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WO2018181511A1 - Procédé de délaminage d'une feuille adhésive - Google Patents

Procédé de délaminage d'une feuille adhésive Download PDF

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Publication number
WO2018181511A1
WO2018181511A1 PCT/JP2018/012838 JP2018012838W WO2018181511A1 WO 2018181511 A1 WO2018181511 A1 WO 2018181511A1 JP 2018012838 W JP2018012838 W JP 2018012838W WO 2018181511 A1 WO2018181511 A1 WO 2018181511A1
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WIPO (PCT)
Prior art keywords
pressure
sensitive adhesive
adhesive sheet
adhesive layer
meth
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PCT/JP2018/012838
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English (en)
Japanese (ja)
Inventor
和恵 上村
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リンテック株式会社
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Publication of WO2018181511A1 publication Critical patent/WO2018181511A1/fr

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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
    • 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
    • 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]
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/683—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping

Definitions

  • the present invention relates to a pressure-sensitive adhesive sheet peeling method capable of reducing the adhesive strength at a desired timing and easily peeling the adherend.
  • an adhesive sheet may be used to temporarily fix a processing target such as an electronic member such as a semiconductor wafer or a display device constituent member (electronic member / optical member).
  • a pressure-sensitive adhesive sheet can reduce the pressure-sensitive adhesive force of the pressure-sensitive adhesive sheet at a desired timing by a method such as applying energy, thereby facilitating the separation of the object to be processed (the adherend).
  • it is subjected to a desired processing step in a state where an adherend such as an electronic member or an optical member is fixed to the adhesive sheet.
  • An object of the present invention is to provide a peeling method between an adhesive sheet and an adherend that can reduce the adhesive force at a desired timing by a novel action mechanism.
  • this invention is a peeling method of the adhesive sheet which peels an adhesive sheet provided with an adhesive layer at least, and the to-be-adhered body stuck on the adhesive surface of the said adhesive layer,
  • the said adhesive layer is
  • the pressure-sensitive adhesive layer has an air chamber inside, and at least the pressure-sensitive adhesive sheet to which the adherend is adhered is subjected to a decompression treatment for expanding the gas in the air chamber, whereby the pressure-sensitive adhesive force of the pressure-sensitive adhesive layer is increased.
  • the pressure-sensitive adhesive sheet peeling method is provided, wherein the pressure-sensitive adhesive sheet and the adherend are peeled off (Invention 1).
  • the “sheet” in the present invention includes the concept of “tape”.
  • the adhesive force can be reduced at a desired timing by a novel action mechanism of expanding the gas in the air chamber by a decompression process. Peeling of the sheet and the adherend can be facilitated.
  • the pressure reduction treatment is made lower than the atmospheric pressure of the environment in which the adhesive sheet is adhered to the adherend (Invention 2).
  • the adhesive composition which forms the said adhesive layer may not have active energy ray curability and thermosetting (invention 3), and this invention (invention) In 3), it is preferable that the pressure-sensitive adhesive composition contains a (meth) acrylic acid ester polymer (Invention 4).
  • the adhesive composition which forms the said adhesive layer may have active energy ray curability or thermosetting (invention 5), and in this invention (invention 5)
  • the active energy ray-curable pressure-sensitive adhesive composition preferably contains a (meth) acrylic acid ester polymer having an active energy ray-curable group in the side chain (Invention 6).
  • the said pressure reduction process may be performed (invention 7), and the said pressure reduction After the treatment, the pressure-sensitive adhesive layer may be cured by irradiating the pressure-sensitive adhesive layer with energy rays (Invention 8).
  • the pressure-sensitive adhesive sheet is preferably used for temporarily fixing the adherend (Invention 9).
  • the adherend is an electronic member or an optical member. It may be a member (Invention 10).
  • this invention is a manufacturing method of the workpiece obtained by processing a workpiece
  • a manufacturing method is provided (Invention 11).
  • the adhesive force can be reduced at a desired timing by a novel action mechanism, and the peeling between the pressure-sensitive adhesive sheet and the adherend is facilitated. be able to.
  • the peeling method of the adhesive sheet which concerns on this embodiment is a method of peeling an adhesive sheet provided with an adhesive layer at least, and the to-be-adhered body stuck on the adhesive surface of the said adhesive layer.
  • the pressure-sensitive adhesive layer has an air chamber inside, and in the present embodiment, at least the pressure-sensitive adhesive sheet to which the adherend is adhered is subjected to a decompression process for expanding the gas in the air chamber. The adhesive strength of the pressure-sensitive adhesive layer is reduced, and the pressure-sensitive adhesive sheet and the adherend are easily separated.
  • FIG. 1 is a sectional view of an adhesive sheet used in one embodiment of the present invention.
  • the pressure-sensitive adhesive sheet 1 according to this embodiment includes a pressure-sensitive adhesive layer 2, and the pressure-sensitive adhesive layer 2 has an air chamber 3 inside.
  • the pressure-sensitive adhesive sheet 1 according to the present embodiment is a surface opposite to the pressure-sensitive adhesive surface P (the surface in contact with the adherend, the upper surface in FIG. 1) in the pressure-sensitive adhesive layer (the lower surface in FIG. 1).
  • a substrate 4 may be further provided.
  • the pressure-sensitive adhesive sheet 1 according to this embodiment can be used for temporarily fixing an electronic member or an optical member, for example.
  • the case where it is used for temporarily fixing a semiconductor wafer will be mainly described.
  • the pressure-sensitive adhesive layer is formed from a pressure-sensitive adhesive composition that does not have active energy ray curability and thermosetting (hereinafter sometimes referred to as “non-curable” in the present specification). It may be a pressure-sensitive adhesive layer, or may be a pressure-sensitive adhesive layer formed from a pressure-sensitive adhesive composition having active energy ray curability or thermosetting. When the pressure-sensitive adhesive layer is composed of multiple layers, a combination of a non-curable pressure-sensitive adhesive layer and a curable pressure-sensitive adhesive layer may be used.
  • Non-curable pressure-sensitive adhesive compositions examples include acrylic pressure-sensitive adhesive compositions, rubber-based pressure-sensitive adhesive compositions, silicone-based pressure-sensitive adhesive compositions, and urethane-based pressure-sensitive adhesives. Examples thereof include a composition, a polyester-based pressure-sensitive adhesive composition, a polyvinyl ether-based pressure-sensitive adhesive composition, and among them, an acrylic pressure-sensitive adhesive composition is preferable.
  • an acrylic adhesive composition what contains a conventionally well-known (meth) acrylic acid ester polymer can be used. In the present specification, the term “polymer” includes the concept of “copolymer”.
  • the (meth) acrylic acid ester polymer (A) contained in the acrylic pressure-sensitive adhesive composition may be a homopolymer formed from one type of (meth) acrylic acid ester monomer, or a plurality of types of ( The copolymer may be a copolymer formed from a (meth) acrylate monomer, or a copolymer formed from one or more types of (meth) acrylate monomers and monomers other than (meth) acrylate monomers. It may be a polymer. Moreover, a (meth) acrylic acid ester polymer (A) may be used individually by 1 type, and may be used in combination of 2 or more type.
