WO2022071212A1 - Feuille adhésive sensible à la pression optique avec séparateur - Google Patents

Feuille adhésive sensible à la pression optique avec séparateur Download PDF

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Publication number
WO2022071212A1
WO2022071212A1 PCT/JP2021/035339 JP2021035339W WO2022071212A1 WO 2022071212 A1 WO2022071212 A1 WO 2022071212A1 JP 2021035339 W JP2021035339 W JP 2021035339W WO 2022071212 A1 WO2022071212 A1 WO 2022071212A1
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WO
WIPO (PCT)
Prior art keywords
separator
less
adhesive sheet
sensitive adhesive
optical
Prior art date
Application number
PCT/JP2021/035339
Other languages
English (en)
Japanese (ja)
Inventor
和広 山村
新 藤原
崇弘 野中
Original Assignee
日東電工株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from JP2021155316A external-priority patent/JP2022058223A/ja
Application filed by 日東電工株式会社 filed Critical 日東電工株式会社
Priority to CN202180066897.6A priority Critical patent/CN116323191A/zh
Priority to KR1020237009951A priority patent/KR20230075430A/ko
Publication of WO2022071212A1 publication Critical patent/WO2022071212A1/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
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/40—Adhesives in the form of films or foils characterised by release liners
    • C09J7/405—Adhesives in the form of films or foils characterised by release liners characterised by the substrate of the release liner
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/10—Adhesives in the form of films or foils without carriers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/38—Pressure-sensitive adhesives [PSA]
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/40—Adhesives in the form of films or foils characterised by release liners
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/40—Adhesives in the form of films or foils characterised by release liners
    • C09J7/401—Adhesives in the form of films or foils characterised by release liners characterised by the release coating composition
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/88—Investigating the presence of flaws or contamination
    • G01N21/89—Investigating the presence of flaws or contamination in moving material, e.g. running paper or textiles
    • G01N21/892—Investigating the presence of flaws or contamination in moving material, e.g. running paper or textiles characterised by the flaw, defect or object feature examined
    • 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 optical adhesive sheet with a separator.
  • the light-transmitting adhesive sheet (optical adhesive sheet) is used for manufacturing optical articles such as display panels.
  • the display panel has a laminated structure including a pixel panel, a cover member, and the like.
  • the optical adhesive sheet is used for joining elements included in the laminated structure on the light emitting side (image display side) of the pixel panel.
  • the optical adhesive sheet is an adhesive sheet arranged at a place where light passes in the optical article.
  • the optical pressure-sensitive adhesive sheet is manufactured, for example, in the form of an optical pressure-sensitive adhesive sheet with a separator in which one side or both sides of the sheet is coated with a separator (peeling liner).
  • a technique relating to such an optical adhesive sheet is described in, for example, Patent Document 1 below.
  • the present invention provides an optical adhesive sheet with a separator suitable for manufacturing an optical article having a high degree of cleanliness at a light passing portion.
  • the present invention is an optical pressure-sensitive adhesive sheet with a separator including a pressure-sensitive adhesive layer and a separator arranged on one side in the thickness direction of the pressure-sensitive adhesive layer, and is a projection surface of a plan view projection by the following evaluation method.
  • a separator including a pressure-sensitive adhesive layer and a separator arranged on one side in the thickness direction of the pressure-sensitive adhesive layer, and is a projection surface of a plan view projection by the following evaluation method.
  • Evaluation method Perform the following steps 1 to 3 using a device equipped with the following light source and camera device.
  • Light source White LED light source for irradiating the sample for evaluation with inspection light
  • Camera device The sample transmitted light and sample reflected light of the inspection light are arranged so as to be able to be imaged, and have a resolution of 2.8 ⁇ m. , Camera device
  • First step The optical adhesive sheet with a separator having a plan view size of 50 mm ⁇ 50 mm is prepared as a sample for evaluation, and the inner region (30 mm ⁇ 30 mm) surrounded by the outer region in the sample is imaged by the camera device.
  • the sample is set in the apparatus in a state where it can be used.
  • Second step While irradiating the sample with inspection light from the white LED light source, the camera device is used to receive the sample transmitted light and / or the sample reflected light, and the received light data is transmitted over the inner region. get.
  • Third step Using the received light data, the position information and the projected image information of the foreign matter on the projection surface of the plan view projection of the inner region are derived.
  • the present invention [2] includes the optical pressure-sensitive adhesive sheet with a separator according to the above [1], further comprising a separator arranged on the other side in the thickness direction of the pressure-sensitive adhesive layer.
  • the present invention [3] includes the optical pressure-sensitive adhesive sheet with a separator according to the above [1] or [2], wherein the maximum length of the maximum foreign matter in the plan view projection is 30 ⁇ m or less.
  • the present invention [4] is described in any one of the above [1] to [3], wherein the separator has a ratio of the total projected area of foreign substances on the projection surface of the plan view projection to 20% or less. Includes optical adhesive sheet with separator.
  • the optical adhesive with a separator according to any one of the above [1] to [4], wherein the separator has a maximum length of 30 ⁇ m or less in the maximum foreign matter in the plan view projection. Includes sheet.
  • the separator according to any one of the above [1] to [5], wherein the separator has a maximum length of 20 ⁇ m or more and 30 ⁇ m or less and the number of foreign substances is 5 or less in the plan view projection. Includes optical adhesive sheet with.
  • the present invention [7] is any one of the above [1] to [6], wherein the maximum length of the maximum foreign matter between the pressure-sensitive adhesive layer and the separator is 30 ⁇ m or less in the plan view projection. Includes the optical adhesive sheet with separator described in one.
