WO2022244558A1 - 粘着シート、光学積層体、画像表示装置及び粘着シートの製造方法 - Google Patents
粘着シート、光学積層体、画像表示装置及び粘着シートの製造方法 Download PDFInfo
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- WO2022244558A1 WO2022244558A1 PCT/JP2022/017653 JP2022017653W WO2022244558A1 WO 2022244558 A1 WO2022244558 A1 WO 2022244558A1 JP 2022017653 W JP2022017653 W JP 2022017653W WO 2022244558 A1 WO2022244558 A1 WO 2022244558A1
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- adhesive sheet
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0025—Crosslinking or vulcanising agents; including accelerators
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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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
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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
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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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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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
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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
- C09J201/10—Adhesives based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing hydrolysable silane 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
- C09J7/38—Pressure-sensitive adhesives [PSA]
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
-
- 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
- C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
Definitions
- the present invention relates to an adhesive sheet, an optical laminate, an image display device, and a method for producing an adhesive sheet.
- image display devices typified by liquid crystal display devices and electroluminescence (EL) display devices (eg, organic EL display devices and inorganic EL display devices) have rapidly spread.
- These various image display devices usually have a laminated structure of an image forming layer such as a liquid crystal layer and an EL light emitting layer, and an optical laminate including an optical film and an adhesive sheet.
- the pressure-sensitive adhesive sheet is mainly used for bonding between films included in the optical layered body and bonding between the image forming layer and the optical layered body.
- the optical film are a polarizing plate, a retardation film, and a polarizing plate with a retardation film in which the polarizing plate and the retardation film are integrated.
- an object of the present invention is to provide a pressure-sensitive adhesive sheet having a sufficient storage modulus and improved durability.
- Patent Literature 1 discloses a pressure-sensitive adhesive sheet having a sea-island structure.
- Patent Document 1 discloses that the maximum length of island-like phases (domains) having a sea-island structure in a pressure-sensitive adhesive sheet is 0.3 ⁇ m to 1.0 ⁇ m. As a result of intensive studies, the present inventors newly discovered that the size of the domain affects the durability of the pressure-sensitive adhesive sheet.
- a pressure-sensitive adhesive sheet having a storage elastic modulus G′ at 25° C. of 0.4 MPa or more Provided is a pressure-sensitive adhesive sheet having a maximum domain diameter of 170 nm or less in a range of 6 ⁇ m long ⁇ 6 ⁇ m wide when a cross section of the pressure-sensitive adhesive sheet is observed with a transmission electron microscope.
- an optical laminate including the pressure-sensitive adhesive sheet described above and an optical film.
- the present invention A method for manufacturing the pressure-sensitive adhesive sheet, Applying a pressure-sensitive adhesive composition containing a (meth)acrylic polymer (A) and an isocyanate cross-linking agent to a substrate to form a coating film; drying the coating film; To provide a method for manufacturing a pressure-sensitive adhesive sheet.
- FIG. 1 is a cross-sectional view schematically showing an example of the pressure-sensitive adhesive sheet of the present invention.
- FIG. 2A is a schematic diagram for explaining an evaluation test for obtaining a stress-strain curve of an adhesive sheet.
- FIG. 2B is a schematic diagram for explaining an evaluation test for obtaining the stress-strain curve of the adhesive sheet.
- FIG. 2C is a schematic diagram for explaining an evaluation test for obtaining a stress-strain curve of an adhesive sheet.
- FIG. 2D is an enlarged view of area A in FIG. 2C.
- FIG. 3 is a graph showing an example of a stress-strain curve of an adhesive sheet.
- FIG. 4 is a schematic diagram for explaining the change in the volume of the pressure-sensitive adhesive sheet that accompanies the change in the dimensions of the optical film.
- FIG. 5 is a cross-sectional view schematically showing an example of the optical layered body of the present invention.
- FIG. 6 is a cross-sectional view schematically showing an example of the optical layered body of the present invention.
- FIG. 7 is a cross-sectional view schematically showing an example of the optical layered body of the present invention.
- FIG. 8 is a cross-sectional view schematically showing an example of the optical layered body of the present invention.
- FIG. 9 is a cross-sectional view schematically showing an example of the image display device of the present invention.
- FIG. 10 is a transmission electron microscope (TEM) image of a cross section of the adhesive sheet of Example 1.
- FIG. 11 is a TEM image of the cross section of the adhesive sheet of Example 2.
- FIG. 12 is a TEM image of the cross section of the adhesive sheet of Example 3.
- FIG. 13 is a TEM image of the cross section of the adhesive sheet of Comparative Example 1.
- FIG. 14 is a TEM image of the cross section of the adhesive sheet of Comparative Example 2.
- the pressure-sensitive adhesive sheet 1 of the present embodiment has a storage elastic modulus G' at 25°C of 0.4 MPa or more. Furthermore, when observing the cross section of the pressure-sensitive adhesive sheet 1 with a transmission electron microscope (TEM), the maximum domain diameter within the range of 6 ⁇ m long ⁇ 6 ⁇ m wide is 170 nm or less. As used herein, a domain means an island-like phase of a sea-island structure formed on a pressure-sensitive adhesive sheet. Domains are usually observed as substantially circular islands.
- TEM transmission electron microscope
- the storage elastic modulus G' of the adhesive sheet 1 at 25°C can be specified by the following method. First, a measurement sample made of the material constituting the adhesive sheet 1 is prepared. The shape of the measurement sample is disc-shaped. The measurement sample has a bottom diameter of 8 mm and a thickness of 2 mm. A sample for measurement may be obtained by punching a disc-shaped laminate from a laminate in which a plurality of pressure-sensitive adhesive sheets 1 are laminated. Next, a dynamic viscoelasticity measurement is performed on the measurement sample. For dynamic viscoelasticity measurement, for example, "ARES-G2" manufactured by TA Instruments can be used. From the results of the dynamic viscoelasticity measurement, the storage elastic modulus G' of the pressure-sensitive adhesive sheet 1 at 25°C can be specified. The conditions for the dynamic viscoelasticity measurement are as follows. ⁇ Measurement conditions Frequency: 1Hz Deformation mode: Torsion Measurement temperature: -70°C to 150°C Heating rate: 5°C/min
- the storage elastic modulus G' of the adhesive sheet 1 at 25°C is preferably 0.5 MPa or more, more preferably 0.8 MPa or more, 1.0 MPa or more, and still more preferably 1.2 MPa or more.
- the upper limit of the storage elastic modulus G' of the pressure-sensitive adhesive sheet 1 at 25°C is not particularly limited, and is, for example, 5 MPa.
- the high elastic modulus pressure-sensitive adhesive sheet 1 having a storage elastic modulus G' within the above range is suitable for suppressing changes in the dimensions of the optical film.
- the maximum diameter of the domain can be specified by the following method. First, the adhesive sheet 1 is cut and the cross section is observed with a TEM. The enlargement magnification at this time is, for example, 20,000 times. In the TEM image, a domain existing within a range of 6 ⁇ m long ⁇ 6 ⁇ m wide is identified. For each identified domain, identify the diameter (diameter of the smallest circle that can enclose the domain). Among the specified diameters, the largest value can be regarded as the maximum diameter of the domain.
- the maximum diameter of the domain is preferably 160 nm or less, more preferably 120 nm or less, even more preferably 100 nm or less, and particularly preferably 50 nm or less. In the present embodiment, it is particularly preferable that no domain is observed at a magnification of 20,000 when the cross section of the pressure-sensitive adhesive sheet 1 is observed with a TEM. In this specification, when a domain is not confirmed, it may be expressed that the maximum diameter of the domain is 0 nm.
- the hardness of the adhesive sheet tends to be uneven. Furthermore, when the pressure-sensitive adhesive sheet is deformed due to a dimensional change of the optical film or the like, regions where the pressure-sensitive adhesive component does not exist, such as voids, are likely to occur at the interfaces of the domains. When this region is generated, the adhesive strength of the adhesive sheet is lowered, and peeling between members is likely to occur. According to the pressure-sensitive adhesive sheet 1 of the present embodiment, since the maximum diameter of the domains is 170 nm or less, the occurrence of areas where the pressure-sensitive adhesive component does not exist is sufficiently suppressed. As a result, the adhesive sheet 1 has improved durability.
- the storage modulus G′ of PSA sheet 1 at 25° C. and the maximum diameter of the domain depend on the type of cross-linking agent contained in the PSA composition for forming PSA sheet 1, the amount of the cross-linking agent, and the PSA composition.
- Various factors such as the glass transition temperature (Tg) of the contained base polymer, the structural units constituting the base polymer, the presence or absence of additives such as tackifiers, and the drying conditions of the adhesive composition when forming the adhesive sheet 1 change based on
- Tg glass transition temperature
- Patent Document 1 by using a pressure-sensitive adhesive composition containing an amine-based compound containing a plurality of hydroxyl groups, the maximum length of the domain in the pressure-sensitive adhesive sheet can be increased from 0.3 to 1 ⁇ m. It can be read that it can be lowered.
- the shortest distance D can be specified by the following method.
- the maximum diameter of the domain is specified by the method described above.
- domains having a diameter of 80% or more of the maximum diameter are identified among a plurality of domains existing within a range of 6 ⁇ m long ⁇ 6 ⁇ m wide.
- Distance measurements are performed for all combinations of identified domains.
- the minimum value of the obtained measurements can be regarded as the shortest distance D.
- the shortest distance D is more preferably 400 nm or longer, and even more preferably 500 nm or longer.
- the upper limit of the shortest distance D is not particularly limited, and is, for example, 2000 nm.
- the number of domains having a diameter of 80% or more of the above-described maximum diameter within a range of 6 ⁇ m long ⁇ 6 ⁇ m wide is, for example, 20. number or less, preferably 15 or less, more preferably 10 or less.
- the number of domains is zero.
- the area ratio R of the domain having a diameter of 80% or more of the maximum diameter is within a range of 6 ⁇ m long ⁇ 6 ⁇ m wide. It is preferably 0.7% or less.
- the ratio R can be specified by the following method. First, the maximum diameter of the domain is specified by the method described above. In the TEM image, among the domains existing within a range of 6 ⁇ m long ⁇ 6 ⁇ m wide, domains having a diameter of 80% or more of the maximum diameter are specified. For each identified domain, the area is calculated by image processing, and the total value T is identified. The ratio of the total value T to the observation range area (36 ⁇ m 2 ) can be regarded as the ratio R. The ratio R is more preferably 0.6% or less, even more preferably 0.5% or less. When the cross section of PSA sheet 1 is observed with a TEM, the ratio R is 0% when no domain is confirmed at a magnification of 20,000.
- the gel fraction is not particularly limited, and is, for example, 60% to 99%.
- the gel fraction of the adhesive sheet 1 is preferably 80% or higher, more preferably 90% or higher, still more preferably 94% or higher, and particularly preferably 95% or higher.
- the gel fraction of the adhesive sheet 1 can be evaluated, for example, by the following method. First, a small piece is obtained by scraping off part of the adhesive sheet 1 . The resulting strip is then wrapped with an expanded porous membrane of polytetrafluoroethylene and tied with kite string. A test piece is thus obtained. Next, the total weight (weight A) of the small piece of adhesive sheet 1, the stretched porous membrane and the kite string is measured.
- the sum of the stretched porous membrane and the kite string used is defined as weight B.