  • Specific types of the compound that becomes the (meth) acrylic acid ester monomer are not particularly limited, and specific examples include (meth) acrylic acid, (meth) acrylic acid ester, and derivatives thereof (acrylonitrile, itaconic acid, and the like).
  • Specific examples of (meth) acrylic acid esters include chain skeletons such as methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, and 2-ethylhexyl (meth) acrylate.
  • (meth) acrylate Having Dorokishi group (meth) acrylate; glycidyl (meth) acrylate, (meth) acrylates having reactive functional groups other than hydroxy group, such as N- methylaminoethyl (meth) acrylate.
  • monomers other than (meth) acrylic acid ester monomers include olefins such as ethylene and norbornene, vinyl acetate, and styrene.
  • the (meth) acrylic acid ester monomer is an alkyl (meth) acrylate, the alkyl group preferably has 1 to 18 carbon atoms.
  • (meth) acrylic acid means both acrylic acid and methacrylic acid. The same applies to other similar terms.
  • the (meth) acrylic acid ester polymer (A) is directly contained in the pressure-sensitive adhesive composition.
  • at least a part thereof may be contained as a crosslinked product by performing a crosslinking reaction with a crosslinking agent.
  • the (meth) acrylic acid ester polymer (A) preferably has a reactive functional group that reacts with the crosslinking agent.
  • the type of the reactive functional group is not particularly limited, and may be appropriately determined based on the type of the crosslinking agent.
  • examples of the reactive functional group of the (meth) acrylic acid ester polymer (A) include a hydroxy group, a carboxyl group, and an amino group. These highly reactive hydroxy groups are preferred.
  • examples of the reactive functional group of the (meth) acrylic acid ester polymer (A) include a carboxyl group, an amino group, an amide group, etc. These highly reactive carboxyl groups are preferred.
  • the method for introducing the reactive functional group into the (meth) acrylic acid ester polymer (A) is not particularly limited.
  • the (meth) acrylic acid ester polymer (A) using a monomer having a reactive functional group is used.
  • a constitutional unit based on a monomer having a reactive functional group is contained in the polymer skeleton.
  • a carboxyl group is introduced into the (meth) acrylic acid ester polymer (A)
  • a (meth) acrylic acid ester polymer (A) is formed using a monomer having a carboxyl group such as (meth) acrylic acid. do it.
  • the (meth) acrylic acid ester polymer (A) When the (meth) acrylic acid ester polymer (A) has a reactive functional group, it accounts for the total mass of the (meth) acrylic acid ester polymer (A) from the viewpoint of making the degree of crosslinking a good range.
  • the proportion of the mass of the structural portion derived from the monomer having a reactive functional group is preferably about 1 to 20% by mass, and more preferably 2 to 10% by mass.
  • the weight average molecular weight (Mw) of the (meth) acrylic acid ester polymer (A) is preferably 10,000 to 2,000,000, and more preferably 100,000 to 1,500,000 from the viewpoint of film forming properties at the time of coating. preferable.
  • the weight average molecular weights of the (meth) acrylic acid ester polymer (A) and the (meth) acrylic acid ester polymers (B1) and (B3) described later are gel permeation chromatography (GPC). It is a value in terms of standard polystyrene measured by the method, and details of the measuring method are shown in the examples described later.
  • the glass transition temperature Tg of the (meth) acrylic acid ester polymer (A) is preferably in the range of ⁇ 70 ° C. to 30 ° C., more preferably in the range of ⁇ 60 ° C. to 20 ° C.
  • the glass transition temperature can be calculated from the Fox equation.
  • the active energy ray-curable pressure-sensitive adhesive composition has an active energy ray-curable compound (B2) and an active energy ray-curable group introduced into the side chain ( It is preferable that at least one of the (meth) acrylic acid ester polymer (B3) is contained.
  • the active energy ray-curable pressure-sensitive adhesive composition is composed of the active energy ray-curable compound (B2) and the (meth) acrylic acid ester polymer (B3) in which an active energy ray-curable group is introduced into the side chain.
  • the active energy ray-curable pressure-sensitive adhesive composition may further contain a (meth) acrylic acid ester polymer (B1) having no active energy ray curability.
  • (1-2-1) (Meth) acrylic acid ester polymer having no active energy ray curability (B1)
  • the adhesive composition which forms the adhesive layer in this embodiment contains the (meth) acrylic acid ester polymer (B1) which does not have active energy ray curability
  • the said (meth) acrylic acid ester polymer (B1) ) May be contained in the pressure-sensitive adhesive composition as it is, or at least a part thereof may be contained as a crosslinked product by performing a crosslinking reaction with a crosslinking agent described later.
  • (meth) acrylic acid ester polymer (B1) the same thing as the (meth) acrylic acid ester polymer (A) mentioned above regarding the non-curable adhesive composition can be used.
  • the active energy ray curable compound (B2) is a compound having an active energy ray curable group and polymerized when irradiated with active energy rays such as ultraviolet rays and electron beams.
  • the active energy ray-curable group possessed by the active energy ray-curable compound (B2) is, for example, a group containing an active energy ray-curable carbon-carbon double bond, and specifically includes a (meth) acryloyl group, vinyl Examples include groups.
  • Examples of the active energy ray-curable compound (B2) are not particularly limited as long as the active energy ray-curable group has the above-mentioned active energy ray-curable group.
  • low molecular weight compounds monofunctional and polyfunctional monomers and Oligomer
  • Specific examples of the low molecular weight active energy ray-curable compound (B2) include trimethylolpropane tri (meth) acrylate, tetramethylolmethanetetra (meth) acrylate, pentaerythritol tri (meth) acrylate, and dipentaerythritol monohydroxypenta.
  • the active energy ray-curable compound (B2) usually has a molecular weight of 100 to 30,000, preferably about 300 to 10,000.
  • the content of the active energy ray-curable compound (B2) in the active energy ray-curable adhesive composition and the content ratio with other components are not particularly limited, but the active energy ray-curable adhesive composition is active energy.
  • the active energy ray-curable adhesive composition is active energy.
  • the active energy ray curable compound (B2) is the above (meth) acrylic acid.
  • the amount is preferably 10 to 400 parts by mass, more preferably about 30 to 350 parts by mass with respect to 100 parts by mass of the ester polymer (B1).
  • the active energy ray-curable compound (B2) when it contains the active energy ray-curable compound (B2) and the (meth) acrylic acid ester polymer (B3) in which an active energy ray-curable group is introduced in the side chain described later, )
  • the content of the active energy ray-curable compound (B2) is preferably in the above range with respect to 100 parts by mass of the acrylic ester polymer (B3).
  • the active energy ray-curable pressure-sensitive adhesive composition has the active energy ray-curable compound (B2), the (meth) acrylic acid ester polymer (B1), and the active energy ray-curable group introduced into the side chain.
  • the total amount of the (meth) acrylic acid ester polymer (B1) and the (meth) acrylic acid ester polymer (B3) is 100 parts by mass.
  • the content of the active energy ray-curable compound (B2) is preferably in the above range.