  • the present invention [8] is the optical adhesive with a separator according to any one of the above [1] to [7], wherein the ratio of the total projected area of bubbles on the projection surface of the plan view projection is 10% or less. Includes sheet.
  • the present invention [9] includes the optical pressure-sensitive adhesive sheet with a separator according to any one of the above [1] to [8], wherein the separator has a surface with a surface roughness Ra of 20 nm or less.
  • the ratio of the total projected area of foreign matter on the projection surface of the plan view projection by the above evaluation method is 20% or less.
  • environmental foreign matter is suppressed from adhering to the pressure-sensitive adhesive layer until the separator is peeled off from the pressure-sensitive adhesive layer.
  • Such an optical pressure-sensitive adhesive sheet with a separator is suitable for supplying an adhesive layer having a high degree of cleanliness as an optical pressure-sensitive adhesive sheet in the process of manufacturing an optical article, and therefore, an optical article having a high degree of cleanliness at a light passing portion is manufactured. Suitable for.
  • the optical pressure-sensitive adhesive sheet X with a separator as an embodiment of the optical pressure-sensitive adhesive sheet with a separator of the present invention includes a first separator 10 (separator 10A), an optical pressure-sensitive adhesive sheet 20, and a second separator. 10 (separator 10B) is provided in this order in the thickness direction D.
  • the optical adhesive sheet X with a separator has a sheet shape and extends in a direction (plane direction) orthogonal to the thickness direction D.
  • the separator 10 is a protective film for an optical adhesive sheet.
  • the separator 10A is arranged on one surface of the optical adhesive sheet 20 in the thickness direction D
  • the separator 10B is arranged on the other surface of the optical adhesive sheet 20 in the thickness direction D.
  • the optical pressure-sensitive adhesive sheet X with a separator does not have to include one of the separators 10.
  • the optical pressure-sensitive adhesive sheet X with a separator takes, for example, a roll (not shown) in a state where both sides or one side is covered with the separator 10.
  • the optical adhesive sheet 20 is an adhesive sheet having a transparent adhesive layer 21 arranged at a light passing portion of the optical article, and is used as a component of the optical article.
  • the optical article include a display panel.
  • the display panel has a laminated structure including a pixel panel, a cover member, and the like. In the process of manufacturing a display panel, predetermined elements arranged on the image display side of the pixel panel are bonded to each other by, for example, an optical adhesive sheet.
  • Such a display panel includes an ultra-high-definition display panel for VR (Virtual Reality) applications or AR (Augmented Reality) applications.
  • the optical adhesive sheet X with a separator has a total ratio of foreign matter projected areas (foreign matter area ratio R1) on the projection surface of the plan view projection by the following evaluation method of 20% or less.
  • Foreign substances include environmental foreign substances, foreign substances as impurities of raw materials, foreign substances caused by material modification, and air bubbles. Examples of environmental foreign substances include fiber pieces, skin pieces, metal fine particles, fine oil droplets, and salt fine particles derived from sweat. These foreign substances are sometimes referred to as defects in separators and optical adhesive sheets.
  • Evaluation method Perform the following first to third steps using an evaluation device equipped with the following light source and camera device.
  • Light source White LED light source for irradiating the sample for evaluation with inspection light
  • Camera device The sample transmitted light and sample reflected light of the inspection light are arranged so as to be able to be imaged, and have a resolution of 2.8 ⁇ m. , Camera device
  • First step An optical adhesive sheet X with a separator having a plan view size of 50 mm ⁇ 50 mm is prepared as a sample for evaluation, and an inner region (30 mm ⁇ 30 mm) surrounded by an outer region in the sample is imaged by the camera device.
  • the sample is set in the evaluation device when it is ready.
  • the sample transmitted light is light that transmits the sample in the thickness direction.
  • the sample reflected light is the light reflected by the sample.
  • Third step Using the received light data, the position information and the projected image information of the foreign matter (each of the foreign matter existing in the inner region) on the projection surface of the plan view projection of the inner region are derived.
  • the above evaluation method may be carried out in the manufacturing process of the optical adhesive sheet 20.
  • the above evaluation method may be carried out as a precise foreign matter inspection (defect inspection) for checking the presence or absence of minute foreign matter on the optical adhesive sheet 20.
  • the optical adhesive sheet 20 is exposed to the optical adhesive sheet 20 from one side of the sheet through the separator 10. It is irradiated with inspection light.
  • Visible light is used as the inspection light.
  • the wavelength of visible light as inspection light is included in the range of, for example, 400 to 800 nm.
  • a white LED light source is used as the light source of this visible light.
  • Infrared rays may be used as the inspection light.
  • the wavelength of infrared rays as inspection light is included in the range of, for example, 800 to 1200 nm.
  • an infrared lamp is used as the light source of this infrared ray.
  • the foreign matter area ratio R1 described above is 20% or less, and environmental foreign matter is suppressed from adhering to the optical adhesive sheet 20 until the separator 10 is peeled off from the optical adhesive sheet 20. Will be done.
  • Such an optical pressure-sensitive adhesive sheet X with a separator is suitable for supplying an optical pressure-sensitive adhesive sheet 20 having a high degree of cleanliness in the process of manufacturing an optical article, and therefore, for producing an optical article having a high degree of cleanliness at a light passing portion. Suitable.
  • the optical pressure-sensitive adhesive sheet X with a separator is used in the manufacturing process of a display panel, the optical pressure-sensitive adhesive sheet X with a separator is used as a supply material for the optical pressure-sensitive adhesive sheet 20 having a high degree of cleanliness. It helps to improve the quality of the displayed image.
