していない場合は、糊付着は0%となる。従って、加熱処理後に加工後のチップに糊付着する量が少ない(糊付着が少ない)であることが、糊付着性が良好であることを意味している。加熱剥離したチップの中から任意に100チップ回収し、式(3)の分母とする(加熱剥離したチップが100を満たさない場合はその数をC0とする)。その中で糊付着したチップの数をCとし、糊付着Zは式(3)に従い求めた。
Z=(C/C0)×100 ・・・(3)
塩化ナトリウム150gと、シリカ有効成分20重量%であるコロイダルシリカ(日産化学株式会社製、商品名「スノーテックス」)70gと、ポリビニルピロリドン1gと、ジエタノールアミンとアジピン酸の縮合物0.5gとを、蒸留水600gに加えた後、得られた混合物のpHを2.8~3.2に調整して水性溶液を得た。
上記水性溶液に、シェルの材料となる油系添加剤として、アクリロニトリル125gと、メタクリル酸120gを加えた。さらに、架橋剤としてのエチレングリコールジメタクリレート1gを加え、反応溶液を得た。
上記反応溶液をホモミキサー(特殊機化工業社製、商品名「TKホモミキサー」)付き耐圧反応容器に加え、さらに、シェルに内包されることを意図した有機溶媒としてイソペンタン(沸点:27.7℃)20gとイソオクタン(沸点:99℃)55gと、開始剤(ジイソプロピルオキシジカーボネート)5gとを耐圧反応容器に加えた。
上記反応溶液をホモミキサー(特殊機化工業社製、商品名「TKホモミキサー」)付き耐圧反応容器に加え、さらに、シェルに内包されることを意図した有機溶媒としてイソブタン(沸点:-11.7℃)70gと、開始剤(ジイソプロピルオキシジカーボネート)5gとを耐圧反応容器に加えた。
ホモミキサーを所定の初期攪拌条件(攪拌速度:8000rpm、攪拌時間:2分間)で回転させて上記混合物を撹拌した後、80rpmで攪拌しながら60℃に加温して24時間反応を行った。反応後の反応溶液をろ過することで得られる固形分を窒素気流下室温に1週間放置することで熱膨張性微小球を得た。
なお、得られた熱膨張性微小球は、島津製作所製の商品名「SALD-2000J」で計測したところ、平均粒径が25μmであった。また、X線CT(ZEISS社製 Xradia520versa(測定条件:管電圧60KV 管電流83μA、ピクセルサイズ0.20μm/pixel)により、熱膨張微小球内の溶媒はイソペンタンおよびイソオクタンであり、熱膨張性微小球の重量に対して、15重量%含むことがわかった。また、上記X線CTにより測定したところ、熱膨張性微小球のシェルの厚みは、2.5μmであった。
油系添加剤(アクリロニトリル、メタクリル酸、メタクリロニトリル、メチルメタクリレート、アクリル酸)の組成を表1に記載のとおりとしたこと以外は、製造例1と同様にして、熱膨張性微小球B~Kを作製した。また、製造例1と同様にして、熱膨張性微小球の平均粒径を測定した。結果を表3に示す。
(弾性層形成用組成物の調製)
アクリル系コポリマー(2-エチルヘキシルアクリレート(2EHA)、エチルアクリレート(EA)、メチルメタクリレート(MMA)および2-ヒドロキシエチルアクリレート(HEA)のコポリマー、2EHA構成単位:EA構成単位:MMA構成単位:HEA構成単位=30:70:5:5(重量比))100重量部と、イソシアネート系架橋剤(東ソー社製、商品名「コロネートL」)1重量部と、トルエンを混合し、弾性層形成用組成物を調製した。
(粘着剤層形成用組成物の調製)
アクリル系コポリマー(2-エチルヘキシルアクリレート(2EHA)、エチルアクリレート(EA)、メチルメタクリレート(MMA)および2-ヒドロキシエチルアクリレート(HEA)のコポリマー、2EHA構成単位:EA構成単位:MMA構成単位:HEA構成単位=30:70:5:5(重量比))100重量部と、粘着付与剤(ヤスハラケミカル社製、商品名「マイティーエースG125」)20重量部と、イソシアネート系架橋剤(東ソー社製、商品名「コロネートL」)2重量部と、熱膨張性微小球Aを30重量部と、トルエンとを混合し、粘着剤層形成用組成物を調製した。
(粘着テープの作製)
基材としてのPETフィルム(東レ社製、商品名「ルミラーS10」、厚み:100μm)に、上記弾性層形成用組成物を塗布し、乾燥して、基材上に弾性層(厚み:15μm)を形成した。
シリコーン離型剤処理面付きポリエチレンテレフタレートフィルム(三菱化学ポリエステルフィルム社製、商品名「MRF38」)に、上記粘着剤層形成用組成物を塗布し、乾燥して、ポリエチレンテレフタレートフィルム上に粘着剤層(35μm)を形成した。
ポリエチレンテレフタレートフィルム上に形成された上記粘着剤層を、上記弾性層に転写して、基材、弾性層および粘着剤層をこの順に備える粘着テープを得た。得られた粘着テープを上記評価(1)~(4)に供した。結果を表3に示す。
弾性層形成用組成物(ベースポリマーの組成、架橋剤量)、および粘着剤層形成用組成物(ベースポリマーの組成、架橋剤種類、架橋剤量、熱膨張性微小球種類)の組成を表1または表2に示す組成としたこと以外は、実施例1と同様にして粘着テープを得た。得られた粘着テープを上記評価(1)~(4)に供した。結果を表3に示す。なお、表1または表2中、「架橋剤テトラッドC」は、三菱ガス化学社製のエポキシ系架橋剤(商品名「テトラッドC」)である。
実施例1と同様にして、粘着剤層形成用組成物を調製した。