  • (1-2-3) (Meth) acrylic acid ester polymer (B3) having an active energy ray-curable group introduced in the side chain
  • the active energy ray-curable pressure-sensitive adhesive composition in the present embodiment contains a (meth) acrylic acid ester polymer (B3) having an active energy ray-curable group introduced in the side chain, such (meth) acrylic acid ester
  • the polymer (B3) may be contained in the pressure-sensitive adhesive composition as it is, or at least a part thereof may be contained as a crosslinked product by performing a crosslinking reaction with a crosslinking agent described later.
  • the main skeleton of the (meth) acrylic acid ester polymer (B3) in which the active energy ray-curable group is introduced into the side chain is not particularly limited, and is the same as that of the aforementioned (meth) acrylic acid ester polymer (B1). Are illustrated.
  • the active energy ray-curable group introduced into the side chain of the (meth) acrylate polymer (B3) is, for example, a group containing an active energy ray-curable carbon-carbon double bond.
  • a meth) acryloyl group etc. can be illustrated.
  • the active energy ray-curable group may be bonded to the (meth) acrylic acid ester polymer (B3) via an alkylene group, an alkyleneoxy group, a polyalkyleneoxy group, or the like.
  • the (meth) acrylic acid ester polymer (B3) in which an active energy ray-curable group is introduced into the side chain contains, for example, a functional group such as a hydroxy group, a carboxyl group, an amino group, a substituted amino group, and an epoxy group.
  • a (meth) acrylic acid ester polymer is reacted with a substituent that reacts with the functional group and a curable group-containing compound having 1 to 5 active energy ray-curable carbon-carbon double bonds per molecule. Obtained.
  • Such a (meth) acrylic acid ester polymer includes a (meth) acrylic acid ester monomer or a derivative thereof having a functional group such as a hydroxy group, a carboxyl group, an amino group, a substituted amino group, and an epoxy group, and the component (B1) described above. It can be obtained by copolymerizing with a monomer that constitutes.
  • curable group-containing compound examples include (meth) acryloyloxyethyl isocyanate, meta-isopropenyl- ⁇ , ⁇ -dimethylbenzyl isocyanate, (meth) acryloyl isocyanate, allyl isocyanate, glycidyl (meth) acrylate, (meth) Acrylic acid etc. are mentioned, These can be used individually by 1 type or in combination of 2 or more types.
  • the active energy ray hardening group was introduce
  • the kind of the reactive functional group is not particularly limited, and the (meth) acrylic acid ester polymer (B1) described above (and the (meth) acrylic acid ester polymer (A) described above with respect to the non-curable pressure-sensitive adhesive composition) and The same thing can be illustrated.
  • the weight average molecular weight (Mw) of the (meth) acrylic acid ester polymer (B3) having an active energy ray-curable group introduced in the side chain is preferably 100,000 to 2,000,000, and 300,000 to 1,500,000. More preferably.
  • the glass transition temperature (Tg) of the (meth) acrylic acid ester polymer (B3) is preferably in the range of ⁇ 70 to 30 ° C., more preferably in the range of ⁇ 60 to 20 ° C.
  • the glass transition temperature (Tg) of the (meth) acrylic acid ester polymer (B3) refers to that of the (meth) acrylic acid ester polymer before being reacted with the curable group-containing compound.
  • thermosetting pressure-sensitive adhesive composition examples include those containing an epoxy resin, a phenol resin, and the like.
  • the adhesive composition forming the adhesive layer in this embodiment may contain a crosslinking agent capable of reacting with the polymer contained in the above-mentioned adhesive composition.
  • the pressure-sensitive adhesive layer in this embodiment comprises a polymer ((meth) acrylic acid ester polymer (A), (B1), (B3), etc.) contained in the pressure-sensitive adhesive composition and a crosslinking agent. Contains a cross-linked product obtained by a cross-linking reaction.
  • crosslinking agent examples include polyimine compounds such as polyisocyanate compounds, epoxy compounds, metal chelate compounds, and aziridine compounds, melamine resins, urea resins, dialdehydes, methylol polymers, metal alkoxides, metal salts, and the like. 1 type can be used individually or in combination of 2 or more types. Among these, an epoxy compound or a polyisocyanate compound is preferable because it is easy to control the crosslinking reaction.
  • a polyisocyanate compound is a compound having two or more isocyanate groups per molecule.
  • aromatic polyisocyanates such as tolylene diisocyanate, diphenylmethane diisocyanate, xylylene diisocyanate, aliphatic polyisocyanates such as hexamethylene diisocyanate, alicyclic polyisocyanates such as isophorone diisocyanate, hydrogenated diphenylmethane diisocyanate, and the like
  • epoxy compound examples include 1,3-bis (N, N′-diglycidylaminomethyl) cyclohexane, N, N, N ′, N′-tetraglycidyl-m-xylylenediamine, ethylene glycol diglycidyl ether. 1,6-hexanediol diglycidyl ether, trimethylolpropane diglycidyl ether, diglycidylaniline, diglycidylamine and the like.
  • the content of the crosslinking agent in the pressure-sensitive adhesive composition that forms the pressure-sensitive adhesive layer is the polymer contained in the pressure-sensitive adhesive composition (for example, (meth) acrylic acid ester polymers (A), (B1) and (B3)). Is preferably 0.01 to 50 parts by mass, more preferably 0.02 to 10 parts by mass, and more preferably 0.03 to 5 parts by mass with respect to 100 parts by mass of the total amount of Part is more preferable, and 0.08 to 0.5 part by mass is particularly preferable.
  • the pressure-sensitive adhesive composition forming the pressure-sensitive adhesive layer in the present embodiment contains a crosslinking agent
  • an appropriate crosslinking accelerator may be contained depending on the type of the crosslinking agent.
  • the pressure-sensitive adhesive composition forming the pressure-sensitive adhesive layer in the present embodiment includes, in addition to the above components, a photopolymerization initiator, a photosensitizer, a crosslinking accelerator, a dye, a pigment, and the like. You may contain various additives, such as a coloring material, a flame retardant, a filler, a heat conductive agent, a tackifier, a plasticizer, and an antistatic agent.
  • the pressure-sensitive adhesive composition when the pressure-sensitive adhesive composition has active energy ray curability that is cured by active energy rays such as ultraviolet rays, the pressure-sensitive adhesive composition preferably contains a photopolymerization initiator.
  • photopolymerization initiators examples include photoinitiators such as benzoin compounds, acetophenone compounds, acylphosphine oxide compounds, titanocene compounds, thioxanthone compounds, and peroxide compounds, and photosensitizers such as amines and quinones.
  • 1-hydroxycyclohexyl phenyl ketone benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzyldiphenyl sulfide, tetramethylthiuram monosulfide, azobisisobutyronitrile, dibenzyl, diacetyl, ⁇ -chloranthraquinone 2,4,6-trimethylbenzoyldiphenylphosphine oxide and the like, and these can be used alone or in combination of two or more.
  • ultraviolet rays When ultraviolet rays are used as energy rays, the irradiation time and irradiation amount can be reduced by blending a photopolymerization initiator.
  • an adhesive layer has an air chamber in the inside.
  • the gas in the air chamber expands due to the decompression process to be described later, whereby a pressure in the direction in which the air chamber expands is applied to the air chamber, and as a result, the adhesive force of the adhesive sheet decreases.
  • the gas contained in the air chamber is not particularly limited, but may be, for example, air or an inert gas such as nitrogen, carbon dioxide, or argon.