  • the resolution of the camera device is 2.8 ⁇ m as described above, but may be, for example, 10 ⁇ m or less, preferably 5 ⁇ m or less.
  • the camera device may include a lens (that is, the light receiving element included in the camera device may have a configuration in which light is received through the lens).
  • the white LED light source and the LED light source of another color can be combined to carry out the evaluation method including the first to third steps and other evaluation methods (LED light source of another color). Examples include a red LED light source and a blue LED light source). For example, by using an LED light source of another color alone as a light source or by using an LED light source of two or more colors in combination as a light source, it becomes easy to carry out the above-mentioned foreign matter inspection depending on the inspection target.
  • the sample is set in the evaluation device by having the chuck mechanism provided in the evaluation device grip the outer region of the sample.
  • the light receiving surface of the camera device to be used is arranged to face the inner region of the sample, and the camera device performs scanning along the inner region.
  • the position information derived in the third step includes, for example, XY coordinate information having the projection plane as the XY plane and Z coordinate information having the thickness direction orthogonal to the XY plane as the Z direction. Is included.
  • the projection image information derived in the third step is information that can derive at least the total area of the foreign matter based on the information, and is, for example, information that can further derive the size of each foreign matter and the size distribution of the foreign matter.
  • the foreign matter area ratio R1 is preferably 18% or less, more preferably 15% or less, still more preferably 12% or less, and particularly preferably 10% or less. From the viewpoint of supplying the optical pressure-sensitive adhesive sheet 20 having a high degree of cleanliness in the manufacturing process of the optical article, the foreign matter area ratio R1 is preferably close to 0%.
  • the optical adhesive sheet X with a separator has a maximum length (maximum foreign matter length L1) of the maximum foreign matter in the plan view projection, preferably 30 ⁇ m or less, more preferably 20 ⁇ m or less, still more preferably 15 ⁇ m or less, and particularly preferably. It is 8 ⁇ m or less.
  • maximum length L1 of the maximum foreign matter in the plan view projection preferably 30 ⁇ m or less, more preferably 20 ⁇ m or less, still more preferably 15 ⁇ m or less, and particularly preferably. It is 8 ⁇ m or less.
  • the optical pressure-sensitive adhesive sheet X with a separator preferably has the maximum length (maximum foreign matter length L2) of the maximum foreign matter between the separator 10 and the optical pressure-sensitive adhesive sheet 20 (adhesive layer 21) in the plan view projection. Is 30 ⁇ m or less, more preferably 20 ⁇ m or less, still more preferably 15 ⁇ m or less, and particularly preferably 8 ⁇ m or less. Such a configuration is suitable for supplying an optical pressure-sensitive adhesive sheet 20 having a high degree of cleanliness in the manufacturing process of an optical article.
  • the ratio of the total projected area of bubbles on the projection surface of the plan view projection is preferably 10% or less, more preferably 8% or less, still more preferably 6%.
  • it is particularly preferably 4% or less, further preferably 2% or less, particularly preferably 1% or less, and extremely preferably 0%.
  • Such a configuration is suitable for supplying an optical pressure-sensitive adhesive sheet 20 having a high degree of cleanliness in the manufacturing process of an optical article.
  • Examples of the bubbles in the optical pressure-sensitive adhesive sheet X with a separator include bubbles existing at the interface between the separator 10 and the pressure-sensitive adhesive layer 21 and bubbles existing inside the pressure-sensitive adhesive layer 21.
  • Methods for controlling foreign matter inside and on the surface of the optical adhesive sheet 20 include, for example, manufacturing in a clean room, prevention of foreign matter from adhering to the surface with a protective film, purification of raw materials, adjustment of raw material composition, and filtering of raw materials. ..
  • the ratio of the total projected area of foreign matter on the projection surface of the plan view projection is preferably 20% or less, more preferably 18% or less, still more preferably 15% or less, and particularly further. It is preferably 12% or less, and particularly preferably 10% or less. From the viewpoint of supplying the optical pressure-sensitive adhesive sheet 20 having a high degree of cleanliness in the manufacturing process of the optical article, the foreign matter area ratio R3 is preferably close to 0%.
  • the separator 10 has a maximum length (maximum foreign matter length L3) of the maximum foreign matter in the plan view projection, preferably 30 ⁇ m or less, more preferably 20 ⁇ m or less, still more preferably 15 ⁇ m or less, and particularly preferably 8 ⁇ m or less. ..
  • a maximum length is suitable for inspecting the optical adhesive sheet for the presence or absence of foreign matter having a maximum length of slightly more than 30 ⁇ m in plan view projection (for example, foreign matter having a maximum length of about 33 ⁇ m). From the viewpoint of carrying out the above-mentioned precise foreign matter inspection, the shorter the maximum foreign matter length L3 is, the more preferable.
  • the separator 10 has a number of foreign substances having a maximum length of 20 ⁇ m or more and 30 ⁇ m or less (number of foreign substances in the first range N1) in the plan view projection, preferably 5 or less, more preferably 4 or less, still more preferably 3 or less. It is particularly preferably 2 or less, particularly preferably 1 or less, and extremely preferably 0.
  • Such a configuration is suitable for performing a precise foreign matter inspection on the optical pressure-sensitive adhesive sheet 20, and is therefore suitable for supplying an optical pressure-sensitive adhesive sheet 20 having a high degree of cleanliness in the manufacturing process of an optical article.
  • the number of foreign substances having a maximum length of 15 ⁇ m or more and 30 ⁇ m or less in the plan view projection is preferably 10 or less, more preferably 7 or less, still more preferably 4 or less. It is particularly preferably 3 or less, further preferably 2 or less, particularly preferably 1 or less, and extremely preferably 0.