基材としてのPETフィルム(東レ社製、商品名「ルミラーES-10」、厚み:100μm)に、上記粘着剤層形成用組成物を塗布し、乾燥して、基材上に粘着剤層を形成し、粘着テープを得た。得られた粘着テープを上記評価(1)~(4)に供した。結果を表3に示す。
実施例1と同様にして、弾性層形成用組成物および粘着剤層形成用組成物を調製した。
さらに、アクリル系コポリマー (2-エチルヘキシルアクリレート(2EHA)、エチルアクリレート(EA)、メチルメタクリレート(MMA)および2-ヒドロキシエチルアクリレート(HEA)のコポリマー、2EHA構成単位:EA構成単位:MMA構成単位:HEA構成単位=30:70:5:5(重量比))100重量部と、粘着付与剤(ヤスハラケミカル社製、商品名「マイティーエースG125」)10重量部と、イソシアネート系架橋剤(東ソー社製、商品名「コロネートL」)3重量部と、トルエンとを混合し、別の粘着剤層形成用組成物を調製した。
基材としてのPETフィルム(東レ社製、商品名「ルミラーS10」、厚み:100μm)に、上記弾性層形成用組成物を塗布し、乾燥して、基材上に弾性層(厚み:15μm)を形成した。
シリコーン離型剤処理面付きポリエチレンテレフタレートフィルム(三菱化学ポリエステルフィルム社製、商品名「MRF38」)に、上記粘着剤層形成用組成物を塗布し、乾燥して、ポリエチレンテレフタレートフィルム上に粘着剤層(35μm)を形成した。
また、シリコーン離型剤処理面付きポリエチレンテレフタレートフィルム(三菱化学ポリエステルフィルム社製、商品名「MRF38」)に、上記別の粘着剤層形成用組成物を塗布し、乾燥して、ポリエチレンテレフタレートフィルム上に別の粘着剤層(10μm)を形成した。
ポリエチレンテレフタレートフィルム上に形成された上記粘着剤層を上記弾性層に転写し、別の粘着剤層を基材の弾性層が形成されていない面に転写して、別の粘着剤層、基材、弾性層および粘着剤層をこの順に備える粘着テープを得た。
得られた粘着テープを上記評価(1)~(4)に供した。結果を表3に示す。
基材としてのPETフィルム(東レ社製、商品名「ルミラーS10」、厚み:100μm)に代えて、PIフィルム(東レ・デュポン社製、商品名「カプトン100H」、厚み:25μm)を用いたこと以外は、実施例1と同様にして粘着テープを得た。得られた粘着テープを上記評価(1)~(4)に供した。結果を表3に示す。
製造例1で作製した熱膨張性微小球Aに代えて、製造例3で作製した熱膨張性微小球Cを用いたこと以外は、実施例17と同様にして粘着テープを得た。得られた粘着テープを上記評価(1)~(4)に供した。結果を表3に示す。
製造例1で作製した熱膨張性微小球Aに代えて、製造例11で作製した熱膨張性微小球Kを用いたこと以外は、実施例15と同様にして粘着テープを得た。得られた粘着テープを上記評価(1)~(4)に供した。結果を表3に示す。
20 基材
100 粘着テープ
Claims (11)
- 基材と、該基材の少なくとも片側に配置された粘着剤層とを備え、
該粘着剤層が熱膨張性微小球および粘着剤を含み、
該熱膨張性微小球が、シェルと、該シェル内に含まれる揮発性物質とから構成され、
該シェルを構成する樹脂がカルボキシル基を有する構成単位を含む、
粘着テープ。 - 前記シェルを構成する樹脂のガラス転移温度(Tg)が120℃以上である、請求項1に記載の粘着テープ。
- 前記カルボキシル基を有する構成単位の含有割合が、前記樹脂100重量部に対して、5重量部~97重量部である、請求項1または2に記載の粘着テープ。
- 前記揮発性物質が有機溶媒であり、
該有機溶媒の沸点(bp)と前記シェルを構成する樹脂のガラス転移温度(Tg)との差(Tg-bp)が、0℃以上である、請求項1から3のいずれかに記載の粘着テープ。 - 前記粘着剤が、アクリル系粘着剤である、請求項1から4のいずれかに記載の粘着テープ。
- 前記粘着材が、イソシアネート系架橋剤またはエポキシ系架橋剤を含む、請求項1から5のいずれかに記載の粘着テープ。
- 25℃の環境温度下、前記粘着テープの粘着面をポリエチレンテレフタレートフィルムに貼着した際の初期粘着力aが、1.5N/20mm~20N/20mmである、請求項1から6のいずれかに記載の粘着テープ。
- 130℃まで加熱した後25℃にまで冷却した前記粘着テープの粘着面をポリエチレンテレフタレートフィルムに貼着した際の粘着力bが、25℃の環境温度下で前記粘着テープの粘着面をポリエチレンテレフタレートフィルムに貼着した際の初期粘着力aに対して、50%以上である、請求項1から7のいずれかに記載の粘着テープ。
- 130℃まで加熱した後25℃にまで冷却するというサイクルを2回行った後の本発明の粘着テープの粘着面をポリエチレンテレフタレートフィルムに貼着した際の粘着力cが、25℃の環境温度下で前記粘着テープの粘着面をポリエチレンテレフタレートフィルムに貼着した際の初期粘着力aに対して、50%以上である、請求項1から8のいずれかに記載の粘着テープ。
- 前記基材の両側に前記粘着剤層を備える、請求項1から9のいずれかに記載の粘着テープ。
- 前記基材の一方の側に前記粘着剤層を備え、該基材の他方の側に別の粘着剤層を備える、請求項1から9のいずれかに記載の粘着テープ。
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