  • the shape of the air chamber is typically substantially spherical from the viewpoint of ease of formation, but is not limited thereto.
  • the average diameter of the air chamber is not particularly limited, but is preferably, for example, 0.1 to 500 ⁇ m, more preferably 1 to 100 ⁇ m, and particularly preferably 10 to 50 ⁇ m.
  • the volume ratio of the air chamber in the pressure-sensitive adhesive layer is, for example, preferably 0.5 to 20.0%, more preferably 1.0 to 10.0%, and more preferably 1.5 to 5%. Particularly preferred is 0.0%.
  • the pressure-sensitive adhesive sheet can easily maintain a desired adhesive force before decompression, and the adherend can be more securely fixed. After pressure reduction, the effect of reducing the adhesive force due to the expansion of the gas in the air chamber becomes more excellent, and the adhesive sheet and the adherend are more easily separated.
  • the average diameter of the air chamber is, for example, photographed the pressure-sensitive adhesive layer with a digital microscope or a scanning electron microscope (SEM), and the air chamber having a diameter of 0.1 ⁇ m or more, preferably about 10 or more air chambers, It can obtain
  • the average diameter is calculated in terms of a spherical air chamber having an equivalent volume.
  • the volume ratio of the air chambers in the pressure-sensitive adhesive layer is obtained by photographing the pressure-sensitive adhesive layer with a digital microscope or SEM and measuring the area ratio of the air chamber portion in the predetermined range, preferably about five or more photographed images. From the result of measuring the area ratio of the air chamber portions, the volume ratio of the air chamber can be obtained.
  • the method for forming the air chamber in the pressure-sensitive adhesive layer is not particularly limited, and a known method can be appropriately employed.
  • a method in which the pressure-sensitive adhesive composition for forming the pressure-sensitive adhesive layer is vigorously stirred and a gas such as air is intentionally mixed a method in which gas is injected (bubbled) into the pressure-sensitive adhesive composition, a hollow filler (a gas in the interior) And the like, and a method of forming an air chamber by foaming after forming a pressure-sensitive adhesive layer by blending a thermal foaming agent or the like into the pressure-sensitive adhesive composition.
  • a surfactant may be added to the pressure-sensitive adhesive composition from the viewpoint of easy formation of the air chamber by mixing and injection of gas and the stability of the formed air chamber.
  • surfactants include ionic surfactants, hydrocarbon surfactants, silicone surfactants, and fluorine surfactants.
  • the thickness of the pressure-sensitive adhesive layer in this embodiment is preferably 5 to 100 ⁇ m, particularly preferably 10 to 50 ⁇ m, and 15 to 30 ⁇ m. More preferably. It is preferable that the pressure-sensitive adhesive layer has a thickness of 5 ⁇ m or more because more space can be secured during decompression. It is preferable for the thickness of the pressure-sensitive adhesive layer to be 100 ⁇ m or less because the film thickness accuracy during application can be ensured.
  • the adhesive strength of the adhesive sheet is preferably 0.5 to 50 N / 25 mm, more preferably 2 to 40 N / 25 mm, and particularly preferably 5 to 30 N / 25 mm. .
  • the adherend can be reliably fixed. For example, it is very useful for temporarily fixing the adherend in the processing step of the adherend.
  • the adhesive force here does not perform the pressure reduction process mentioned later (When the adhesive composition has active energy ray curable property or thermosetting property, irradiation and heating of the active energy ray are not further performed).
  • a silicon mirror wafer is used as an adherend, and the adhesive sheet is bonded to the mirror surface, and the adhesive strength (N / 25 mm) measured by the 180 ° peeling method according to JIS Z0237: 2009 is used.
  • the adhesive strength reduction rate of the adhesive sheet is preferably 5% or more, more preferably 10% or more, and particularly preferably 30% or more. When the adhesive strength of the adhesive sheet is within the above range, in this embodiment, the adhesive sheet and the adherend are more easily separated.
  • the adhesive force decreasing rate here is before performing the pressure reduction process mentioned later (When the adhesive composition has active energy ray curable or thermosetting, after irradiation or heating of active energy rays)
  • the adhesive strength is measured as described above, and is calculated by the following formula based on the obtained value.
  • Adhesive strength reduction rate (%) (adhesive strength before decompression ⁇ adhesive strength after decompression) / (adhesive strength after decompression) ⁇ 100
  • the irradiation or heating of the active energy ray when the pressure-sensitive adhesive composition has active energy ray curable property or thermosetting property may be before or after the decompression treatment, Even in this case, the adhesive strength reduction rate is calculated by the above formula.
  • the lower limit of the stress relaxation rate of the pressure-sensitive adhesive layer is preferably 30% or more, particularly preferably 45% or more, and 60% or more. Is more preferable.
  • the upper limit of the stress relaxation rate of the pressure-sensitive adhesive layer is preferably 100% or less, particularly preferably 90% or less, and further preferably 80% or less.
  • the stress relaxation rate of the pressure-sensitive adhesive layer here is not subjected to a decompression treatment described later (if the pressure-sensitive adhesive composition has active energy ray curable or thermosetting properties, irradiation or heating with active energy rays is further performed.
  • the stress relaxation rate after being stretched by 300% in a tensile test and held for 300 seconds. Specifically, the tensile test was performed at a speed of 200 mm / min with an adhesive formed into a thickness of 500 ⁇ m, a width of 15 mm, and a length of 55 mm (of which the measurement range is 25 mm) in an environment of 23 ° C. and 50% RH. It is assumed that the stretching is performed by 300%.
  • the lower limit of the breaking elongation of the pressure-sensitive adhesive layer is preferably 200% or more, particularly preferably 500% or more, and preferably 1000% or more. Is more preferable.
  • the upper limit of the elongation at break of the pressure-sensitive adhesive layer is preferably 5000% or less, particularly preferably 4000% or less, and further preferably 3000% or less.
  • the pressure-sensitive adhesive layer was measured as a single pressure-sensitive adhesive layer without a substrate or the like, and specifically, molded into a thickness of 500 ⁇ m, a width of 15 mm, and a length of 55 mm (of which the measurement range is 25 mm). The obtained adhesive is stretched at a speed of 200 mm / min in an environment of 23 ° C. and 50% RH.
  • the lower limit of the gel fraction of the pressure-sensitive adhesive layer is preferably 1% or more, particularly preferably 2% or more, and 3% or more. Is more preferable.
  • the upper limit of the gel fraction of the pressure-sensitive adhesive layer is preferably 80% or less, particularly preferably 70% or less, and further preferably 60% or less.
  • the lower limit of the gel fraction of the pressure-sensitive adhesive layer is 1% or more, stability as a pressure-sensitive adhesive sheet can be ensured by reaction between the pressure-sensitive adhesives due to crosslinking.
  • the upper limit of the gel fraction of the pressure-sensitive adhesive layer is 80% or less, it is easy to impart tack to the pressure-sensitive adhesive sheet, and good temporary fixability can be obtained.
  • the gel fraction of an adhesive layer here is not performing the pressure reduction process mentioned later (When an adhesive composition has active energy ray sclerosis
  • the pressure-sensitive adhesive sheet according to this embodiment may include a base material in addition to the pressure-sensitive adhesive layer.