  • Such a configuration is suitable for performing a precise foreign matter inspection on the optical pressure-sensitive adhesive sheet 20, and is therefore suitable for supplying an optical pressure-sensitive adhesive sheet 20 having a high degree of cleanliness in the manufacturing process of an optical article.
  • the separator 10 (separator 10A, separator 10B) includes the base film 11 and the release layer 12 in the present embodiment.
  • the release layer 12 is arranged on one side of the base film 11.
  • the base film 11 is, for example, a flexible and transparent resin film.
  • the resin material of the base film 11 include polyolefin, polyester, acrylic, polyamide, polyimide, polyvinyl chloride, polyvinylidene chloride, cellulose, modified cellulose, polystyrene, and polycarbonate.
  • the polyolefin include polyethylene, polypropylene, cycloolefin polymer (COP), poly-1-butene, poly-4-methyl-1-pentene, ethylene / propylene copolymer, ethylene / 1-butene copolymer, and ethylene.
  • Examples include vinyl acetate copolymers, ethylene / ethyl acrylate copolymers, and ethylene / vinyl alcohol copolymers.
  • Examples of the polyester include polyethylene terephthalate, polyethylene naphthalate, and polybutylene terephthalate.
  • Examples of the polyamide include polyamide 6, polyamide 6, 6 and partially aromatic polyamide.
  • Examples of the modified cellulose include triacetyl cellulose (TAC). These resin materials may be used alone or in combination of two or more.
  • the resin material preferably contains no filler or substantially no filler.
  • the filler is preferably a nanofiller (the nanofiller means particles having a maximum length of 100 nm or less). These configurations are preferable from the viewpoint of obtaining a separator 10 having a high degree of cleanliness.
  • the thickness of the base film 11 is preferably 5 ⁇ m or more, more preferably 10 ⁇ m or more, and more preferably 20 ⁇ m or more from the viewpoint of ensuring the strength of the separator 10. Further, from the viewpoint of ensuring appropriate flexibility in the separator 10, the thickness of the base film 11 is preferably 200 ⁇ m or less, more preferably 150 ⁇ m or less, still more preferably 100 ⁇ m or less.
  • the release layer 12 is a layer for ensuring the peelability of the optical adhesive sheet from the separator surface.
  • the material of the release layer 12 include a silicone resin, a long-chain alkyl resin, and a fatty acid amide resin. These resins may contain fluorine atoms in the polymer side chains.
  • the silicone resin may be a fluorinated silicone resin containing a fluorine atom in the side chain.
  • the separator 10 can be manufactured, for example, as follows. First, the molten resin material is molded into a film to produce a base film 11. Molding methods include, for example, extrusion molding, inflation molding, and calendar molding. Next, one side of the base film 11 is treated with a release agent to form a release layer 12 (a film of a release agent).
  • the release agent contains, for example, any one of the above-mentioned resins as the material of the release layer 12.
  • the separator 10 is preferably manufactured in a clean room. The higher the air cleanliness in the production line of the separator 10 (for example, the air cleanliness in the clean room), the smaller the amount of environmental foreign matter inside and the surface of the separator 10 to be manufactured, and the smaller the size of the environmental foreign matter.
  • the air cleanliness of the production line is preferably class 3 or less, more preferably class 2 or less, still more preferably class 1 in the ISO 146444-1 standard.
  • the separator 10 has transparency in this embodiment.
  • the haze of the separator 10 is preferably 3% or less, more preferably 2% or less, still more preferably 1% or less.
  • the haze of the separator 10 can be measured using a haze meter in accordance with JIS K7136 (2000).
  • the transmittance of the light emitted from the white LED light source in the separator 10 is, for example, 50% or more, preferably 80% or more, and more preferably 90% or more. Such a configuration is preferable from the viewpoint of appropriately performing a foreign matter inspection using a white LED light source.
  • the infrared transmittance of the separator 10 is, for example, 50% or more, preferably 80% or more, and more preferably 90% or more. Such a configuration is preferable from the viewpoint of appropriately performing a foreign matter inspection using infrared rays.
  • the separator 10 preferably has a surface having a surface roughness Ra of 20 nm or less.
  • the surface roughness Ra of the exposed surface of the release layer 12 is preferably 20 nm or less.
  • the surface roughness Ra is more preferably 17 nm or less, further preferably 15 nm or less, particularly preferably 12 nm or less, still more preferably 10 nm or less, still more preferably 8 nm or less, particularly preferably 6 nm or less, and extremely preferably 5 nm or less. Is.
  • Such a configuration regarding surface roughness is preferable from the viewpoint of suppressing foreign matter from entering the surface of the separator, and is useful for manufacturing an optical adhesive sheet that requires a high degree of cleanliness by using the separator 10.
  • the surface roughness Ra is, for example, 0.1 nm or more.
  • the surface roughness Ra is the arithmetic mean roughness of the surface and can be measured by the method described later with respect to the examples.
  • the separator 10 preferably has a surface having a surface roughness Rz of 600 nm or less.
  • the surface roughness Rz of the exposed surface of the release layer 12 is preferably 600 nm or less.
  • the surface roughness Rz is more preferably 400 nm or less, further preferably 300 nm or less, particularly preferably 200 nm or less, still more preferably 100 nm or less, still more preferably 80 nm or less, particularly preferably 60 nm or less, and extremely preferably 50 nm or less. Is.
  • Such a configuration regarding surface roughness is preferable from the viewpoint of suppressing foreign matter from adhering to the surface of the separator, and is useful for manufacturing an optical pressure-sensitive adhesive sheet that requires a high degree of cleanliness by using the separator 10.