- the test piece is immersed in a container filled with ethyl acetate and allowed to stand at 23° C. for one week. After standing still, the test piece is taken out from the container, dried for 2 hours in a dryer set at 130° C., and then the weight C of the test piece is measured.
- the adhesive sheet 1 preferably has high transparency.
- the haze of the adhesive sheet 1 is, for example, 1% or less, preferably 0.8% or less, and more preferably 0.5% or less.
- the pressure-sensitive adhesive sheet 1 may have a peak top stress X max satisfying the following formula (1).
- X max ⁇ 0.5 MPa (1)
- the peak top stress X max is the peak value of the stress X in the stress-strain curve determined by the following evaluation test for the adhesive sheet 1.
- the thickness of the adhesive sheet 1 to be attached is preferably 200 ⁇ m or more. If the thickness does not reach 200 ⁇ m, the thickness may be increased to 200 ⁇ m or more by stacking two or more pressure-sensitive adhesive sheets 1 and bonding them together by heating I using an autoclave or the like.
- the glass plate 51 can be selected from those having a flat surface to which the adhesive sheet 1 is attached and from which the adhesive sheet 1 does not peel off during the evaluation test. The adhesion of the adhesive sheet 1 to the glass plate 51 should be carried out so that the adhesive sheet 1 does not peel off during the evaluation test. If necessary, the state of bonding between the adhesive sheet 1 and the glass plate 51 may be stabilized by heating II using an autoclave or the like.
- heating I and heating II are, for example, 30 to 90° C. and 0.5 to 4 hours. pressure). Heating I and Heating II may be performed at the same time while the adhesive sheet 1 is adhered to the glass plate 51 .
- the evaluation probe 52 a probe tack test probe complying with ASTM D-2979 can be used.
- the evaluation probe 52 is displaced in a direction perpendicular to the surface of the adhesive sheet 1 and away from the adhesive sheet 1 (FIG. 2C).
- the direction usually coincides with the thickness direction of the adhesive sheet 1 .
- the rate of displacement is kept constant at 2 ⁇ m/min.
- the stress X and strain Y in the thickness direction generated in the adhesive sheet 1 due to the displacement of the evaluation probe 52 are measured, and from the measured stress X and strain Y, the strain Y is the horizontal axis and the stress X is the vertical axis. get the curve.
- a tensile tester can be used for the evaluation test.
- the stress X can be measured by a load cell of a tensile tester connected to the evaluation probe 52, for example.
- the amount of displacement d corresponds to the amount of deformation t 1 in the thickness direction of the adhesive sheet 1 due to the displacement of the evaluation probe 52 .
- FIG. 3 shows stress-strain curves 101, 102, 103 and 104 of four types of adhesive sheets.
- PSA sheet 1 showing curves 101, 103 and 104 satisfies formula (1).
- the adhesive sheet showing curve 102 does not satisfy formula (1). Note that for curve 101, X max is achieved at its vertex A.
- the volume of the adhesive sheet 112 attached thereto also changes.
- the volume of the pressure-sensitive adhesive sheet 112 increases by the amount of the expanded region 115 (note that reference numerals 114 and 116 indicate before expansion and expansion, respectively).
- 113 is an adherend such as a glass substrate).
- X max may be 0.6 MPa or more, 0.8 MPa or more, 0.9 MPa or more, 1.0 MPa or more, 1.2 MPa or more, 1.4 MPa or more, or even 1.5 MPa or more.
- the upper limit of X max is, for example, 5 MPa or less.
- the strain Y m when the stress X reaches the peak top stress X max may satisfy the following formula (2). Ym ⁇ 0.05 (2)
- PSA sheet 1 showing curves 101 and 104 in FIG. 3 satisfies formula (2).
- Y m of curve 101 is reached at vertex A.
- Y m is 0.07 or more, 0.08 or more, 0.09 or more, 0.10 or more, 0.11 or more, 0.12 or more, 0.13 or more, 0.14 or more, 0.15 or more, and may be 0.16 or more.
- the upper limit of Y m is, for example, 0.3.
- the strain Y 0.15 when the stress X drops to 0.15 MPa after reaching the peak top stress X max may satisfy the following formula (3). Y 0.15 ⁇ 0.28 (3)
- PSA sheet 1 showing curve 101 satisfies formula (3).
- Y 0.15 of curve 101 is achieved at point B.
- Y 0.15 is 0.28 or more, even after the stress of the pressure-sensitive adhesive sheet 1 that resists the change in volume has exceeded the peak, for example, areas (voids, etc.) where the pressure-sensitive adhesive component does not exist inside the pressure-sensitive adhesive sheet 1 It means that a constant stress can be maintained up to a larger strain by suppressing the occurrence of Y 0.15 may be 0.29 or more, 0.30 or more, 0.31 or more, 0.32 or more, or even 0.33 or more.
- the upper limit of Y 0.15 is, for example, 1.00 or less.
- PSA sheet 1 satisfying the above range for Y 0.15 and having strain Y m of 0.09 or more, particularly 0.13 or more, is particularly suitable for improving durability.
- the pressure-sensitive adhesive sheet 1 satisfying the above range for Y 0.15 and having a peak top stress X max of 0.9 or more, particularly 1 or more, 1.1 or more, further 1.2 or more suppresses dimensional change and It is particularly suitable for balancing with ensuring durability.
- the ratio of the strain Y 0.15 when the stress X drops to 0.15 MPa after the stress X reaches the peak top stress X max to the strain Y m when the stress X reaches the peak top stress X max Y 0.15 /Y m may satisfy the following formula (4). Y0.15 / Ym ⁇ 2 (4)
- PSA sheet 1 showing curve 101 in FIG. 3 satisfies formula (4).
- the fact that the ratio Y 0.15 /Y m is 2 or more means that the occurrence of voids and the like and the rate of occurrence of voids can be suppressed after the stress of the pressure-sensitive adhesive sheet 1 that resists changes in volume reaches its peak and until it reaches a larger strain. means.
- the ratio Y 0.15 /Y m may be 2.1 or more.
- the upper limit of the ratio Y 0.15 /Y m is, for example, 10 or less.
- the thickness of the adhesive sheet 1 is not particularly limited, and is, for example, about 1 to 100 ⁇ m, preferably 2 to 50 ⁇ m, more preferably 2 to 40 ⁇ m, still more preferably 5 to 35 ⁇ m.
- composition of the pressure-sensitive adhesive sheet 1 is not particularly limited as long as the storage modulus G' at 25°C and the maximum domain diameter are within the ranges described above, but it preferably contains two or more types of polymers.
- the domains may be formed by precipitation of at least one of the two or more polymers contained in the adhesive sheet 1 .
- the adhesive sheet 1 is formed from an adhesive composition containing a (meth)acrylic polymer (A) and a cross-linking agent.
- the cross-linking agent is typically an isocyanate-based cross-linking agent.
- the pressure-sensitive adhesive sheet 1 formed from this pressure-sensitive adhesive composition contains a cross-linked product of a (meth)acrylic polymer (A) and a polymer (B) containing, as a main component, a structural unit derived from an isocyanate-based cross-linking agent.
- the term “main component” means a structural unit that is the most contained on a weight basis among all the structural units that constitute the polymer.
- the content of structural units derived from the isocyanate cross-linking agent is, for example, 70% by weight or more, preferably 90% by weight or more.
- the polymer (B), for example, consists essentially of structural units derived from an isocyanate-based cross-linking agent.
- the crosslinked product of the (meth)acrylic polymer (A) and the polymer (B) may constitute an interpenetrating network (IPN) structure. This IPN structure is suitable for improving the durability while increasing the elastic modulus of the pressure-sensitive adhesive sheet 1 .
- the domains are formed, for example, by precipitation of the polymer (B), and substantially the polymer (B ).
- the domain may contain impurities other than the polymer (B).
- the (meth)acrylic polymer (A) can function as a base polymer for acrylic pressure-sensitive adhesives.
- Acrylic pressure-sensitive adhesives tend to have excellent optical transparency, appropriate wettability, cohesiveness, adhesiveness and other adhesive properties, and excellent weather resistance, heat resistance, and the like.
- the (meth)acrylic polymer (A) contains, for example, a structural unit derived from an alkyl (meth)acrylate as a main component.
- “(meth)acrylate” means acrylate and/or methacrylate.
- the number of carbon atoms in the alkyl group contained in the alkyl (meth)acrylate for forming the main skeleton of the (meth)acrylic polymer (A) is not particularly limited, and is, for example, 1-30.
- This alkyl group may be linear, branched, or cyclic.
- Examples of alkyl groups include methyl group, ethyl group, propyl group, isopropyl group, butyl group, isobutyl group, amyl group, hexyl group, cyclohexyl group, heptyl group, 2-ethylhexyl group, isooctyl group, nonyl group and decyl group.
- Alkyl (meth)acrylates can be used alone or in combination.
- the average carbon number of the alkyl group is preferably 3-9.
- Alkyl (meth)acrylate is preferably butyl acrylate.
- the content of structural units derived from alkyl (meth)acrylate is, for example, 50% by weight or more, preferably 60% by weight or more, from the viewpoint of improving the adhesiveness of the pressure-sensitive adhesive sheet 1. , more preferably 70% by weight or more, and still more preferably 80% by weight or more.
- (meth)acrylic polymer (A) in addition to alkyl (meth)acrylates, aromatic ring-containing monomers, amide group-containing monomers, carboxyl group-containing monomers, hydroxyl group-containing monomers, At least one comonomer selected from the group consisting of monomers is included. Comonomers can be used alone or in combination.
- the (meth)acrylic polymer (A) preferably contains structural units derived from aromatic ring-containing monomers.
- the aromatic ring-containing monomer is a compound containing an aromatic ring structure in its structure and a polymerizable unsaturated double bond such as a (meth)acryloyl group or vinyl group. Examples of aromatic rings include benzene ring, naphthalene ring, and biphenyl ring.
- the aromatic ring-containing monomer is preferably an aromatic ring-containing (meth)acrylate.
- aromatic ring-containing (meth)acrylates examples include benzyl (meth)acrylate, phenyl (meth)acrylate, o-phenylphenol (meth)acrylate, phenoxy (meth)acrylate, phenoxyethyl (meth)acrylate, phenoxypropyl (meth)acrylate, ) acrylate, phenoxydiethylene glycol (meth) acrylate, ethylene oxide-modified nonylphenol (meth) acrylate, ethylene oxide-modified cresol (meth) acrylate, phenol ethylene oxide-modified (meth) acrylate, 2-hydroxy-3-phenoxypropyl (meth) acrylate, Those having a benzene ring such as methoxybenzyl (meth)acrylate, chlorobenzyl (meth)acrylate, cresyl (meth)acrylate, polystyryl (meth)acrylate; hydroxyethylated ⁇ -naphthol acryl
- the (meth)acrylic polymer (A) may contain structural units derived from amide group-containing monomers.
- the amide group-containing monomer is a compound containing an amide group in its structure and a polymerizable unsaturated double bond such as a (meth)acryloyl group or vinyl group.
- amide group-containing monomers include (meth)acrylamide, N,N-dimethyl(meth)acrylamide, N,N-diethyl(meth)acrylamide, N-isopropylacrylamide, N-methyl(meth)acrylamide, N -butyl (meth)acrylamide, N-hexyl (meth)acrylamide, N-methylol (meth)acrylamide, N-methylol-N-propane (meth)acrylamide, aminomethyl (meth)acrylamide, aminoethyl (meth)acrylamide, mercapto acrylamide-based monomers such as methyl (meth)acrylamide and mercaptoethyl (meth)acrylamide; N-acryloyl heterocycles such as N-(meth)acryloylmorpholine, N-(meth)acryloylpiperidine, and N-(meth)acryloylpyrrolidine Monomers: N-vinyl group-containing lactam monomers such as N-vinyl
- the (meth)acrylic polymer (A) may contain a structural unit derived from a carboxyl group-containing monomer.