  • the base material is not particularly limited as long as the pressure-sensitive adhesive sheet can appropriately function in a desired process such as an adherend processing process.
  • a paper base material, a resin film or sheet, a paper base The base material etc. which laminated the material with resin are mentioned, According to the use of the adhesive sheet of 1 aspect of this embodiment, it can select suitably.
  • the film is composed of a resin-based material as a main material because of its advantage against the pressure reduction effect.
  • Such films include ethylene-copolymer films such as ethylene-vinyl acetate copolymer films, ethylene- (meth) acrylic acid copolymer films, and ethylene- (meth) acrylic acid ester copolymer films; low density Polyethylene film such as polyethylene (LDPE) film, linear low density polyethylene (LLDPE) film, high density polyethylene (HDPE) film, polypropylene film, polybutene film, polybutadiene film, polymethylpentene film, ethylene-norbornene copolymer film, Polyolefin film such as norbornene resin film; Polyvinyl chloride film such as polyvinyl chloride film and vinyl chloride copolymer film; Polyethylene terephthalate film, Polybutylene tele Polyester film of tallate films; polyurethane film; polyimide film; polystyrene films; polycarbonate films; and fluorine resin film. Further, modified films such as these crosslinked films and ionomer films are also used
  • the film constituting the base material preferably includes at least one of an ethylene copolymer film and a polyolefin film. It is easy to control the mechanical characteristics of an ethylene copolymer film in a wide range by changing the copolymerization ratio. For this reason, the base material provided with the ethylene-based copolymer film easily satisfies the mechanical properties required as the base material of the pressure-sensitive adhesive sheet according to this embodiment. Moreover, since the ethylene copolymer film has relatively high adhesion to the pressure-sensitive adhesive layer, peeling at the interface between the base material and the pressure-sensitive adhesive layer hardly occurs when used as a pressure-sensitive adhesive sheet.
  • the base material used in the present embodiment contains various additives such as pigments, dyes, flame retardants, plasticizers, antistatic agents, lubricants, fillers, etc., in the film mainly composed of the above-mentioned resin-based material. May be.
  • the pigment include titanium dioxide and carbon black.
  • the filler include organic materials such as melamine resin, inorganic materials such as fumed silica, and metal materials such as nickel particles. The content of such an additive is not particularly limited, but should be within a range where the substrate exhibits a desired function and does not lose smoothness and flexibility.
  • the substrate is preferably permeable to ultraviolet rays.
  • the base material has the transparency of an electron beam.
  • the adherend has energy ray permeability and the energy beam is irradiated from the adherend side, the substrate does not need to have energy ray permeability.
  • a component having one or more kinds selected from the group consisting of a carboxyl group and its ions and salts is provided on the surface of the substrate on the side of the pressure-sensitive adhesive layer (hereinafter also referred to as “substrate-coated surface”). Is preferably present.
  • substrate-coated surface a component having one or more kinds selected from the group consisting of a carboxyl group and its ions and salts.
  • the base material itself is an ethylene- (meth) acrylic acid copolymer film, an ionomer resin film, etc., and the resin constituting the base material is selected from the group consisting of carboxyl groups, ions and salts thereof. Or you may have 2 or more types.
  • the substrate is, for example, a polyolefin film, and the substrate-adhered surface side is subjected to corona treatment or a primer layer is provided. May be.
  • Various coating films may be provided on the surface of the substrate opposite to the substrate deposition surface.
  • the thickness of the substrate is not limited as long as the pressure-sensitive adhesive sheet can function properly in a desired process, but it is preferably 5 to 1000 ⁇ m, more preferably 10 to 500 ⁇ m, and still more preferably 12 to 12 from the viewpoint of handleability and economy.
  • the thickness is 250 ⁇ m, more preferably 15 to 150 ⁇ m.
  • the release sheet is laminated on the adhesive surface of the adhesive layer for the purpose of protecting the adhesive layer until the adhesive layer is applied to the adherend. It may be.
  • the configuration of the release sheet is arbitrary, and examples include a release film of a plastic film with a release agent.
  • Specific examples of the plastic film include polyester films such as polyethylene terephthalate, polybutylene terephthalate, and polyethylene naphthalate, and polyolefin films such as polypropylene and polyethylene.
  • the release agent silicone-based, fluorine-based, long-chain alkyl-based, and the like can be used, and among these, a silicone-based material that is inexpensive and provides stable performance is preferable.
  • the thickness of the release sheet is not particularly limited, but is usually about 20 to 250 ⁇ m.
  • the manufacturing method of an adhesive sheet is a method which can form the adhesive layer formed from the above-mentioned adhesive composition, and can form an air chamber inside an adhesive layer. If there is, the detailed method is not particularly limited.
  • a method for producing a pressure-sensitive adhesive sheet comprising a base material and a pressure-sensitive adhesive layer it is only necessary that a pressure-sensitive adhesive layer formed from the above-mentioned pressure-sensitive adhesive composition can be laminated on one surface of the base material.
  • a coating composition containing the above-mentioned pressure-sensitive adhesive composition and optionally further containing a solvent or a dispersion medium is prepared.
  • the coating composition may be vigorously stirred and a gas such as air may be intentionally mixed, or a gas may be injected (bubbled) into the coating composition.
  • a gas such as air
  • a gas may be injected (bubbled) into the coating composition.
  • the coating composition thus obtained is applied on one surface of the substrate by a die coater, curtain coater, spray coater, slit coater, knife coater, etc. to form a coating film, and the coating film
  • a pressure-sensitive adhesive sheet comprising a pressure-sensitive adhesive layer and a substrate can be formed.
  • the release sheet in this laminate may be peeled off as a process material, or the adhesive layer may be protected until being attached to an adherend such as an electronic member or an optical member.
  • the properties of the coating composition are not particularly limited as long as it can be applied, and may contain a component for forming the pressure-sensitive adhesive layer as a solute or a dispersoid.
  • the coating composition contains a thermal foaming agent
  • the thermal foaming agent is foamed by changing the drying conditions (temperature, time, etc.) or by separately providing a heat treatment.
  • a chamber may be formed.
  • the coating composition contains a cross-linking agent, (meth) acrylic acid in the coating film can be obtained by changing the drying conditions (temperature, time, etc.) or by separately providing a heat treatment.
  • crosslinking refers to a reaction performed before sticking the pressure-sensitive adhesive sheet to the adherend, and before sticking to the adherend is, for example, the pressure-sensitive adhesive described above. A step of forming a layer may be mentioned. Therefore, “crosslinking” of the pressure-sensitive adhesive is clearly distinguished from “curing” described later.
  • a coating film is formed on the release surface of the above-described release sheet to form a coating film, which is dried to form a laminate composed of the pressure-sensitive adhesive layer and the release sheet.
  • a laminate of the pressure-sensitive adhesive sheet and the release sheet may be obtained by forming a body and attaching the surface of the pressure-sensitive adhesive layer of the laminate opposite to the surface on the release sheet side to the substrate.
  • the release sheet in this laminate may be peeled off as a process material, or the adhesive layer may be protected until being attached to an adherend such as an electronic member or an optical member.