  • the surface roughness Rz is, for example, 1 nm or more.
  • the surface roughness Rz is a ten-point average roughness of the surface, and can be measured by the method described later with respect to Examples.
  • first peeling adhesive force is larger than the second peeling adhesive force
  • the separator 10B is first peeled off from the optical adhesive sheet X with a separator. Ru.
  • the surface of the pressure-sensitive adhesive layer 21 exposed by the peeling is attached to the adherend.
  • the separator 10A is peeled off from the optical pressure-sensitive adhesive sheet X with a separator on the adherend.
  • the peeling adhesive force between the release layer 12 and the pressure-sensitive adhesive layer 21 can be adjusted, for example, by selecting the type of material of the release layer 12 and adjusting the concentration of the material.
  • the optical adhesive sheet 20 is an optical adhesive sheet having a transparent adhesive layer 21.
  • the pressure-sensitive adhesive layer 21 is a pressure-sensitive adhesive layer formed from the pressure-sensitive adhesive composition and has transparency (visible light transmission).
  • the tacky composition contains a base polymer.
  • the base polymer is an adhesive component for developing adhesiveness in the adhesive layer 21.
  • the base polymer exhibits rubber elasticity at room temperature.
  • examples of the base polymer include acrylic polymers, rubber polymers, polyester polymers, urethane polymers, polyether polymers, silicone polymers, polyamide polymers, and fluoropolymers.
  • an acrylic base polymer is preferably used from the viewpoint of ensuring good transparency and tackiness in the pressure-sensitive adhesive layer 21.
  • the acrylic base polymer contains (meth) acrylic acid alkyl ester as the main constituent monomer component.
  • (meth) acrylic is meant acrylic and / or methacrylic.
  • a (meth) acrylic acid alkyl ester having an alkyl group having 1 to 20 carbon atoms that is, a (meth) acrylic acid C 1-20 alkyl ester is preferably used.
  • the (meth) acrylic acid alkyl ester may have a linear or branched alkyl group, or may have a cyclic alkyl group such as an alicyclic alkyl group.
  • Examples of the (meth) acrylic acid alkyl ester having a linear or branched alkyl group include methyl (meth) acrylate, ethyl (meth) acrylate, butyl (meth) acrylate, and isobutyl (meth) acrylate.
  • Examples of the (meth) acrylic acid alkyl ester having an alicyclic alkyl group include a (meth) acrylic acid cycloalkyl ester, a (meth) acrylic acid ester having a bicyclic aliphatic hydrocarbon ring, and a tricycle. Examples thereof include (meth) acrylic acid esters having the above aliphatic hydrocarbon rings. Examples of the (meth) acrylic acid cycloalkyl ester include (meth) acrylic acid cyclopentyl, (meth) acrylic acid cyclohexyl, (meth) acrylic acid cycloheptyl, and (meth) acrylic acid cyclooctyl.
  • Examples of the (meth) acrylic acid ester having a bicyclic aliphatic hydrocarbon ring include isobornyl (meth) acrylic acid.
  • Examples of the (meth) acrylic acid ester having three or more aliphatic hydrocarbon rings include dicyclopentanyl (meth) acrylate, dicyclopentanyloxyethyl (meth) acrylate, and tricyclopentanyl (meth) acrylate. , 1-adamantyl (meth) acrylate, 2-methyl-2-adamantyl (meth) acrylate, and 2-ethyl-2-adamantyl (meth) acrylate.
  • the amount of (meth) acrylic acid alkyl ester with respect to a total of 100 parts by mass of the monomer components forming the acrylic base polymer is preferably 60 parts by mass or more, more preferably 70 parts by mass or more, and further preferably 75 parts by mass or more.
  • the amount of the (meth) acrylic acid alkyl ester with respect to 100 parts by mass of the total of the monomer components forming the acrylic base polymer is preferably 100 parts by mass or less, more preferably 95 parts by mass or less, and further preferably 92 parts by mass or less.
  • the acrylic base polymer preferably contains a polar group-containing monomer in addition to the above-mentioned (meth) acrylic acid alkyl ester as a monomer component.
  • the polar group-containing monomer include a hydroxy group-containing monomer, a carboxy group-containing monomer, and a nitrogen-containing monomer.
  • the monomer component contains a polar group-containing monomer, the cohesive force of the polymer is enhanced, and the adhesive retention at high temperature tends to be improved.
  • a crosslinked structure is introduced into an acrylic base polymer by a crosslinking agent such as an isocyanate crosslinking agent or an epoxy crosslinking agent, the hydroxy group or the carboxy group becomes the introduction point of the crosslinked structure.
  • the hydroxy group-containing monomer examples include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, and 6-hydroxyhexyl (meth) acrylate.
  • Examples include 8-hydroxyoctyl acrylate, 10-hydroxydecyl (meth) acrylate, and 12-hydroxylauryl (meth) acrylate.
  • the hydroxy group-containing monomers include 2-hydroxyethyl acrylate and acrylic acid 4. -Hydroxybutyl is preferred.
  • carboxy group-containing monomer examples include (meth) acrylic acid, (meth) carboxyethyl acrylate, (meth) carboxypentyl acrylate, itaconic acid, maleic acid, fumaric acid, and crotonic acid.
  • Examples of the nitrogen-containing monomer include a nitrogen-containing vinyl-based monomer and a cyanoacrylate monomer.
  • Examples of the nitrogen-containing vinyl-based monomer include N-vinylpyrrolidone, methylvinylpyrrolidone, vinylpyridine, vinylpiperidone, vinylpyrimidine, vinylpiperazine, vinylpyrazine, vinylpyrrole, vinylimidazole, vinyloxazole, vinylmorpholine, and (meth) acryloylmorpholine. , N-vinylcarboxylic acid amides, and N-vinylcaprolactam.