- a carboxyl group-containing monomer is a compound containing a carboxyl group in its structure and a polymerizable unsaturated double bond such as a (meth)acryloyl group and a vinyl group.
- Examples of carboxyl group-containing monomers include (meth)acrylic acid, carboxyethyl (meth)acrylate, carboxypentyl (meth)acrylate, itaconic acid, maleic acid, fumaric acid, and crotonic acid.
- acrylic acid is preferable from the viewpoint of improving copolymerizability, price, and adhesive properties of the adhesive sheet 1 .
- the self-polymerizability of the cross-linking agent can be enhanced. Improvement of the self-polymerization property of the cross-linking agent can contribute to suppression of peeling of the pressure-sensitive adhesive sheet in a humidified environment, and stabilization of the physical properties of the pressure-sensitive adhesive sheet in a system having a high content of the cross-linking agent.
- the (meth)acrylic polymer (A) may contain structural units derived from hydroxyl group-containing monomers.
- a hydroxyl group-containing monomer is a compound containing a hydroxyl group in its structure and a polymerizable unsaturated double bond such as a (meth)acryloyl group or a vinyl group.
- Examples of hydroxyl group-containing monomers include 2-hydroxyethyl (meth)acrylate, 3-hydroxypropyl (meth)acrylate, 4-hydroxybutyl (meth)acrylate, 6-hydroxyhexyl (meth)acrylate, and 8-hydroxyoctyl.
- (meth)acrylate 10-hydroxydecyl (meth)acrylate, 12-hydroxylauryl (meth)acrylate and other hydroxyl group-containing alkyl (meth)acrylates; (4-hydroxymethylcyclohexyl)-methylacrylate and other hydroxyl group-containing cycloalkyl (meth)acrylates; ) acrylates.
- 2-hydroxyethyl (meth)acrylate and 4-hydroxybutyl (meth)acrylate are preferred.
- aromatic ring-containing monomers and carboxyl group-containing monomers are preferably used from the viewpoint of adhesiveness, durability, etc., and aromatic ring-containing monomers are particularly preferably used.
- the (meth)acrylic polymer (A) containing a structural unit derived from a carboxyl group-containing monomer tends to promote the reaction between isocyanate cross-linking agents by taking in water molecules in the surrounding atmosphere.
- the aromatic ring-containing monomer is suitable for improving the compatibility between the (meth)acrylic polymer (A) and the polymer (B) and suppressing the formation of domains in the pressure-sensitive adhesive sheet 1 . This also tends to improve the durability of the optical layered body in a hot and humid environment.
- the content of structural units derived from copolymer monomers is not particularly limited, and is, for example, 0 to 40% by weight, and 0.1 to 30% by weight. may be 0.1 to 20% by weight.
- the content of structural units derived from aromatic ring-containing monomers is not particularly limited, and is, for example, 3 to 25% by weight, more preferably 22% by weight or less, and 20% by weight. Weight % or less is more preferable. This content is more preferably 8% by weight or more, and even more preferably 12% by weight or more.
- the content of structural units derived from the amide group-containing monomer is not particularly limited, and is, for example, 0.1 to 10% by weight, and 0.2 to 8% by weight. is more preferred, and 0.6 to 6% by weight is even more preferred.
- the content of structural units derived from a carboxyl group-containing monomer is not particularly limited, and is, for example, 0.1 to 25% by weight, more preferably 3% by weight or more. . This content is preferably 20% by weight or less, more preferably 10% by weight or less.
- the content of structural units derived from hydroxyl group-containing monomers is, for example, 1% by weight or less, more preferably 0.5% by weight or less, and 0.2% by weight or less. is more preferred.
- the (meth)acrylic polymer (A) may be substantially free of structural units derived from hydroxyl group-containing monomers.
- an inert such as a (meth)acryloyl group or a vinyl group can be used for the purpose of improving the adhesiveness and heat resistance of the pressure-sensitive adhesive sheet 1.
- an inert such as a (meth)acryloyl group or a vinyl group
- Other comonomers having polymerizable functional groups containing saturated double bonds can be used.
- Other comonomers can be used alone or in combination.
- copolymerizable monomers include, for example, acid anhydride group-containing monomers such as maleic anhydride and itaconic anhydride; caprolactone adducts of acrylic acid; allylsulfonic acid, 2-(meth)acrylamide-2- sulfonic acid group-containing monomers such as methylpropanesulfonic acid, (meth)acrylamidopropanesulfonic acid, and sulfopropyl (meth)acrylate; phosphoric acid group-containing monomers such as 2-hydroxyethyl acryloyl phosphate; aminoethyl (meth) Alkylaminoalkyl (meth)acrylates such as acrylates, N,N-dimethylaminoethyl (meth)acrylate and t-butylaminoethyl (meth)acrylate; Alkoxyalkyls such as methoxyethyl (meth)acrylate and ethoxyethyl (meth)
- copolymer monomers include, for example, tripropylene glycol di(meth)acrylate, tetraethylene glycol di(meth)acrylate, 1,6-hexanediol di(meth)acrylate, bisphenol A diglycidyl ether di (Meth)acrylate, neopentyl glycol di(meth)acrylate, trimethylolpropane tri(meth)acrylate, pentaerythritol tri(meth)acrylate, pentaerythritol tetra(meth)acrylate, dipentaerythritol penta(meth)acrylate, dipenta Polyfunctional monomers having two or more unsaturated double bonds, such as erythritol hexa(meth)acrylate and caprolactone-modified dipentaerythritol hexa(meth)acrylate, can be mentioned.
- the content of structural units derived from the other copolymerization monomer in the (meth)acrylic polymer (A) is 10% by weight or less. is preferably 7% by weight or less, and even more preferably 5% by weight or less.
- the (meth)acrylic polymer (A) usually has a weight average molecular weight of 300,000 to 4,000,000. From the viewpoint of durability, the (meth)acrylic polymer (A) preferably has a weight average molecular weight of 300,000 to 3,000,000, more preferably 400,000 to 2,200,000. A weight average molecular weight of 300,000 or more is preferable from the viewpoint of heat resistance. When the weight-average molecular weight is 4,000,000 or less, the pressure-sensitive adhesive sheet tends to be hard to harden and peeling is hard to occur.
- Weight average molecular weight (Mw)/number average molecular weight (Mn) which means molecular weight distribution, is preferably 1.8 to 10, more preferably 1.8 to 7, and 1.8 to 5. is more preferred.
- a molecular weight distribution (Mw/Mn) of 10 or less is preferable from the standpoint of durability.
- the weight average molecular weight and molecular weight distribution (Mw/Mn) are measured by GPC (gel permeation chromatography) and obtained from values calculated by polystyrene conversion.
- the (meth)acrylic polymer (A) can be produced by known polymerization methods such as solution polymerization, radiation polymerization such as electron beam and UV, bulk polymerization, and various radical polymerizations such as emulsion polymerization.
- the (meth)acrylic polymer (A) to be obtained may be any of random copolymers, block copolymers, graft copolymers, and the like.
- solution polymerization for example, ethyl acetate, toluene, etc. are used as polymerization solvents.
- Solution polymerization is carried out, for example, by adding a polymerization initiator under an inert gas stream such as nitrogen, and usually under reaction conditions of about 50 to 70° C. for about 5 to 30 hours.
- the polymerization initiator, chain transfer agent, emulsifier, etc. used for radical polymerization are not particularly limited and can be appropriately selected and used.
- the weight average molecular weight of the (meth)acrylic polymer (A) can be controlled by adjusting the amount of polymerization initiator and chain transfer agent used, the reaction conditions, and the like. Therefore, the amounts of the polymerization initiator and the chain transfer agent to be used are appropriately adjusted depending on the composition.
- polymerization initiators examples include 2,2′-azobisisobutyronitrile, 2,2′-azobis(2-amidinopropane) dihydrochloride, 2,2′-azobis[2-(5-methyl-2 -imidazolin-2-yl)propane]dihydrochloride, 2,2'-azobis(2-methylpropionamidine) disulfate, 2,2'-azobis(N,N'-dimethyleneisobutyramidine), 2,2 Azo initiators such as '-azobis[N-(2-carboxyethyl)-2-methylpropionamidine] hydrate (manufactured by Wako Pure Chemical Industries, Ltd., VA-057); persulfates such as potassium persulfate and ammonium persulfate ; di(2-ethylhexyl) peroxydicarbonate, di(4-t-butylcyclohexyl) peroxydicarbonate, di-sec-butyl peroxydi
- the polymerization initiator can be used alone or in combination. More preferably, it is about 0.5 parts by weight.
- chain transfer agents examples include lauryl mercaptan, glycidyl mercaptan, mercaptoacetic acid, 2-mercaptoethanol, thioglycolic acid, 2-ethylhexyl thioglycolate, and 2,3-dimercapto-1-propanol.
- the chain transfer agent may be used alone or in combination of two or more. less than a degree.
- emulsifiers used in emulsion polymerization include anionic emulsifiers such as sodium lauryl sulfate, ammonium lauryl sulfate, sodium dodecylbenzenesulfonate, ammonium polyoxyethylene alkyl ether sulfate, and sodium polyoxyethylene alkylphenyl ether sulfate; Examples include nonionic emulsifiers such as ethers, polyoxyethylene alkylphenyl ethers, polyoxyethylene fatty acid esters, and polyoxyethylene-polyoxypropylene block polymers. Emulsifiers can be used alone or in combination.
- Examples of reactive emulsifiers include emulsifiers into which radically polymerizable functional groups such as propenyl groups and allyl ether groups have been introduced.
- Specific examples of this emulsifier include Aqualon HS-10, HS-20, KH-10, BC-05, BC-10, and BC-20 (all of which are manufactured by Dai-ichi Kogyo Seiyaku Co., Ltd.), Adekaria Soap SE10N (ADEKA company), etc.
- a reactive emulsifier is preferable because it is incorporated into the polymer chain after polymerization and improves the water resistance.
- the amount of the emulsifier to be used is preferably 0.3 to 5 parts by weight, more preferably 0.5 to 1 part by weight, based on 100 parts by weight of the total amount of the monomer components, from the viewpoint of polymerization stability and mechanical stability.
- a (meth)acrylic polymer (A) is produced by irradiating a monomer component with radiation such as an electron beam or UV.
- radiation such as an electron beam or UV.
- the radiation polymerization is carried out with an electron beam, it is not particularly necessary to contain a photopolymerization initiator in the monomer component.
- the monomer component may contain a photopolymerization initiator for the advantage of being able to shorten the polymerization time.
- Photoinitiators can be used alone or in combination.
- the photopolymerization initiator is not particularly limited as long as it initiates photopolymerization, and commonly used photopolymerization initiators can be used.
- Examples of photopolymerization initiators that can be used include benzoin ether-based, acetophenone-based, ⁇ -ketol-based, photoactive oxime-based, benzoin-based, benzyl-based, benzophenone-based, ketal-based, and thioxanthone-based initiators.
- the amount of the photopolymerization initiator used is 0.05 to 1.5 parts by weight, preferably 0.1 to 1 part by weight, per 100 parts by weight of the monomer component. Photoinitiators can be used alone or in combination.