  • the composition for coating on the release surface of the aforementioned release sheet Is applied to form a coating film, which is dried to form a laminate composed of a pressure-sensitive adhesive layer and a release sheet, and the surface on the side opposite to the release sheet side of the pressure-sensitive adhesive layer of this laminate is It can affix on the peeling surface of this release sheet, and can obtain the laminated body which consists of a release sheet / adhesive sheet / release sheet.
  • the release sheet in this laminate may be peeled off as a process material, or the adhesive layer may be protected until being attached to an adherend such as an electronic member or an optical member.
  • Examples of the workpiece W to be subjected to the peeling method according to this embodiment include electronic members such as a semiconductor wafer, a semiconductor package, a multilayer substrate, a ceramic green sheet laminate, a batch sealing module; a liquid crystal display member, and an organic EL display member. And optical members such as an optical filter, a polarizing plate, and a retardation plate.
  • the attachment of the workpiece W and the pressure-sensitive adhesive sheet 1 may be performed under atmospheric pressure, or may be performed in a chamber in which the atmospheric pressure is controlled by the pressure control device 10 described later.
  • the atmospheric pressure in which the sticking process is performed or the atmospheric pressure in the chamber corresponds to the pressure of the gas in the air chamber 3 in the subsequent process, and the sticking process is performed after appropriately adjusting the atmospheric pressure. It becomes easy to control the amount of gas expansion in the decompression process.
  • work W stuck on the adhesive sheet 1 by the sticking process can be attached
  • processing steps include a back grinding process, a circuit forming process, a dicing process, a die sort process, and the like if the work W is a semiconductor wafer, and a laminating process and a transfer process if the work W is a display device component. Etc.
  • the workpiece W is processed into a workpiece W ′.
  • the adhesive sheet 1 is peeled from the workpiece W as described later after the processing step of the workpiece W, it can be said that it is used for temporarily fixing the workpiece W during the processing step.
  • the adhesive sheet 1 in a state where the workpiece W ′ is adhered is placed in the chamber of the pressure control device 10 (FIG. 2C).
  • the pressure-sensitive adhesive sheet 1 in a state where the workpiece W ′ is adhered is placed so that the workpiece W ′ is on the lower side of the pressure-sensitive adhesive sheet 1. It is preferable to place in the chamber.
  • the workpiece W ′ can be expanded when the air chamber 3 can be expanded in the decompression process. It may be placed in the chamber so that is on the upper side of the adhesive sheet 1.
  • the pressure reduction treatment is preferably lower than the atmospheric pressure of the pasting environment, more preferably lower so that the atmospheric pressure in the chamber has a difference of 10 kPa or more than the atmospheric pressure of the pasting environment.
  • the difference is more preferably 30 kPa or more, still more preferably 50 kPa or more, further preferably 80 kPa or more, and particularly preferably 90 kPa or more.
  • the lower limit value of the pressure in the chamber is not particularly limited, but is usually 10 ⁇ 7 Pa or more, preferably 10 ⁇ 5 Pa or more, more preferably 10 ⁇ 1 Pa or more, and even more, from a technical viewpoint.
  • it is 10 Pa or more, More preferably, it is 100 Pa or more, Especially preferably, it is 1000 Pa or more.
  • the pressure-sensitive adhesive layer 2 is relatively soft as a result of the decompression process, a convex portion is formed on a part of the pressure-sensitive adhesive surface P following the expansion of the air chamber 3 as shown in FIG. Arise.
  • the plurality of air chambers 3 may communicate with each other to form a larger air chamber 3. It is preferable to form a larger air chamber 3 because the expansion effect due to the reduced pressure becomes more remarkable.
  • the air chamber 3 in the vicinity of the adhesive surface P expands, it may be exposed on the adhesive surface P, and the portion that was the air chamber 3 may become a concave portion of the adhesive surface P. As a result, irregularities are formed on the adhesive surface P.
  • the adhesive area between the pressure-sensitive adhesive layer 2 and the workpiece W ′ decreases, and the adhesive force of the pressure-sensitive adhesive sheet 1 to the workpiece W ′ decreases.
  • the adhesive layer 2 peels a part or all from the workpiece W 'from the location (FIG. 2 ( e)).
  • the pressure-sensitive adhesive layer 2 when the pressure-sensitive adhesive layer 2 is relatively hard, the processed product of the pressure-sensitive adhesive sheet 1 with almost no expansion of the air chamber 3 and deformation of the pressure-sensitive adhesive surface P as shown in FIG. In some cases, the adhesive strength to W ′ decreases, and the adhesive layer 2 peels from the workpiece W ′ as shown in FIG. This is considered to be because the force that pushes up the base material in the longitudinal direction of the adhesive is prioritized over the expansion of the adhesive because the adhesive is relatively hard.
  • the pressure-sensitive adhesive sheet 1 and the workpiece W ′ can be easily peeled off by decreasing the adhesive force of the pressure-sensitive adhesive layer 2 to the workpiece W ′.
  • the pressure-sensitive adhesive sheet 1 and the workpiece W ′ can be peeled as they are in the state shown in FIG. 2E.
  • the pressure-sensitive adhesive sheet 1 is placed in the chamber so that the workpiece W ′ is on the upper side of the pressure-sensitive adhesive sheet 1.
  • the pressure-sensitive adhesive sheet 1 and the workpiece W ′ are peeled off by the weight of the workpiece W ′. You can also.
  • the pressure-sensitive adhesive composition forming the pressure-sensitive adhesive layer 2 has active energy ray curable or thermosetting property, the active energy ray irradiation or after the above-described processing step and before or after the decompression treatment. It is preferable to cure the pressure-sensitive adhesive layer 2 by heating.
  • the pressure-sensitive adhesive layer 2 is cured before the pressure reduction treatment, the pressure-sensitive adhesive layer 2 is relatively hard at the stage of the pressure reduction treatment. The pressure-sensitive adhesive layer 2, the workpiece W ′, and the adhesive force can be reduced with almost no unevenness formation.
  • the pressure-sensitive adhesive layer 2 when the pressure-sensitive adhesive layer 2 is cured after the pressure reduction treatment, the pressure-sensitive adhesive layer 2 is relatively soft at the stage of the pressure reduction treatment, so that the expansion of the air chamber 3 and the formation of irregularities on the pressure-sensitive adhesive surface P (FIG. 2D) ), The pressure-sensitive adhesive force can be further reduced by curing the pressure-sensitive adhesive layer 2, and the pressure-sensitive adhesive layer 2 and the workpiece W ′ can be easily separated from each other.
  • “curing” of the pressure-sensitive adhesive refers to a reaction performed after the pressure-sensitive adhesive sheet 1 is adhered to an adherend (work W, workpiece W ′). Therefore, for example, it is clearly distinguished from the above-mentioned “crosslinking” of the pressure-sensitive adhesive.
  • examples of the active energy ray for curing the pressure-sensitive adhesive composition include ionizing radiation, that is, ultraviolet rays, X-rays, and electron beams. Among these, ultraviolet rays that are relatively easy to introduce irradiation equipment are preferable.
  • near ultraviolet rays including ultraviolet rays having a wavelength of about 200 to 380 nm may be used for ease of handling.