  • Examples of the cyanoacrylate-based monomer include acrylonitrile and methacrylonitrile. From the viewpoint of ensuring a cohesive force in the pressure-sensitive adhesive layer 21 and realizing a good adhesive force, N-vinylpyrrolidone is preferably used as the nitrogen-containing monomer.
  • the amount of the polar group-containing monomer is preferably 5 parts by mass or more, more preferably 5 parts by mass or more, based on 100 parts by mass of the total monomer components of the acrylic base polymer. It is 8 parts by mass or more, more preferably 10 parts by mass or more.
  • the amount of the polar group-containing monomer with respect to 100 parts by mass of the total monomer components of the acrylic base polymer is preferably 25 parts by mass or less, more preferably 20 parts by mass or less, still more preferably 17 parts by mass or less, and particularly preferably 15 parts by mass. It is less than a part.
  • the monomer component forming the acrylic base polymer preferably contains a hydroxy group-containing monomer as a polar group-containing monomer component. Such a configuration is suitable for ensuring good adhesive strength in the pressure-sensitive adhesive layer 21, and is also suitable for suppressing white turbidity of the pressure-sensitive adhesive layer 21 in a high humidity environment. Further, the monomer component forming the acrylic base polymer preferably contains a nitrogen-containing monomer as a polar group-containing monomer component. Such a configuration is suitable for ensuring good adhesive strength in the pressure-sensitive adhesive layer 21.
  • the amount of the hydroxy group-containing monomer with respect to 100 parts by mass of the total monomer components is preferably 2 parts by mass or more, more preferably 3 parts by mass or more, and further preferably 4 parts by mass or more.
  • the amount of the hydroxy group-containing monomer with respect to 100 parts by mass of the total monomer components is preferably 15 parts by mass or less, more preferably 12 parts by mass or less, and further preferably 10 parts by mass or less.
  • the total amount of 2-hydroxyethyl acrylate and 4-hydroxybutyl acrylate is preferably in such a range, and the amount of 4-hydroxybutyl acrylate is more preferably in such a range.
  • the amount of the nitrogen group-containing monomer with respect to 100 parts by mass of the total monomer components of the acrylic base polymer is preferably 2 parts by mass or more, more preferably 3 parts by mass or more, and further preferably 4 parts by mass or more.
  • the amount of the nitrogen group-containing monomer with respect to 100 parts by mass of the total monomer components of the acrylic base polymer is preferably 20 parts by mass or less, more preferably 15 parts by mass or less, still more preferably 12 parts by mass or less.
  • the amount of N-vinylpyrrolidone is preferably in such a range.
  • the optical adhesive sheet 20 When the optical adhesive sheet 20 is used for adhering a touch panel sensor, it is preferable that the optical adhesive sheet 20 has a small acid content in order to prevent corrosion of the electrodes due to an acid component. Further, when the optical pressure-sensitive adhesive sheet 20 is used for adhering a polarizing plate, it is preferable that the optical pressure-sensitive adhesive sheet 20 has a small acid content in order to suppress polyene formation of a polyvinyl alcohol-based polarizing element by an acid component.
  • the content of the organic acid monomer such as (meth) acrylic acid in such an acid-free optical pressure-sensitive adhesive sheet 20 is preferably 100 ppm or less, more preferably 70 ppm or less, still more preferably 50 ppm or less.
  • the organic acid monomer content of the optical pressure-sensitive adhesive sheet 20 is determined by immersing the optical pressure-sensitive adhesive sheet 20 in pure water and heating it at 100 ° C. for 45 minutes, thereby quantifying the acid monomer extracted into water by an ion chromatograph. Demanded by.
  • the amount of the organic acid monomer component such as (meth) acrylic acid in the monomer component constituting the base polymer is small. Therefore, in order to make the optical pressure-sensitive adhesive sheet 20 acid-free, it is preferable that the base polymer does not substantially contain an organic acid monomer (carboxy group-containing monomer) as a monomer component.
  • the amount of the carboxy group-containing monomer with respect to 100 parts by mass of the total monomer components of the base polymer is preferably 0.5 parts by mass or less, more preferably 0.1 parts by mass or less, still more preferably 0. It is 05 parts by mass or less, ideally 0.
  • the acrylic base polymer may contain a monomer other than the above-mentioned (meth) acrylic acid alkyl ester and a polar group-containing monomer as a monomer component.
  • examples of other monomer components include vinyl-based monomers other than the above, cyanoacrylate-based monomers other than the above, glycol-based acrylic ester monomers, and acrylic acid ester-based monomers other than the above.
  • vinyl-based monomers other than the above include caprolactone adducts of (meth) acrylic acid, sulfonic acid group-containing monomers, phosphoric acid group-containing monomers, vinyl acetate, vinyl propionate, styrene, and ⁇ -methylstyrene.
  • Examples of the cyanoacrylate-based monomer other than the above include acrylonitrile and methacrylonitrile.
  • Examples of the epoxy group-containing monomer include glycidyl (meth) acrylate.
  • Examples of the glycol-based acrylic ester monomer include polyethylene glycol (meth) acrylate, polypropylene glycol (meth) acrylate, methoxyethylene glycol (meth) acrylate, and methoxypolypropylene glycol (meth) acrylate.
  • Examples of the acrylic acid ester-based monomer other than the above include tetrahydrofurfuryl (meth) acrylic acid, fluorine (meth) acrylate, and silicone (meth) acrylate.