- a compound having at least two isocyanate groups can be used as the isocyanate-based cross-linking agent.
- the number of isocyanate groups contained in the isocyanate compound is preferably 3 or more.
- the upper limit of the number of isocyanate groups is not particularly limited, and is 5, for example.
- Examples of isocyanate compounds include aromatic isocyanate compounds, alicyclic isocyanate compounds, and aliphatic isocyanate compounds.
- the isocyanate-based cross-linking agent is preferably capable of self-polymerization by reacting with water.
- aromatic isocyanate compounds include phenylene diisocyanate, 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate, 2,2′-diphenylmethane diisocyanate, 4,4′-diphenylmethane diisocyanate, and 4,4′-toluidine. diisocyanate, 4,4'-diphenyl ether diisocyanate, 4,4'-diphenyl diisocyanate, 1,5-naphthalene diisocyanate, xylylene diisocyanate and the like.
- alicyclic isocyanate compounds include 1,3-cyclopentene diisocyanate, 1,3-cyclohexane diisocyanate, 1,4-cyclohexane diisocyanate, isophorone diisocyanate, hydrogenated diphenylmethane diisocyanate, hydrogenated xylylene diisocyanate, and hydrogenated tolylene diisocyanate. , hydrogenated tetramethylxylylene diisocyanate, and the like.
- aliphatic isocyanate compounds include trimethylene diisocyanate, tetramethylene diisocyanate, hexamethylene diisocyanate, pentamethylene diisocyanate, 1,2-propylene diisocyanate, 1,3-butylene diisocyanate, dodecamethylene diisocyanate, and 2,4,4-trimethylhexamethylene. and diisocyanate.
- isocyanate-based cross-linking agents examples include polymers of the above isocyanate compounds (dimers, trimers, pentamers, etc.), adducts obtained by addition to polyhydric alcohols such as trimethylolpropane, urea modified products, Urethane prepolymers obtained by addition to biuret-modified, allophanate-modified, isocyanurate-modified, carbodiimide-modified, polyether polyol, polyester polyol, acrylic polyol, polybutadiene polyol, polyisoprene polyol and the like are also included.
- the isocyanate-based cross-linking agent is preferably an aromatic isocyanate compound and its derivative, more preferably tolylene diisocyanate and its derivative, in other words, a tolylene diisocyanate-based (TDI-based) cross-linking agent.
- the TDI-based cross-linking agent is more suitable for producing the adhesive sheet 1 of the present embodiment than xylylene diisocyanate and its derivatives, in other words, the xylylene diisocyanate-based (XDI-based) cross-linking agent.
- the isocyanate-based cross-linking agent preferably contains an adduct of a polyhydric alcohol and tolylene diisocyanate as a TDI-based cross-linking agent.
- a specific example of this adduct is a trimethylolpropane/tolylene diisocyanate trimer adduct.
- isocyanate-based cross-linking agents examples include, for example, Tosoh's trade names “Millionate MT”, “Millionate MTL”, “Millionate MR-200”, “Millionate MR-400", “Coronate L”, and “Coronate HL”. ”, “Coronate HX”, trade names manufactured by Mitsui Chemicals “Takenate D-110N”, “Takenate D-120N”, “Takenate D-140N”, “Takenate D-160N”, “Takenate D-165N”, “ Takenate D-170HN", “Takenate D-178N”, “Takenate 500", "Takenate 600” and the like, preferably Coronate L.
- the isocyanate-based cross-linking agents may be used singly or in combination of two or more.
- the amount of the isocyanate-based cross-linking agent is, for example, 5 parts by weight or more, preferably 8 parts by weight or more, and more preferably 10 parts by weight or more with respect to 100 parts by weight of the (meth)acrylic polymer (A). Yes, more preferably 11 parts by weight or more.
- the amount of the isocyanate-based cross-linking agent is, for example, 30 parts by weight or less, preferably 20 parts by weight or less, more preferably 15 parts by weight or less with respect to 100 parts by weight of the (meth)acrylic polymer (A). Yes, more preferably 13 parts by weight or less.
- the isocyanate-based cross-linking agents when the amount of the isocyanate-based cross-linking agent per 100 parts by weight of the (meth)acrylic polymer (A) is as large as about 5 parts by weight or more, when the pressure-sensitive adhesive sheet is produced, the isocyanate-based cross-linking agents
- the reaction may form a polymer (B) containing structural units derived from the isocyanate-based cross-linking agent as a main component. At this time, the formation of the polymer (B) tends to proceed dominantly over the reaction between the isocyanate-based cross-linking agent and the (meth)acrylic polymer (A).
- the polymer (B) is suitable for suppressing dimensional change of the pressure-sensitive adhesive sheet by imparting sufficient cohesion to the pressure-sensitive adhesive sheet. That is, the polymer (B) is suitable for suppressing display unevenness and light leakage in an image display device. Furthermore, the combination of (meth)acrylic polymer (A) and polymer (B) is suitable for improving the durability of the pressure-sensitive adhesive sheet in hot and humid environments.
- the pressure-sensitive adhesive composition may contain a cross-linking agent other than the isocyanate-based cross-linking agent.
- Other cross-linking agents include peroxide-based cross-linking agents, epoxy-based cross-linking agents, imine-based cross-linking agents, polyfunctional metal chelates, and the like.
- the amount of the other cross-linking agent to be added is preferably 2 parts by weight or less, more preferably 1 part by weight or less, per 100 parts by weight of the (meth)acrylic polymer (A). From the viewpoint of durability of the PSA sheet, the PSA composition preferably does not substantially contain other cross-linking agents, especially epoxy-based cross-linking agents.
- the adhesive composition may further contain a (meth)acrylic oligomer.
- the (meth)acrylic oligomer can have the same composition as the (meth)acrylic polymer (A) described above, except that the weight average molecular weight (Mw) is different.
- the weight average molecular weight (Mw) of the (meth)acrylic oligomer is, for example, 1000 or more, and may be 2000 or more, 3000 or more, or even 4000 or more.
- the upper limit of the weight average molecular weight (Mw) of the (meth)acrylic oligomer is, for example, 30,000 or less, and may be 15,000 or less, 10,000 or less, or even 7,000 or less.
- the (meth)acrylic oligomer has, for example, one or more structural units derived from the following monomers: methyl (meth)acrylate, ethyl (meth)acrylate, propyl (meth)acrylate. , isopropyl (meth) acrylate, butyl (meth) acrylate, isobutyl (meth) acrylate, s-butyl (meth) acrylate, t-butyl (meth) acrylate, pentyl (meth) acrylate, isopentyl (meth) acrylate, hexyl (meth) acrylate ) acrylate, 2-ethylhexyl (meth) acrylate, heptyl (meth) acrylate, octyl (meth) acrylate, isooctyl (meth) acrylate, nonyl (meth) acrylate, isononyl (meth) acrylate, de
- the (meth)acrylic oligomer preferably has structural units derived from a (meth)acrylic monomer having a relatively bulky structure.
- the adhesiveness of the adhesive sheet can be further enhanced.
- the acrylic monomer include alkyl (meth)acrylates having a branched alkyl group such as isobutyl (meth)acrylate and t-butyl (meth)acrylate; cyclohexyl (meth)acrylate and isobornyl (meth)acrylate.
- the monomer preferably has a cyclic structure, more preferably two or more cyclic structures.
- the (meth)acrylic oligomer is polymerized and/or the adhesive sheet is irradiated with ultraviolet rays during the formation of the pressure-sensitive adhesive sheet, the progress of polymerization and/or formation is less likely to be inhibited.
- an alkyl (meth)acrylate having an alkyl group having a branched structure, or an ester of (meth)acrylic acid and an alicyclic alcohol can be used.
- (meth)acrylic oligomers include copolymers of butyl acrylate, methyl acrylate and acrylic acid, copolymers of cyclohexyl methacrylate and isobutyl methacrylate, copolymers of cyclohexyl methacrylate and isobornyl methacrylate, cyclohexyl Copolymers of methacrylate and acryloylmorpholine, copolymers of cyclohexyl methacrylate and diethylacrylamide, copolymers of 1-adamantyl acrylate and methyl methacrylate, copolymers of dicyclopentanyl methacrylate and isobornyl methacrylate, Copolymers of methyl methacrylate and at least one selected from dicyclopentanyl methacrylate, cyclohexyl methacrylate, isobornyl methacrylate, isobornyl acrylate and cyclopentanyl methacrylate,
- the polymerization method for the (meth)acrylic polymer (A) described above can be employed for the polymerization of the (meth)acrylic oligomer.
- the amount thereof is, for example, 70 parts by weight or less, 50 parts by weight or less, and further 100 parts by weight of the (meth)acrylic polymer (A). may be 40 parts by weight or less.
- the lower limit of the amount to be blended is, for example, 1 part by weight or more, 2 parts by weight or more, and may be 3 parts by weight or more with respect to 100 parts by weight of the (meth)acrylic polymer (A).
- the pressure-sensitive adhesive composition may not contain a (meth)acrylic oligomer.
- the adhesive composition may further contain known additives.
- Additives include, for example, silane coupling agents, solvents, colorants, powders such as pigments, dyes, surfactants, plasticizers, tackifiers, surface lubricants, leveling agents, rework improvement agents, softeners, antioxidants, anti-aging agents, light stabilizers, ultraviolet absorbers, polymerization inhibitors, inorganic or organic fillers, metal powders, particles, and foil-like materials.
- a redox system with a reducing agent may be employed within a controllable range.
- These additives can be used in an amount of, for example, 10 parts by weight or less, preferably 5 parts by weight or less, and more preferably 1 part by weight or less per 100 parts by weight of the (meth)acrylic polymer (A).
- silane coupling agents include 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 3-glycidoxypropylmethyldiethoxysilane, 2-(3,4- Epoxy group-containing silane coupling agents such as epoxycyclohexyl)ethyltrimethoxysilane; 3-aminopropyltrimethoxysilane, N-2-(aminoethyl)-3-aminopropylmethyldimethoxysilane, 3-triethoxysilyl-N- Amino group-containing silane coupling agents such as (1,3-dimethylbutylidene)propylamine and N-phenyl- ⁇ -aminopropyltrimethoxysilane; 3-acryloxypropyltrimethoxysilane, 3-methacryloxypropyltriethoxysilane; (Meth)acrylic group-containing silane coupling agents such as; isocyanate group-
- the amount is, for example, 5 parts by weight or less, 3 parts by weight or less, and 1 part by weight with respect to 100 parts by weight of the (meth)acrylic polymer (A). It may be 0.5 parts by weight or less, 0.2 parts by weight or less, 0.1 parts by weight or less, or even 0.05 parts by weight or less.
- the adhesive composition may not contain a silane coupling agent.
- the adhesive composition may further contain an amine-based compound containing multiple hydroxyl groups, but it does not have to.
- Types of pressure-sensitive adhesive compositions are, for example, emulsion type, solvent type (solution type), active energy ray-curable type (light-curing type), and heat-melting type (hot-melt type).
- the pressure-sensitive adhesive composition may be of a solvent type from the viewpoint of forming the pressure-sensitive adhesive sheet 1 having excellent durability.
- the solvent-based pressure-sensitive adhesive composition may not contain a photocuring agent such as an ultraviolet curing agent.