  • the amount of light may be appropriately selected according to the type of active energy ray-curable group possessed by the active energy ray-curable pressure-sensitive adhesive composition and the thickness of the pressure-sensitive adhesive layer 2, and is usually about 50 to 1500 mJ / cm 2 . 200 to 1000 mJ / cm 2 is preferable, and 300 to 800 mJ / cm 2 is more preferable.
  • the ultraviolet illumination is usually 50 ⁇ 1500mW / cm 2 or so, preferably 200 ⁇ 1000mW / cm 2, more preferably 300 ⁇ 800mW / cm 2.
  • the ultraviolet light source is not particularly limited, and for example, an electrodeless lamp, a high-pressure mercury lamp, a metal halide lamp, a UV-LED, or the like is used.
  • the acceleration voltage is appropriately selected according to the type of active energy ray-curable group possessed by the active energy ray-curable adhesive composition and the thickness of the adhesive layer 2. Usually, the acceleration voltage is preferably about 10 to 1000 kV.
  • the irradiation dose may be set within a range where the active energy ray-curable pressure-sensitive adhesive composition is appropriately cured, and is usually selected within a range of 10 to 1000 krad.
  • the electron beam source is not particularly limited.
  • various electron beam accelerators such as a cockcroft Walton type, a bandegraph type, a resonant transformer type, an insulated core transformer type, a linear type, a dynamitron type, and a high frequency type may be used. it can.
  • these active energy rays may be irradiated from the surface opposite to the pressure-sensitive adhesive surface P (the surface on which the workpiece W ′ is adhered) in the pressure-sensitive adhesive sheet 1. preferable.
  • the pressure-sensitive adhesive composition has thermosetting properties
  • a heating means for curing the pressure-sensitive adhesive composition for example, an appropriate means such as a hot plate, a hot air dryer, or a near infrared lamp can be adopted. It can.
  • the heating conditions are appropriately set depending on the heating temperature required for the thermosetting of the pressure-sensitive adhesive layer 2, the desired peelability, the heat resistance of the workpiece W and the workpiece W ', the heating means, and the like.
  • As general heating conditions for example, when a hot plate is used, a temperature of 80 to 250 ° C., a heating time of 5 seconds to 60 seconds, and the like are exemplified.
  • the pressure-sensitive adhesive layer 2 of the pressure-sensitive adhesive sheet 1 has an air chamber 3 therein, and a decompression process for expanding the gas in the air chamber 3, The adhesive force to the adherend of the adhesive sheet 1 is reduced.
  • the adhesive force can be reduced at a desired timing by a novel mechanism of expanding the gas by the decompression process, thereby facilitating the peeling between the adhesive sheet and the adherend. Can do.
  • the adhesive force of the pressure-sensitive adhesive layer 2 is reduced using only active energy ray curable or thermosetting, the selection of materials is limited because the curing reaction (that is, chemical reaction) is sufficiently advanced. End up.
  • the adhesive force can be reduced by the expansion of the gas due to the decompression process, so that the active energy ray curable property or thermosetting property is not used at all or only partially used. Therefore, the freedom degree of the material which comprises the adhesive layer 2 can be made large.
  • the adhesive strength of the adhesive layer 2 decreases.
  • thermosetting property is not used at all or only partially used. Even if a heating process is included in the workpiece, the workpiece W can be sufficiently temporarily fixed.
  • another layer may be interposed between the base material 4 and the pressure-sensitive adhesive layer 2 in the pressure-sensitive adhesive sheet 1.
  • the pressure-sensitive adhesive sheet may be a double-sided pressure-sensitive adhesive sheet comprising only a pressure-sensitive adhesive layer without a base material.
  • a method of peeling a double-sided pressure-sensitive adhesive sheet having a first pressure-sensitive adhesive surface and a second pressure-sensitive adhesive surface, and a first adherend adhered to the first pressure-sensitive adhesive surface can do.
  • a second adherend may be attached to the second adhesive surface.
  • an air chamber is formed inside the pressure-sensitive adhesive layer.
  • the gas in the air chamber expands, and the first adherend
  • the first adherend and the pressure-sensitive adhesive sheet can be peeled off.
  • the pressure-sensitive adhesive prepared in (1) above was applied to the release-treated surface of a release sheet (product of Lintec Co., Ltd., product name “SP-PET381031”, thickness 38 ⁇ m, polyethylene terephthalate film laminated with a silicone release agent). 1) was applied with an applicator and dried at 100 ° C. for 1 minute to form an adhesive layer. The thickness of the pressure-sensitive adhesive layer after drying was 25 ⁇ m. A polyethylene terephthalate film (manufactured by Toray Industries, Inc., product name “Lumirror T-60”, thickness 50 ⁇ m) is bonded to the obtained pressure-sensitive adhesive layer, and then, under conditions of 23 ° C. and relative humidity 50%. This was seasoned for 7 days and used as an adhesive sheet.
  • a release sheet product of Lintec Co., Ltd., product name “SP-PET381031”, thickness 38 ⁇ m, polyethylene terephthalate film laminated with a silicone release agent.
  • the obtained adhesive sheet it observed with the digital microscope from the base material side, and measured the average diameter and volume ratio of the air chamber in an adhesive layer.
  • the average diameter of the air chamber was 21 ⁇ m.
  • the volume ratio of the air chamber which occupies for an adhesive layer was 2.1%.
  • Composition comprising 100 parts by mass (solid content) of the above-mentioned energy beam curable acrylic ester copolymer and energy beam curable acrylate polyfunctional monomer and oligomer as an energy beam polymerizable group-containing oligomer (Nippon Kayaku Co., Ltd.) 80 parts by mass (solid name) manufactured by company, product name “KAYARAD NKR-001” and energy ray curable urethane acrylate oligomer (manufactured by Nippon Synthetic Chemical Industry Co., Ltd., product name “UV-3210EA”, mass average molecular weight: 9000 , Glass transition temperature: ⁇ 27 ° C.) 20 parts by mass (solid content), isocyanate-based crosslinking agent (product name “Coronate L” manufactured by Tosoh Corporation), 0.1 part by mass (solid content), and photopolymerization initiator 1-Hydroxy-cyclohexyl-phenyl-ketone (Ciba Specialty Chemicals) Mixed product name
  • a pressure-sensitive adhesive sheet was produced in the same manner as in Production Example 1 except that the obtained pressure-sensitive adhesive (2) was used in place of the pressure-sensitive adhesive (1).
  • the average diameter and volume ratio of the air chamber were measured in the same manner as the adhesive sheet of Production Example 1.
  • the average diameter of the air chamber was 18 ⁇ m.
  • the volume ratio of the air chamber which occupies for an adhesive layer was 1.6%.
  • polystyrene equivalent weight average molecular weight is a standard polystyrene equivalent value measured (GPC measurement) under the following conditions using a gel permeation chromatograph (manufactured by Tosoh Corporation, product name “HLC-8020”).
  • the ultraviolet irradiation conditions are an illuminance of 700 mW / cm 2 and a light amount of 700 mJ / cm 2 in a wavelength range of 200 to 380 nm.
  • the illuminance and light amount are determined by an illuminance / light meter (product name “UV Power Pack II” manufactured by EIT). Used to measure illuminance and light intensity.