  • the glass transition temperature (Tg) of the polymer the glass transition temperature (theoretical value) obtained based on the Fox formula below can be used.
  • the Fox formula is a relational expression between the glass transition temperature Tg of the polymer and the glass transition temperature Tgi of the homopolymer of the monomer constituting the polymer.
  • Tg represents the glass transition temperature (° C.) of the polymer
  • Wi represents the weight fraction of the monomer i constituting the polymer
  • Tgi represents the glass transition of the homopolymer formed from the monomer i. Indicates the temperature (° C).
  • Literature values can be used for the glass transition temperature of homopolymers, for example, "Polymer Handbook” (4th edition, John Wiley & Sons, Inc., 1999) and "New Polymer Bunko 7 Introduction to Synthetic Resins for Paints”. (Kyozo Kitaoka, Polymer Publications, 1995) lists the glass transition temperatures of various homopolymers.
  • Tg the peak top temperature of the loss tangent (tan ⁇ ) obtained by the dynamic viscoelasticity measurement may be adopted.
  • a specific method for measuring the peak top temperature is described in, for example, Japanese Patent Application Laid-Open No. 2007-51271.
  • the gel fraction can be determined as an insoluble fraction in a solvent such as ethyl acetate. Specifically, the gel fraction is determined as the weight fraction (unit: mass%) of the insoluble component after immersing the pressure-sensitive adhesive layer as a sample in ethyl acetate at 23 ° C. for 7 days with respect to the sample before immersion. Be done. In general, the higher the degree of cross-linking of a polymer, the higher the gel fraction of the polymer tends to be.
  • the gel fraction (introduction amount of the crosslinked structure) can be adjusted, for example, by selecting the method for introducing the crosslinked structure, selecting the type of the crosslinking agent, and the amount of the crosslinking agent used.
  • a method for introducing a cross-linked structure into the base polymer for example, a method of polymerizing a base polymer having a functional group capable of reacting with the cross-linking agent and then adding a cross-linking agent to react the base polymer with the cross-linking agent (No. 1). 1) and a method (second method) of introducing a branched structure (crosslinked structure) into the polymer chain by including a polyfunctional compound in the polymer component of the base polymer. These may be used in combination to introduce a plurality of crosslinked structures into the base polymer.
  • a cross-linking structure is introduced into the base polymer by adding a cross-linking agent to the polymerized base polymer and heating as necessary.
  • the cross-linking agent include compounds that react with functional groups (for example, hydroxy groups and carboxy groups) contained in the base polymer.
  • the cross-linking agent include an isocyanate cross-linking agent, an epoxy cross-linking agent, an oxazoline cross-linking agent, an aziridine cross-linking agent, a carbodiimide cross-linking agent, and a metal chelate cross-linking agent.
  • an isocyanate cross-linking agent and an epoxy cross-linking agent are used because they have high reactivity with the functional groups (for example, hydroxy group and carboxy group) of the base polymer and the cross-linking structure can be easily introduced.
  • These cross-linking agents react with functional groups (eg, hydroxy and carboxy groups) introduced into the base polymer to form a cross-linked structure.
  • an isocyanate cross-linking agent to form a cross-linked structure by reacting the hydroxy group in the base polymer with the isocyanate cross-linking agent.
  • isocyanate cross-linking agent for example, polyisocyanate having two or more isocyanate groups in one molecule is used.
  • isocyanate cross-linking agent examples include lower aliphatic polyisocyanates, alicyclic isocyanates, aromatic isocyanates, and isocyanate adducts.
  • the lower aliphatic polyisocyanates include butylene diisocyanate and hexamethylene diisocyanate.
  • alicyclic isocyanates include cyclopentylene diisocyanate, cyclohexylene diisocyanate, and isophorone diisocyanate.
  • aromatic isocyanates examples include 2,4-tolylene diisocyanate, 4,4'-diphenylmethane diisocyanate, and xylylene diisocyanate.
  • isocyanate additive examples include a trimethylol propane / tolylene diisocyanate trimer adduct (for example, “Coronate L” manufactured by Tosoh) and a trimethylol propane / hexamethylene diisocyanate trimer adduct (for example, “Coronate L” manufactured by Tosoh).
  • Coronate HL trimethylol propane adduct of xylylene diisocyanate (eg,“ Takenate D110N ”manufactured by Mitsui Chemicals, Inc.), and isocyanurates of hexamethylene diisocyanate (eg,“ Coronate HX ”manufactured by Toso).
  • the monomer component constituting the acrylic base polymer and the total amount of the polyfunctional compound for introducing the crosslinked structure may be reacted (polymerized) at one time or polymerized in multiple steps. good.
  • the multi-step polymerization method for example, first, the monofunctional monomers constituting the base polymer are polymerized (prepolymerized) to prepare a partial polymer (prepolymer composition). Next, a polyfunctional compound such as a polyfunctional (meth) acrylate is added to the prepolymer composition to polymerize (mainly polymerize) the prepolymer composition and the polyfunctional monomer.
  • the prepolymer composition is a partial polymer containing a polymer having a low degree of polymerization and an unreacted monomer.
  • branch points (crosslinking points) due to the polyfunctional compound can be uniformly introduced into the base polymer.
  • a mixture (adhesive composition) of a low molecular weight polymer or a partial polymer and an unpolymerized monomer component is applied onto a substrate and then main-polymerized on the substrate to form an optical pressure-sensitive adhesive sheet 20.
  • Low-polymerization compositions such as prepolymer compositions have low viscosity and excellent coatability
  • the method of main polymerization on a substrate after coating a tacky composition which is a mixture of a prepolymer composition and a polyfunctional compound is used. It is preferable from the viewpoint of productivity of the optical pressure-sensitive adhesive sheet 20 and from the viewpoint of uniform thickness.