- the method for producing the pressure-sensitive adhesive sheet 1 includes, for example, applying a pressure-sensitive adhesive composition containing a (meth)acrylic polymer (A) and an isocyanate-based cross-linking agent to a substrate to form a coating film, and the resulting coating film. and drying.
- a release film can be used as the base material.
- the pressure-sensitive adhesive sheet 1 formed on the release film can be transferred to, for example, an optical film.
- the substrate may be an optical film.
- an optical laminate can be obtained by forming the adhesive sheet 1 .
- the release film After transferring the adhesive sheet 1 to the optical film, the release film can be used as a release liner until the adhesive sheet 1 is put to practical use, and the process can be simplified.
- Examples of materials constituting the release film include porous materials such as plastic films, paper, cloth, and nonwoven fabrics, nets, foam sheets, metal foils, and appropriate thin sheets such as laminates thereof.
- a plastic film is preferably used because of its excellent surface smoothness.
- the plastic film is not particularly limited, and examples thereof include polyethylene film, polypropylene film, polybutene film, polybutadiene film, polymethylpentene film, polyvinyl chloride film, vinyl chloride copolymer film, polyethylene terephthalate film, polybutylene terephthalate film, Polyurethane films, ethylene-vinyl acetate copolymer films and the like are included.
- the thickness of the release film is usually 5-200 ⁇ m, preferably about 5-100 ⁇ m.
- the release film is subjected to a release treatment such as a silicone-based, fluorine-based, or long-chain alkyl-based release treatment.
- the release film may be subjected to a release and antifouling treatment using a fatty acid amide release agent, silica powder, or the like, or an antistatic treatment such as a coating type, a kneading type, or a vapor deposition type.
- a solution containing an adhesive composition may be applied to the substrate.
- the solid content concentration of the adhesive solution is, for example, 5 to 50% by weight, preferably 10 to 40% by weight.
- the pressure-sensitive adhesive solution can be prepared by appropriately adding the same solvent or a different solvent as the polymerization solvent to the pressure-sensitive adhesive composition depending on the polymerization form of the (meth)acrylic polymer (A).
- Various methods are used to apply the adhesive composition to the substrate, for example, roll coating, kiss roll coating, gravure coating, reverse coating, roll brushing, spray coating, dip roll coating, bar coating, and knife coating. , air knife coating, curtain coating, lip coating, and extrusion coating using a die coater.
- the amount of the adhesive composition to be applied can be appropriately adjusted according to the desired thickness of the adhesive sheet 1 .
- the drying temperature of the coating film is not particularly limited, and is, for example, 130°C or lower, preferably 125°C or lower, more preferably 120°C or lower, still more preferably 110°C or lower, and particularly preferably 100°C. It is below.
- the drying temperature of the coating film may be 60° C. or higher, or may be 80° C. or higher. When the drying temperature is 60° C. or higher, for example, the reaction of the isocyanate-based cross-linking agent proceeds smoothly, the cohesive force of the adhesive sheet 1 can be improved, and the display unevenness of the image display device tends to be reduced. There is When the drying temperature is 130° C.
- the reaction rate of the isocyanate-based cross-linking agent can be appropriately adjusted, and the compatibility between the (meth)acrylic polymer (A) and the polymer (B) can be maintained satisfactorily. They tend to be able to ensure transparency. In other words, setting the drying temperature to 130° C. or lower tends to reduce the maximum domain diameter of the adhesive sheet 1 .
- the drying time of the coating film can be appropriately adjusted according to the composition of the adhesive composition, preferably 30 seconds to 300 seconds, more preferably 40 seconds to 240 seconds, particularly preferably 60 seconds to 180 seconds. .
- FIG. 5 An example of the optical laminate of this embodiment is shown in FIG.
- An optical laminate 10A in FIG. 5 includes an adhesive sheet 1 and an optical film 2. As shown in FIG. The adhesive sheet 1 and the optical film 2 are laminated together. 10 A of optical laminated bodies can be used as an optical film with an adhesive sheet.
- optical film 2 examples are a polarizing plate, a retardation film, and a laminated film containing a polarizing plate and/or a retardation film.
- the optical film 2 is not limited to the above examples.
- the optical film 2 may contain a film made of glass.
- a polarizing plate is, for example, a laminate containing a polarizer and a transparent protective film.
- the transparent protective film is arranged, for example, in contact with the main surface (the surface having the widest area) of the layered polarizer.
- a polarizer may be placed between two transparent protective films.
- the polarizer is not particularly limited, and various types can be used.
- a polarizer for example, hydrophilic polymer films such as polyvinyl alcohol films, partially formalized polyvinyl alcohol films, and partially saponified ethylene-vinyl acetate copolymer films are added with dichroic properties such as iodine and dichroic dyes. Monoaxially stretched after adsorbing a substance; oriented polyene films such as dehydrated polyvinyl alcohol and dehydrochlorinated polyvinyl chloride.
- a polarizer composed of a polyvinyl alcohol-based film and a dichroic substance such as iodine is preferable, and an iodine-based polarizer containing iodine and/or iodine ions is more preferable.
- the thickness of the polarizer is not particularly limited, it is generally about 5 to 80 ⁇ m.
- a polarizer made by dyeing a polyvinyl alcohol film with iodine and uniaxially stretching it can be produced, for example, by dyeing polyvinyl alcohol by immersing it in an aqueous solution of iodine and stretching it to 3 to 7 times its original length. If necessary, the polyvinyl alcohol can be immersed in an aqueous solution of potassium iodide containing boric acid, zinc sulfate, zinc chloride and the like. Furthermore, if necessary, the polyvinyl alcohol-based film may be immersed in water and washed with water before dyeing.
- the stretching of the polyvinyl alcohol-based film may be performed after dyeing with iodine, may be performed while dyeing, or may be performed before dyeing with iodine. Stretching may be performed in an aqueous solution of boric acid, potassium iodide, or the like, or in a water bath.
- a thin polarizer with a thickness of 10 ⁇ m or less can also be used as the polarizer.
- the thickness of the polarizer is preferably 1 to 7 ⁇ m.
- Such a thin polarizer is preferable because it has little unevenness in thickness, is excellent in visibility, is excellent in durability due to little dimensional change, and is capable of achieving a thin polarizing plate.
- Typical thin polarizers include JP-A-51-069644, JP-A-2000-338329, WO2010/100917, JP-A-4751481, JP-A-2012-073563. can be mentioned thin polarizers described in.
- These thin polarizers can be obtained by a manufacturing method including a step of stretching a polyvinyl alcohol-based resin (hereinafter also referred to as a PVA-based resin) layer and a stretching resin substrate in the state of a laminate, and a step of dyeing. With this manufacturing method, the PVA-based resin layer is supported by the stretching resin base material, so even if the PVA-based resin layer is thin, problems such as breakage due to stretching can be suppressed.
- a method including a step of stretching in an aqueous boric acid solution is preferable, and in particular, auxiliary before stretching in an aqueous boric acid solution described in Japanese Patent No. 4751481 and Japanese Patent Application Laid-Open No. 2012-073563.
- a manufacturing method including a step of stretching in the air is preferred.
- thermoplastic resin that is excellent in transparency, mechanical strength, thermal stability, moisture blocking property, isotropy, etc.
- thermoplastic resins include cellulose resins such as triacetyl cellulose, polyester resins, polyethersulfone resins, polysulfone resins, polycarbonate resins, polyamide resins, polyimide resins, polyolefin resins, (meth)acrylic resins, cyclic Polyolefin resins (norbornene-based resins), polyarylate resins, polystyrene resins, polyvinyl alcohol resins, and mixtures thereof can be used.
- the material of the transparent protective film may be a thermosetting resin such as (meth)acrylic, urethane, acrylic urethane, epoxy, or silicone, or an ultraviolet curable resin.
- a transparent protective film made of a thermoplastic resin is attached to one main surface of the polarizer via an adhesive, and a thermosetting resin or ultraviolet light is applied to the other main surface of the polarizer.
- a transparent protective film made of a curable resin may be attached.
- the transparent protective film may contain one or more optional additives.
- thermoplastic resin content in the transparent protective film is preferably 50 to 100% by weight, more preferably 50 to 99% by weight, even more preferably 60 to 98% by weight, particularly preferably 70 to 97% by weight.
- content of the thermoplastic resin in the transparent protective film is 50% by weight or more, there is a tendency that the high transparency inherent in the thermoplastic resin can be sufficiently exhibited.
- the thickness of the transparent protective film can be determined as appropriate, it is generally about 10 to 200 ⁇ m in terms of strength, workability such as handleability, and thinness.
- the polarizer and transparent protective film are usually in close contact with each other via a water-based adhesive or the like.
- water-based adhesives include isocyanate-based adhesives, polyvinyl alcohol-based adhesives, gelatin-based adhesives, vinyl-based latexes, water-based polyurethanes, and water-based polyesters.
- adhesives other than the adhesives described above include ultraviolet curing adhesives, electron beam curing adhesives, and the like.
- the electron beam curable polarizing plate adhesive exhibits suitable adhesion to various transparent protective films.
- the adhesive may contain a metallic compound filler.
- a retardation film or the like can be formed on the polarizer instead of the transparent protective film.
- the transparent protective film it is also possible to provide another transparent protective film, or to provide a retardation film or the like.
- a hard coat layer may be provided on the surface facing the surface adhered to the polarizer, and it is also possible to apply treatments for the purpose of antireflection, antisticking, diffusion, antiglare, etc. can.
- a retardation film one obtained by stretching a polymer film or one obtained by aligning and fixing a liquid crystal material can be used.
- a retardation film has, for example, birefringence in the plane and/or in the thickness direction.
- antireflection retardation film see JP 2012-133303 [0221], [0222], [0228]
- viewing angle compensation retardation film JP 2012-133303 [0225 ], see [0226]
- oblique orientation retardation film for viewing angle compensation see JP-A-2012-133303 [0227]
- retardation film as long as it substantially has the above functions, for example, retardation value, arrangement angle, three-dimensional birefringence, monolayer or multilayer is not particularly limited, and known retardation film Film can be used.
- the thickness of the retardation film is preferably 20 ⁇ m or less, more preferably 10 ⁇ m or less, still more preferably 1 to 9 ⁇ m, and particularly preferably 3 to 8 ⁇ m.
- a retardation film is composed of two layers, for example, a quarter-wave plate and a half-wave plate in which a liquid crystal material is oriented and fixed.
- FIG. 6 Another example of the optical laminate of this embodiment is shown in FIG.
- the optical layered body 10B of FIG. 6 has a layered structure in which a release liner 3, an adhesive sheet 1 and an optical film 2 are layered in this order. By peeling off the release liner 3, the optical laminate 10B can be used as an optical film with an adhesive sheet.
- Materials constituting the release liner 3 include, for example, plastic films such as polyethylene, polypropylene, polyethylene terephthalate, and polyester films; porous materials such as paper, cloth, and nonwoven fabric; nets, foam sheets, metal foils, and laminates thereof.
- plastic films such as polyethylene, polypropylene, polyethylene terephthalate, and polyester films
- porous materials such as paper, cloth, and nonwoven fabric
- nets, foam sheets, metal foils, and laminates thereof are preferably used because of its excellent surface smoothness.
- the plastic film is not particularly limited as long as it is a film capable of protecting the adhesive sheet 1.
- examples include polyethylene film, polypropylene film, polybutene film, polybutadiene film, polymethylpentene film, polyvinyl chloride film, and vinyl chloride copolymer. film, polyethylene terephthalate film, polybutylene terephthalate film, polyurethane film, ethylene-vinyl acetate copolymer film and the like.