  • Example 3 The pressure-sensitive adhesive sheet obtained in Production Example 2 was cut into a size of 25 mm in length and 300 mm in width, and then a glass plate (manufactured by Nippon Sheet Glass Co., Ltd., soda lime glass) in an environment of 23 ° C. and 50% RH (relative humidity). , Length 150 mm ⁇ width 70 mm ⁇ thickness 2 mm) and allowed to stand for 24 hours in the same environment. After standing, leave it in a quartz glass chamber and use a decompressor connected to the chamber with a hose to reduce the atmospheric pressure in the chamber to 2 kPa and hold it for 10 seconds while irradiating with ultraviolet rays.
  • a decompressor connected to the chamber with a hose to reduce the atmospheric pressure in the chamber to 2 kPa and hold it for 10 seconds while irradiating with ultraviolet rays.
  • Adhesive strength reduction rate (%) (adhesive strength before decompression ⁇ adhesive strength after decompression) / (adhesive strength before decompression) ⁇ 100
  • Adhesive strength reduction rate (%) (adhesive strength before decompression ⁇ adhesive strength after decompression) / (adhesive strength before decompression) ⁇ 100
  • the adhesive force after UV curing is used instead of the adhesive force before decompression in the above formula
  • the adhesive force after decompression and UV curing is used instead of the adhesive force after decompression, and the same formula as above.
  • the adhesive strength reduction rate was calculated.
  • Example 4 the adhesive strength after UV curing is used instead of the adhesive strength before decompression in the above formula, and the adhesive strength after UV curing and after decompression is used instead of the adhesive strength after decompression, and the same formula as above.
  • the adhesive strength reduction rate was calculated. The results are shown in Table 1.
  • ⁇ Stress relaxation rate> In each production example, the substrate was changed to a heavy release sheet (product name “SP-PET 382050”, thickness 38 ⁇ m, polyethylene terephthalate film laminated with a silicone release agent) manufactured by Lintec Corporation, and dried. A substrate-less double-sided pressure-sensitive adhesive sheet sandwiched between two release sheets was prepared in the same manner as described in the production examples except that the pressure-sensitive adhesive layer was applied to have a thickness of 500 ⁇ m.
  • SP-PET 382050 thickness 38 ⁇ m, polyethylene terephthalate film laminated with a silicone release agent
  • the substrate-less double-sided pressure-sensitive adhesive sheet was allowed to stand in an atmosphere of 23 ° C. and 50% RH for 2 weeks, and then a sample having a width of 15 mm ⁇ 55 mm was cut out from the pressure-sensitive adhesive sheet in which a plurality of the pressure-sensitive adhesive layers were laminated.
  • the release sheet laminated on the surface layer was peeled off, and the sample was set in a universal tensile testing machine (manufactured by Shimadzu Corporation, Autograph AG-10kNIS) so that the sample measurement range was 15 mm wide ⁇ 25 mm long. Then, in an environment of 23 ° C.
  • the base material-less pressure-sensitive adhesive sheet used for the measurement of the stress relaxation rate was cut into a size of 80 mm ⁇ 80 mm, and the pressure-sensitive adhesive layer from which the release sheet was removed was wrapped in a polyester mesh (number of meshes: 200 mesh / inch), The mass of only the adhesive was weighed with a precision balance. The mass at this time is M1.
  • the pressure-sensitive adhesive sample was immersed in an ethyl acetate solvent at room temperature (23 ° C.) for 24 hours. Thereafter, the pressure-sensitive adhesive was taken out and air-dried for 24 hours in an environment of a temperature of 23 ° C. and 50% RH, and further dried in an oven at 80 ° C. for 12 hours. The mass of only the pressure-sensitive adhesive after drying was weighed with a precision balance. The mass at this time is M2.
  • the gel fraction (%) is represented by (M2 / M1) ⁇ 100.
  • the measurement results are shown in Table 1.

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Abstract

La présente invention concerne un procédé de délaminage de feuille adhésive (1) permettant le délaminage de la feuille adhésive (1) pourvue d'au moins une couche adhésive (2) et le délaminage de corps de fixation (W, W') fixés à la surface adhésive (P) de la couche adhésive (2), le procédé étant caractérisé en ce que : la couche adhésive (2) contient une chambre à air (3) ; et un processus de dépressurisation pour dilater un gaz à l'intérieur de la chambre à air (3) est réalisé sur la feuille adhésive (1), à laquelle sont fixés au moins les corps de fixation (W, W'), pour réduire ainsi l'adhérence de la couche adhésive (2) et délaminer la feuille adhésive (1) et les corps de fixation (W, W'). Grâce à ce procédé, l'adhérence peut être réduite à un moment souhaité au moyen d'un nouveau mécanisme d'action.
PCT/JP2018/012838 2017-03-31 2018-03-28 Procédé de délaminage d'une feuille adhésive WO2018181511A1 (fr)

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JP2020164787A (ja) * 2019-03-27 2020-10-08 住友ベークライト株式会社 粘着テープ
JP7642551B2 (ja) 2019-10-04 2025-03-10 リンテック株式会社 粘着シート
WO2021065071A1 (fr) * 2019-10-04 2021-04-08 リンテック株式会社 Feuille adhésive auto-collante
WO2021065073A1 (fr) * 2019-10-04 2021-04-08 リンテック株式会社 Feuille adhésive sensible à la pression
WO2021065070A1 (fr) * 2019-10-04 2021-04-08 リンテック株式会社 Feuille adhésive et procédé de production de feuille adhésive
WO2021065074A1 (fr) * 2019-10-04 2021-04-08 リンテック株式会社 Feuille adhésive
CN114514296B (zh) * 2019-10-04 2024-03-29 琳得科株式会社 粘合片
JP7541019B2 (ja) 2019-10-04 2024-08-27 リンテック株式会社 粘着シート
CN114514295A (zh) * 2019-10-04 2022-05-17 琳得科株式会社 粘合片
CN114514296A (zh) * 2019-10-04 2022-05-17 琳得科株式会社 粘合片
JP7541020B2 (ja) 2019-10-04 2024-08-27 リンテック株式会社 エキスパンドシート
JP7541021B2 (ja) 2019-10-04 2024-08-27 リンテック株式会社 エキスパンドシート
CN114514295B (zh) * 2019-10-04 2024-02-06 琳得科株式会社 粘合片
CN112992763A (zh) * 2019-12-13 2021-06-18 日东电工株式会社 粘合片剥离方法
JP7523216B2 (ja) 2019-12-13 2024-07-26 日東電工株式会社 粘着シート剥離方法
JP2021095449A (ja) * 2019-12-13 2021-06-24 日東電工株式会社 粘着シート剥離方法
JP2021123603A (ja) * 2020-01-31 2021-08-30 リンテック株式会社 粘着シート
JP7564625B2 (ja) 2020-01-31 2024-10-09 リンテック株式会社 仮固定粘着シート
JP7283702B2 (ja) 2020-12-08 2023-05-30 トラス カンパニー リミテッド 光硬化型粘着剤と熱発泡剤を含む再剥離可能な粘着剤及びそれを含む再剥離可能な粘着テープ
JP2022091078A (ja) * 2020-12-08 2022-06-20 トラス カンパニー リミテッド 光硬化型粘着剤と熱発泡剤を含む再剥離可能な粘着剤及びそれを含む再剥離可能な粘着テープ

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