- the thickness of the release liner 3 is usually 5-200 ⁇ m, preferably about 5-100 ⁇ m.
- the release liner 3 may be subjected, if necessary, to silicone-based, fluorine-based, long-chain alkyl-based or fatty acid amide-based release agents, release and antifouling treatment using silica powder, etc., coating type, kneading type, vapor deposition.
- the mold may be subjected to antistatic treatment.
- a release treatment such as silicone treatment, long-chain alkyl treatment, fluorine treatment, etc.
- the release film used when producing the pressure-sensitive adhesive sheet 1 may be used as the release liner 3.
- the optical layered body 10C of FIG. 7 has a laminated structure in which a release liner 3, an adhesive sheet 1, a retardation film 2A, an interlayer adhesive 4 and a polarizing plate 2B are laminated in this order. After peeling off the release liner 3, the optical layered body 10C can be used by attaching it to, for example, an image forming layer.
- a known adhesive can be used for the interlayer adhesive 4 .
- the adhesive sheet 1 may be used as the interlayer adhesive 4 .
- the optical laminate 10D of FIG. 8 has a laminate structure in which a release liner 3, an adhesive sheet 1, a retardation film 2A, an interlayer adhesive 4, a polarizing plate 2B and a protective film 5 are laminated in this order. After peeling off the release liner 3, the optical layered body 10D can be used by attaching it to, for example, an image forming layer.
- the protective film 5 has a function of protecting the outermost optical film 2 (polarizing plate 2B) during distribution and storage of the optical layered body 10D and when the optical layered body 10D is incorporated in an image display device. Moreover, it may be the protective film 5 that functions as a window to an external space when incorporated in the image display device.
- Protective film 5 is typically a resin film.
- the resin constituting the protective film 5 is, for example, polyester such as PET, polyolefin such as polyethylene and polypropylene, acrylic, cycloolefin, polyimide, and polyamide, preferably polyester.
- the protective film 5 is not limited to the above examples.
- the protective film 5 may be a glass film or a laminated film containing a glass film.
- the protective film 5 may be subjected to surface treatments such as antiglare, antireflection, and antistatic.
- the protective film 5 may be bonded to the optical film 2 with any adhesive. Bonding with the adhesive sheet 1 is also possible.
- the optical layered body of the present embodiment can be distributed and stored, for example, as a wound body in which a strip-shaped optical layered body is wound, or as a sheet-shaped optical layered body.
- the optical laminate of this embodiment is typically used in an image display device.
- the image display device is, for example, an EL display such as a liquid crystal display, an organic EL display and an inorganic EL display.
- the image display device 11 of FIG. 9 includes a substrate 7, an image forming layer (for example, an organic EL layer or a liquid crystal layer) 6, an adhesive sheet 1, a retardation film 2A, an interlayer adhesive 4, a polarizing plate 2B and a protective film 5 in this order. It has a laminated structure.
- the image display device 11 has the optical laminates 10B, 10C and 10D shown in FIGS. 6 to 8 (excluding the release liner 3).
- the substrate 7 and the image forming layer 6 may have the same configurations as those of the substrate and the image forming layer provided in a known image display device.
- the image display device 11 in FIG. 9 may be an organic EL display or a liquid crystal display. However, the image display device 11 is not limited to this example.
- the image display device 11 may be an electroluminescence (EL) display, a plasma display (PD), a field emission display (FED: Field Emission Display), or the like.
- EL electroluminescence
- PD plasma display
- FED Field Emission Display
- the image display device 11 can be used for home appliance applications, vehicle applications, public information display (PID) applications, and the like.
- the image display device of this embodiment can have any configuration as long as it includes the optical layered body of this embodiment.
- AIBN 2,2'-azobisisobutyronitrile
- ⁇ Thickness> The thickness of the adhesive sheet and the like was measured using a dial gauge (manufactured by Mitutoyo).
- ⁇ Storage elastic modulus G'> The storage modulus G' of the PSA sheet at 25°C was evaluated by the method described above. Dynamic viscoelasticity measurement was performed using "ARES-G2" manufactured by TA Instruments.
- FIGS. 10 and 11 are TEM images of cross sections of the adhesive sheets of Examples 1 and 2, respectively. As can be seen from FIGS. 10 and 11, no domain could be confirmed from the cross sections of the pressure-sensitive adhesive sheets of Examples 1 and 2. FIG. Similarly, no domain could be confirmed from the cross sections of the pressure-sensitive adhesive sheets of Examples 4 and 5, either.
- FIGS. 12 to 14 are TEM images of cross sections of the adhesive sheets of Example 3 and Comparative Examples 1 and 2, respectively. As can be seen from FIGS. 12 to 14, domains were confirmed from the cross sections of the pressure-sensitive adhesive sheets of Example 3 and Comparative Examples 1 and 2.
- FIG. TEM images of the cross section of these pressure-sensitive adhesive sheets are subjected to image processing, and the maximum diameter of the domains, the shortest distance D between two domains having a diameter of 80% or more of the maximum diameter, The number of domains having a diameter of 80% or more of the maximum diameter and the area ratio R of the domains having a diameter of 80% or more of the maximum diameter were specified.
- Humidification durability (corresponding to an accelerated durability test) of the PSA sheet was evaluated by the following method. First, a pressure-sensitive adhesive sheet-attached circularly polarizing plate having the pressure-sensitive adhesive sheets prepared in Examples and Comparative Examples on one exposed surface was formed. Next, a circularly polarizing plate was fixed to the surface of a glass plate (Eagle XG manufactured by Corning) via the adhesive sheet. Fixing of the circularly polarizing plate was performed in an atmosphere of 23° C. and 50% RH. Next, after treatment in an autoclave at 50 ° C.
- polarizing plate P1> (Production of polarizer) A long polyvinyl alcohol (PVA) resin film (manufactured by Kuraray, product name “PE3000”, thickness 30 ⁇ m) is uniaxially stretched in the longitudinal direction using a roll stretching machine (total stretching ratio 5.9 times) at the same time. , swelling, dyeing, cross-linking, washing and drying were sequentially performed on the resin film to prepare a polarizer having a thickness of 12 ⁇ m. In the swelling treatment, the resin film was stretched 2.2 times while being treated with pure water at 20°C.
- PVA polyvinyl alcohol
- the resin film was stretched 1.4 times while being treated with an aqueous solution containing iodine and potassium iodide at a weight ratio of 1:7 at 30°C.
- the iodine concentration in the aqueous solution was adjusted so that the single transmittance of the polarizer to be produced was 45.0%.
- a two-step process was employed for the cross-linking treatment.
- the resin film was stretched 1.2 times while being treated with an aqueous solution of boric acid and potassium iodide at 40°C.
- the content of boric acid in the aqueous solution used for the first-stage cross-linking treatment was 5.0% by weight, and the content of potassium iodide was 3.0% by weight.
- the resin film was stretched 1.6 times while being treated with an aqueous solution of boric acid and potassium iodide at 65°C.
- the content of boric acid in the aqueous solution used in the second-stage cross-linking treatment was 4.3% by weight, and the content of potassium iodide was 5.0% by weight.
- a potassium iodide aqueous solution at 20° C. was used for the cleaning treatment.
- the content of potassium iodide in the aqueous solution used for the cleaning treatment was 2.6% by weight.
- the drying treatment was performed under drying conditions of 70° C. and 5 minutes.
- polarizing plate P1 Preparation of polarizing plate P1
- TAC triacetyl cellulose
- KC2UA product name “KC2UA”, thickness 25 ⁇ m
- a hard coat 7 ⁇ m thick
- ⁇ Preparation of retardation film R1> (Preparation of first retardation film) Isosorbide (ISB) 26.2 parts by weight, 9,9-[4-(2-hydroxyethoxy)phenyl]fluorene (BHEPF) 100.5 parts by weight, 1,4-cyclohexanedimethanol (1,4-CHDM) 10 .7 parts by weight, 105.1 parts by weight of diphenyl carbonate (DPC), and 0.591 parts by weight of cesium carbonate (0.2% by weight aqueous solution) as a catalyst were charged into a reaction vessel and dissolved under a nitrogen atmosphere ( about 15 minutes). At this time, the temperature of the heat medium in the reaction vessel was set at 150° C., and stirring was carried out as necessary.
- the pressure inside the reaction vessel was reduced to 13.3 kPa, and the temperature of the heat medium was raised to 190° C. in 1 hour. Phenol generated as the temperature of the heat medium increased was discharged out of the reaction vessel (the same applies hereinafter).
- the pressure in the reaction vessel was changed to 6.67 kPa, and the temperature of the heat medium was raised to 230° C. in 15 minutes.
- the stirring torque of the stirrer provided in the reaction vessel increased, the temperature of the heat medium was raised to 250° C. in 8 minutes, and the pressure in the reaction vessel was reduced to 0.200 kPa or less.
- a single screw extruder manufactured by Isuzu Kakoki, screw diameter 25 mm, cylinder set temperature 220 ° C.), T die (width 200 mm, set temperature 220 ° C.), chill roll A long resin film having a thickness of 120 ⁇ m was obtained using a film forming apparatus equipped with a set temperature of 120 to 130° C. and a winder. Next, the obtained resin film was stretched in the width direction with a tenter stretching machine at a stretching temperature of 137 to 139° C. and a stretching ratio of 2.5 to obtain a first retardation film.
- a side chain type liquid crystal polymer (weight average molecular weight 5000) represented by the following chemical formula (I) (where 65 and 35 are mol% of each structural unit), a polymerizable liquid crystal exhibiting a nematic liquid crystal phase (manufactured by BASF) , trade name “Paliocolor LC242”) 80 parts by weight, and a photopolymerization initiator (manufactured by Ciba Specialty Chemicals, trade name “Irgacure 907”) 5 parts by weight are dissolved in 200 parts by weight of cyclopentanone to form a liquid crystal coating liquid.
- a side chain type liquid crystal polymer (weight average molecular weight 5000) represented by the following chemical formula (I) (where 65 and 35 are mol% of each structural unit)
- a polymerizable liquid crystal exhibiting a nematic liquid crystal phase manufactured by BASF
- Paliocolor LC242 trade name “Paliocolor LC242”
- a norbornene-based resin film manufactured by Nippon Zeon, trade name “Zeonex”
- Zeonex which is a base film
- the coating film was cured by irradiation with ultraviolet rays to form a liquid crystal solidified layer (thickness: 0.58 ⁇ m) as a second retardation film on the substrate film.
- the polymerization reaction was allowed to proceed for 7 hours while maintaining the liquid temperature in the flask around 55°C.
- ethyl acetate was added to the resulting reaction solution to adjust the solid content concentration to 30% by weight to obtain a solution of a (meth)acrylic polymer used as an interlaminar pressure-sensitive adhesive.
- the weight average molecular weight of the obtained polymer was 2,200,000.
- trimethylolpropane/tolylene diisocyanate trimer adduct manufactured by Tosoh, trade name "Coronate L" is added to 100 parts by weight of the solid content of the solution.
- the pressure-sensitive adhesive composition PSA1 prepared above is applied to the release surface of a polyethylene terephthalate (PET) film (manufactured by Mitsubishi Chemical Polyester Film Co., Ltd., MRF38) having a thickness of 38 ⁇ m, which is a release film having a silicone-treated release surface. It was coated so that the thickness of the layer after drying was 12 ⁇ m, and dried at 155° C. for 1 minute to form an interlayer pressure-sensitive adhesive layer. Next, the formed interlayer pressure-sensitive adhesive layer was transferred to the protective layer (no hard coat) side of the polarizing plate P1 to obtain a polarizing plate with an interlayer pressure-sensitive adhesive layer.
- PET polyethylene terephthalate
- MRF38 silicone-treated release surface
- each pressure-sensitive adhesive sheet prepared in Examples and Comparative Examples was transferred from the release film and pasted.
- the polarizing plate with an interlayer pressure-sensitive adhesive layer prepared above was attached to the first retardation film side of the retardation film R1 via the interlayer pressure-sensitive adhesive layer to obtain a circularly polarizing plate with an pressure-sensitive adhesive sheet.
- the attachment of the retardation film R1 and the polarizing plate with an interlayer pressure-sensitive adhesive layer is performed by adjusting the angle formed by the slow axis of the first retardation film and the absorption axis of the polarizer when viewed from the side of the first retardation film. was 45 degrees counterclockwise.
- the domains could not be confirmed, or even if they could be confirmed, the maximum diameter was 170 nm or less, and the maximum diameter was 170 nm or less compared to the pressure-sensitive adhesive sheets of Comparative Examples. It was small.
- the pressure-sensitive adhesive sheets of Examples having domains with a maximum diameter of 170 nm or less had improved durability compared to the pressure-sensitive adhesive sheets of Comparative Examples.
- the adhesive sheet of the present invention can be suitably used for image display devices such as EL displays and liquid crystal displays.
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Abstract
Description
25℃の貯蔵弾性率G’が0.4MPa以上である粘着シートであって、
前記粘着シートの断面を透過型電子顕微鏡で観察したときに、縦6μm×横6μmの範囲内におけるドメインの最大径が170nm以下である、粘着シートを提供する。
上記の粘着シートと、光学フィルムと、を含む、光学積層体を提供する。
上記の光学積層体を備える画像表示装置を提供する。
上記の粘着シートの製造方法であって、
(メタ)アクリル系ポリマー(A)及びイソシアネート系架橋剤を含む粘着剤組成物を基材に塗布し、塗布膜を形成することと、
前記塗布膜を乾燥させることと、
を含む、粘着シートの製造方法を提供する。
本実施形態の粘着シートの一例を図1に示す。本実施形態の粘着シート1は、25℃の貯蔵弾性率G’が0.4MPa以上である。さらに、粘着シート1の断面を透過型電子顕微鏡(TEM)で観察したときに、縦6μm×横6μmの範囲内におけるドメインの最大径が170nm以下である。本明細書において、ドメインとは、粘着シートに形成された海島構造の島状相を意味する。ドメインは、通常、実質的に円形の島状領域として観察される。
・測定条件
周波数:1Hz
変形モード:ねじり
測定温度:-70℃~150℃
昇温速度:5℃/分
ゲル分率(重量%)=(C-B)/(A-B)×100
Xmax≧0.5MPa (1)
ただし、ピークトップ応力Xmaxは、粘着シート1に対する以下の評価試験により求めた応力-歪み曲線における応力Xのピーク値である。
粘着シート1の応力-歪み曲線を求める評価試験について、図2A~図2Dを参照しながら説明する。最初に、ガラス板51に貼り付けた粘着シート1の粘着面11(露出面)に対して評価用プローブ52(直径5mmの円柱状、ステンレス製)の端面53を接触させ、粘着シート1の厚さ方向に100Nの接触荷重54を加えながら300秒間保持して、評価用プローブ52と粘着シート1とを密着させる(図2A,図2B)。端面53は、プローブ52の底面であり、その直径は5mmである。応力X及び歪みYを精度よく測定するためには、貼り付ける粘着シート1の厚さを200μm以上とすることが好ましい。厚さが200μmに達しない場合は、2以上の粘着シート1を重ね、オートクレーブ等を用いた加熱Iにより互いに接合することで、厚さ200μm以上としてもよい。ガラス板51には、粘着シート1を貼り付ける面が平坦であると共に、評価試験中に粘着シート1が剥離しないものを選択できる。ガラス板51への粘着シート1の貼り付けは、評価試験中に粘着シート1が剥離しないように実施すればよい。必要に応じて、オートクレーブ等を用いた加熱IIにより、粘着シート1とガラス板51との接合の状態を安定させてもよい。加熱I及び加熱IIの条件は、例えば、30~90℃及び0.5~4時間であり、オートクレーブを使用する場合は、例えば、30~70℃、5~30分及び2~10気圧(絶対圧)である。加熱I及び加熱IIは、重ねた粘着シート1をガラス板51に貼り付けた状態で、同時に実施してもよい。評価用プローブ52には、ASTM D-2979の規定に準拠したプローブタック試験用プローブを利用できる。
Ym≧0.05 (2)
Y0.15≧0.28 (3)
Y0.15/Ym≧2 (4)
(メタ)アクリル系ポリマー(A)は、アクリル系粘着剤のベースポリマーとして機能しうる。アクリル系粘着剤は、光学的透明性に優れ、適切な濡れ性、凝集性、接着性などの粘着特性を有し、耐候性、耐熱性等に優れる傾向がある。(メタ)アクリル系ポリマー(A)は、例えば、アルキル(メタ)アクリレートに由来する構成単位を主成分として含有する。本明細書において、「(メタ)アクリレート」は、アクリレート及び/又はメタクリレートを意味する。
イソシアネート系架橋剤としては、少なくとも2個のイソシアネート基を有する化合物(イソシアネート化合物)を用いることができる。イソシアネート化合物に含まれるイソシアネート基の数は、3以上であることが好ましい。イソシアネート基の数の上限値は、特に限定されず、例えば5である。イソシアネート化合物としては、芳香族イソシアネート化合物、脂環族イソシアネート化合物、脂肪族イソシアネート化合物などが挙げられる。イソシアネート系架橋剤は、水と反応することによって自己重合できることが好ましい。
粘着剤組成物は、イソシアネート系架橋剤以外の他の架橋剤を含んでいてもよい。他の架橋剤としては、過酸化物系架橋剤、エポキシ系架橋剤、イミン系架橋剤、多官能性金属キレートなどが挙げられる。他の架橋剤の配合量は、(メタ)アクリル系ポリマー(A)100重量部に対して、2重量部以下が好ましく、1重量部以下がより好ましい。粘着シートの耐久性の観点から、粘着剤組成物は、他の架橋剤、特にエポキシ系架橋剤、を実質的に含まないことが好ましい。
本実施形態の光学積層体の一例を図5に示す。図5の光学積層体10Aは、粘着シート1と光学フィルム2とを含む。粘着シート1と光学フィルム2とは互いに積層されている。光学積層体10Aは、粘着シート付き光学フィルムとして使用できる。
本実施形態の画像表示装置の一例を図9に示す。図9の画像表示装置11は、基板7、画像形成層(例えば有機EL層又は液晶層)6、粘着シート1、位相差フィルム2A、層間粘着剤4、偏光板2B及び保護フィルム5がこの順に積層された積層構造を有している。画像表示装置11は、図6~8の光学積層体10B,10C,10Dを有している(ただし、はく離ライナー3を除く)。基板7及び画像形成層6は、公知の画像表示装置が備える基板及び画像形成層と、それぞれ同様の構成を有していればよい。
攪拌羽根、温度計、窒素ガス導入管、冷却器を備えた4つ口フラスコに、ブチルアクリレート(BA)94.9重量部、アクリル酸(AA)5重量部、4-ヒドロキシブチルアクリレート0.1重量部を含有する単量体混合物を仕込んだ。さらに、単量体混合物100重量部に対して、重合開始剤として2,2’-アゾビスイソブチロニトリル(AIBN)0.1重量部を酢酸エチルと共に仕込み、緩やかに攪拌しながら窒素ガスを導入して窒素置換した後、フラスコ内の液温を55℃付近に保って7時間重合反応を行った。その後、得られた反応液に酢酸エチルを加えて、固形分濃度30%に調整して、(メタ)アクリル系ポリマーA1の溶液を得た。
使用する単量体を表1のように変更したことを除き、(メタ)アクリル系ポリマーA1と同じ方法で、(メタ)アクリル系ポリマーA2の溶液を調製した。
BA:n-ブチルアクリレート
BzA:ベンジルアクリレート
AA:アクリル酸
HBA:4-ヒドロキシブチルアクリレート
AIBN:アゾ系重合開始剤、2,2’-アゾビスイソブチロニトリル(キシダ化学社製)
(実施例1~5及び比較例1~2)
以下の表2に示す組成となるように(メタ)アクリル系ポリマー、架橋剤及び添加剤を混合して、溶剤型の粘着剤組成物を得た。次に、基材フィルム(はく離ライナー)であるPETフィルムの表面に、乾燥後の粘着シートの厚さが15μmになるように粘着剤組成物を塗布した。粘着剤組成物の塗布には、ファウンテンコーターを使用した。得られた塗布膜を表2に示す乾燥温度に設定した空気循環式恒温オーブンにて1分間乾燥させて、実施例1~5及び比較例1~2の粘着シートを形成した。
C/L:トリメチロールプロパン/トリレンジイソシアネート(東ソー社製、商品名:コロネートL)
KBM403:γ-グリシドキシプロピルトリメトキシシラン(信越化学工業社製)
<(メタ)アクリル系ポリマーの重量平均分子量(Mw)>
得られた(メタ)アクリル系ポリマーの重量平均分子量(Mw)は、GPC(ゲル・パーミエーション・クロマトグラフィー)により測定した。
・分析装置:東ソー社製、HLC-8120GPC
・カラム:東ソー社製、G7000HXL+GMHXL+GMHXL
・カラムサイズ:各7.8mmφ×30cm 計90cm
・カラム温度:40℃
・流量:0.8ml/min
・注入量:100μl
・溶離液:テトラヒドロフラン
・検出器:示差屈折計(RI)
・標準試料:ポリスチレン
粘着シート等の厚みは、ダイヤルゲージ(ミツトヨ製)を用いて測定した。
作製した粘着シートに対するゲル分率の評価は、上述の方法により実施した。粘着シートの一部を掻き取って得られた小片の重量は、約0.2gであった。ポリテトラフルオロエチレンの延伸多孔質膜には、日東電工製NTF1122(平均孔径0.2μm)を用いた。
粘着シートの25℃における貯蔵弾性率G’の評価は、上述の方法により実施した。動的粘弾性測定は、TA Instruments社製「ARES-G2」を用いて行った。
TEMによる粘着シートの断面の観察は、次の方法によって行った。まず、粘着シートに、重金属(RuO4)染色処理を施した。次に、この粘着シートを樹脂に包埋した。超薄切片法によって、包埋処理を行った粘着シートを切断し、厚さ約100nmの測定試料を作製した。得られた測定試料の断面をTEMによって観察した。TEMとしては、日立ハイテク社製のHT7820を用いた。TEM観察では、加速電圧を100kVに設定し、拡大倍率を20,000倍に設定した。
粘着シートの加湿耐久性(耐久性の加速試験に相当)は、以下の方法により評価した。最初に、実施例及び比較例で作製した各粘着シートを一方の露出面に備える粘着シート付き円偏光板を形成した。次に、上記粘着シートを介して、ガラス板(コーニング製、イーグルXG)の表面に円偏光板を固定した。円偏光板の固定は、23℃及び50%RHの雰囲気で実施した。次に、50℃及び5気圧(絶対圧)のオートクレーブにて15分処理した後、23℃に冷えるまで放置して、ガラス板への円偏光板の接合を安定させた後、60℃及び95%RHの加熱加湿雰囲気に500時間放置した。放置後、23℃及び50%RHの雰囲気に戻し、ガラス板からの円偏光板の剥がれや、ガラス板と円偏光板との間に発泡が生じていないかを目視により確認して、以下のように、加湿耐久性を評価した。
A:発泡や剥がれ等の外観上の変化がみられない。
B:端部において、単独の剥がれ又は発泡がわずかにみられるが、実用上、問題ない範囲にある。
C:端部において、連続した剥がれ又は発泡がわずかにみられるが、実用上、問題ない範囲にある。
D:端部に著しい剥がれ又は発泡がみられ、実用上、問題がある。
(偏光子の作製)
長尺状のポリビニルアルコール(PVA)系樹脂フィルム(クラレ製、製品名「PE3000」、厚さ30μm)を、ロール延伸機を用いて長手方向に一軸延伸(総延伸倍率5.9倍)すると同時に、上記樹脂フィルムに対して膨潤、染色、架橋、洗浄及び乾燥の各処理を順に施して、厚さ12μmの偏光子を作製した。膨潤処理では、上記樹脂フィルムを20℃の純水で処理しながら2.2倍延伸した。染色処理では、ヨウ素及びヨウ化カリウムを重量比1:7で含有する30℃の水溶液で処理しながら、上記樹脂フィルムを1.4倍延伸した。水溶液中のヨウ素濃度は、作製する偏光子の単体透過率が45.0%となるように調整された。架橋処理には、2段階処理を採用した。1段階目の架橋処理では、ホウ酸及びヨウ化カリウムを溶解させた40℃の水溶液で処理しながら、上記樹脂フィルムを1.2倍延伸した。1段階目の架橋処理に用いた水溶液におけるホウ酸の含有率は5.0重量%、ヨウ化カリウムの含有率は3.0重量%とした。2段階目の架橋処理では、ホウ酸及びヨウ化カリウムを溶解させた65℃の水溶液で処理しながら、上記樹脂フィルムを1.6倍延伸した。2段階目の架橋処理に用いた水溶液におけるホウ酸の含有率は4.3重量%、ヨウ化カリウムの含有率は5.0重量%とした。洗浄処理には、20℃のヨウ化カリウム水溶液を用いた。洗浄処理に用いた水溶液におけるヨウ化カリウムの含有率は2.6重量%とした。乾燥処理は、70℃及び5分間の乾燥条件で実施した。
上記作製した偏光子の各主面に、それぞれ、トリアセチルセルロース(TAC)フィルム(コニカミノルタ製、製品名「KC2UA」、厚さ25μm)をポリビニルアルコール系接着剤により貼り合わせた。ただし、一方の主面に貼り合わせたTACフィルムには、偏光子側とは反対側の主面にハードコート(厚さ7μm)が形成されていた。このようにして、ハードコート付き保護層/偏光子/保護層(ハードコートなし)の構成を有する偏光板P1を得た。
(第1の位相差フィルムの作製)
イソソルビド(ISB)26.2重量部、9,9-[4-(2-ヒドロキシエトキシ)フェニル]フルオレン(BHEPF)100.5重量部、1,4-シクロヘキサンジメタノール(1,4-CHDM)10.7重量部、ジフェニルカーボネート(DPC)105.1重量部、及び触媒として炭酸セシウム(0.2重量%水溶液)0.591重量部を反応容器に投入し、窒素雰囲気下にて溶解させた(約15分)。このとき、反応容器の熱媒温度は150℃とし、必要に応じて撹拌を実施した。次に、反応容器内の圧力を13.3kPaに減圧すると共に、熱媒温度を190℃まで1時間で上昇させた。熱媒温度の上昇に伴って発生するフェノールは、反応容器外へ抜き出した(以下、同じ)。次に、反応容器内の温度を190℃で15分保持した後、反応容器内の圧力を6.67kPaに変更すると共に、熱媒温度を230℃まで15分で上昇させた。反応容器が備える撹拌機の撹拌トルクが上昇してきた時点で、熱媒温度を250℃まで8分で上昇させ、更に、反応容器内の圧力を0.200kPa以下とした。所定の撹拌トルクに到達後、反応を終了させ、生成した反応物を水中に押し出してペレット化した。このようにして、BHEPF/ISB/1,4-CHDM=47.4モル%/37.1モル%/15.5モル%の組成を有するポリカーボネート樹脂を得た。得られたポリカーボネート樹脂のガラス転移温度は136.6℃であり、還元粘度は0.395dL/gであった。
下記化学式(I)(式中、65及び35は、各構成単位のモル%)により示される側鎖型液晶ポリマー(重量平均分子量5000)20重量部、ネマチック液晶相を示す重合性液晶(BASF製、商品名「PaliocolorLC242」)80重量部、及び光重合開始剤(チバスペシャリティーケミカルズ製、商品名「イルガキュア907」)5重量部をシクロペンタノン200重量部に溶解して、液晶塗工液を調製した。次に、基材フィルムであるノルボルネン系樹脂フィルム(日本ゼオン製、商品名「ゼオネックス」)の表面に、調製した液晶塗工液をバーコーターにより塗工した後、80℃で4分間、加熱及び乾燥させて、塗布膜に含まれる液晶を配向させた。次に、紫外線の照射により塗布膜を硬化させて、第2の位相差フィルムである液晶固化層(厚さ0.58μm)を基材フィルム上に形成した。波長550nmの光に対する液晶固化層の面内位相差Reは0nm、厚さ方向の位相差Rthは-71nmであり(nx=1.5326、ny=1.5326、nz=1.6550)、液晶固化層は、nz>nx=nyの屈折率特性を示した。
上記作製した第1の位相差フィルムの一方の面と、第2の位相差フィルムの液晶固化層とを接着剤を介して貼合せて、位相差フィルムR1を作製した。
(層間粘着剤の作製)
撹拌羽根、温度計、窒素ガス導入管、及び冷却器を備えた4つ口フラスコに、ブチルアクリレート79.9重量部、ベンジルアクリレート15重量部、アクリル酸5重量部及び4-ヒドロキシブチルアクリレート0.1重量部を含有する単量体混合物を仕込んだ。次に、単量体混合物100重量部に対して、重合開始剤として2,2’-アゾイソブチロニトリル0.1重量部を酢酸エチルと共に加え、緩やかに撹拌しながら窒素ガスを導入してフラスコ内を窒素置換した後、フラスコ内の液温を55℃付近に保って重合反応を7時間進行させた。次に、得られた反応液に酢酸エチルを加えて固形分濃度30重量%に調整して、層間粘着剤に使用する(メタ)アクリル系ポリマーの溶液を得た。得られたポリマーの重量平均分子量は、220万であった。
上記作製した粘着剤組成物PSA1を、剥離面にシリコーン処理が施された剥離フィルムである、厚さ38μmのポリエチレンテレフタレート(PET)フィルム(三菱化学ポリエステルフィルム製、MRF38)の剥離面に対して、乾燥後の層の厚さが12μmとなるように塗布し、155℃で1分間乾燥処理して、層間粘着剤層を形成した。次に、形成した層間粘着剤層を偏光板P1における保護層(ハードコートなし)側に転写して、層間粘着剤層付き偏光板を得た。
位相差フィルムR1における第2の位相差フィルム側(第2の位相差フィルムを作製する際に基材フィルムとして用いたノルボルネン系樹脂フィルムは剥離)に、実施例及び比較例で作製した各粘着シートを剥離フィルムから転写して貼りつけた。次に、位相差フィルムR1における第1の位相差フィルム側に、上記作製した層間粘着剤層付き偏光板を、層間粘着剤層を介して貼りつけて、粘着シート付き円偏光板を得た。位相差フィルムR1と層間粘着剤層付き偏光板との貼りつけは、第1の位相差フィルムの側から見て、第1の位相差フィルムの遅相軸と偏光子の吸収軸との成す角度が反時計回りに45度となるように実施した。
Claims (15)
- 25℃の貯蔵弾性率G’が0.4MPa以上である粘着シートであって、
前記粘着シートの断面を透過型電子顕微鏡で観察したときに、縦6μm×横6μmの範囲内におけるドメインの最大径が170nm以下である、粘着シート。 - 2種類以上のポリマーを含む、請求項1に記載の粘着シート。
- 前記粘着シートの断面を透過型電子顕微鏡で観察したときに、縦6μm×横6μmの範囲内に複数のドメインが存在し、
前記複数のドメインのうち、前記最大径の80%以上の大きさの径を有する2つのドメインの間の最短距離が350nm以上である、請求項1又は2に記載の粘着シート。 - 前記粘着シートの断面を透過型電子顕微鏡で観察したときに、縦6μm×横6μmの範囲内において、前記最大径の80%以上の大きさの径を有するドメインの数が20個以下である、請求項1~3のいずれか1項に記載の粘着シート。
- 前記粘着シートの断面を透過型電子顕微鏡で観察したときに、縦6μm×横6μmの範囲内において、前記最大径の80%以上の大きさの径を有するドメインの面積の比率が0.7%以下である、請求項1~4のいずれか1項に記載の粘着シート。
- (メタ)アクリル系ポリマー(A)及びイソシアネート系架橋剤を含む粘着剤組成物から形成された、請求項1~5のいずれか1項に記載の粘着シート。
- 前記ドメインは、前記イソシアネート系架橋剤に由来する構成単位を主成分として含むポリマー(B)から実質的に構成されている、請求項6に記載の粘着シート。
- 前記粘着剤組成物における前記イソシアネート系架橋剤の配合量が、前記(メタ)アクリル系ポリマー(A)100重量部に対して5重量部以上である、請求項6又は7に記載の粘着シート。
- 前記粘着剤組成物における前記イソシアネート系架橋剤の配合量が、前記(メタ)アクリル系ポリマー(A)100重量部に対して15重量部以下である、請求項6~8のいずれか1項に記載の粘着シート。
- 前記イソシアネート系架橋剤は、トリレンジイソシアネート系架橋剤である、請求項6~9のいずれか1項に記載の粘着シート。
- 前記(メタ)アクリル系ポリマー(A)は、芳香環含有単量体に由来する構成単位を含む、請求項6~10のいずれか1項に記載の粘着シート。
- 請求項1~11のいずれか1項に記載の粘着シートと、光学フィルムと、を含む、光学積層体。
- 請求項12に記載の光学積層体を備える画像表示装置。
- 請求項1~11のいずれか1項に記載の粘着シートの製造方法であって、
(メタ)アクリル系ポリマー(A)及びイソシアネート系架橋剤を含む粘着剤組成物を基材に塗布し、塗布膜を形成することと、
前記塗布膜を乾燥させることと、
を含む、粘着シートの製造方法。 - 130℃以下の温度で前記塗布膜を乾燥させる、請求項14に記載の製造方法。
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JP2016188310A (ja) * | 2015-03-30 | 2016-11-04 | 日本カーバイド工業株式会社 | 粘着剤組成物及び粘着シート |
JP6484484B2 (ja) * | 2015-03-30 | 2019-03-13 | 日本カーバイド工業株式会社 | 粘着剤組成物及び粘着シート |
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JP2016188310A (ja) * | 2015-03-30 | 2016-11-04 | 日本カーバイド工業株式会社 | 粘着剤組成物及び粘着シート |
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