  • polyfunctional compound used for introducing the crosslinked structure examples include compounds containing two or more polymerizable functional groups (ethylenically unsaturated groups) having an unsaturated double bond in one molecule.
  • polyfunctional (meth) acrylate is preferable because it can be easily copolymerized with the monomer component of the acrylic base polymer.
  • a polyfunctional acrylate is preferable.
  • polyfunctional (meth) acrylate examples include polyethylene glycol di (meth) acrylate, polypropylene glycol di (meth) acrylate, polytetramethylene glycol di (meth) acrylate, bisphenol A ethylene oxide-modified di (meth) acrylate, and bisphenol A.
  • the molecular weight of a polyfunctional compound such as a polyfunctional (meth) acrylate is preferably 1500 from the viewpoint of appropriately adjusting viscoelasticity (for example, storage elastic modulus G'and loss tangent tan ⁇ ) by introducing a crosslinked structure in an acrylic base polymer. Below, it is more preferably 1000 or less.
  • the functional group equivalent (g / eq) of the polyfunctional compound is preferably 50 or more, more preferably 70 or more, still more preferably 80.
  • the functional group equivalent is preferably 500, more preferably 300 or less, still more preferably 200.
  • Examples of the polymerization method of the acrylic base polymer include solution polymerization, active energy ray polymerization method, bulk polymerization, and emulsion polymerization.
  • a solution polymerization method and an active energy ray polymerization method are preferable in terms of the transparency, water resistance, and cost of the pressure-sensitive adhesive.
  • Examples of the solvent for solution polymerization include ethyl acetate and toluene.
  • a polymerization initiator When preparing the acrylic base polymer, a polymerization initiator may be used depending on the type of polymerization reaction.
  • the polymerization initiator include a photopolymerization initiator and a thermal polymerization initiator.
  • the photopolymerization initiator include a benzoin ether-based photopolymerization initiator, an acetophenone-based photopolymerization initiator, an ⁇ -ketol-based photopolymerization initiator, an aromatic sulfonyl chloride-based photopolymerization initiator, and a photoactive oxime-based photopolymerization initiator.
  • benzoin-based photopolymerization initiators benzoin-based photopolymerization initiators, benzyl-based photopolymerization initiators, benzophenone-based photopolymerization initiators, ketal-based photopolymerization initiators, thioxanthone-based photopolymerization initiators, and acylphosphine oxide-based photopolymerization initiators.
  • the thermal polymerization initiator include an azo-based initiator, a peroxide-based initiator, and a redox-based initiator in which a peroxide and a reducing agent are combined (for example, a combination of a persulfate and sodium bisulfite). And a combination of peroxide and sodium ascorbate).
  • a chain transfer agent and a polymerization inhibitor may be used.
  • the chain transfer agent include thiols such as ⁇ -thioglycerol, lauryl mercaptan, glycidyl mercaptan, mercaptoacetic acid, 2-mercaptoethanol, thioglycolic acid, 2-ethylhexyl thioglycolate, and 2,3-dimercapto-1-propanol. , And ⁇ -methylstyrene dimer.
  • the molecular weight of the base polymer can be adjusted by adjusting the type and amount of the polymerization initiator.
  • the amount of the polymerization initiator the higher the radical concentration of the reaction system, so that the density of the reaction starting point tends to be high and the polymer molecular weight tends to be small.
  • the amount of the polymerization initiator is smaller, the density of the reaction initiation point is smaller, so that the polymer chain tends to be easily extended and the polymer molecular weight tends to be large.
  • the acrylic base polymer has a high gel fraction with a small crosslink point density.
  • the molecular weight (length of the polymer chain) of the base polymer may be increased.
  • the amount of the polymerization initiator used during the polymerization of the base polymer is appropriately set according to, for example, the type of the polymerization reaction, the composition of the monomer, the type of the polymerization initiator, and the target molecular weight.
  • the amount of the polymerization initiator used is preferably 0.001 with respect to a total of 100 parts by mass of the monomer components constituting the base polymer. By mass or more, more preferably 0.003 parts by mass or more, still more preferably 0.005 parts by mass or more.
  • the amount used is preferably 0.4 parts by mass or less, more preferably 0.1 parts by mass or less, and further preferably 0.05 parts by mass or less.
  • a crosslinked structure with an isocyanate cross-linking agent After polymerizing the base polymer by solution polymerization, the cross-linking agent is added to the polymerization solution, and the solution is heated as necessary to introduce the cross-linked structure into the base polymer.
  • a crosslinked structure is introduced by a polyfunctional compound such as a polyfunctional (meth) acrylate
  • the base polymer is polymerized or a prepolymer composition is prepared by solution polymerization or active energy ray polymerization, and the polyfunctional compound is added to the polymerization solution. It is preferable to add and introduce a crosslinked structure by a polyfunctional compound by further active energy ray polymerization.
  • the prepolymer composition can be prepared, for example, by partially polymerizing (prepolymerizing) a composition (composition for forming a prepolymer) in which a monomer component constituting an acrylic base polymer and a polymerization initiator are mixed.
  • the monomer component in the composition for forming a prepolymer is preferably a monofunctional monomer component among the monomer components constituting the acrylic base polymer.
  • the monofunctional monomer component is, for example, the above-mentioned (meth) acrylic acid alkyl ester and a polar group-containing monomer.
  • the composition for forming a prepolymer may contain a polyfunctional monomer in addition to the monofunctional monomer. For example, a part of the polyfunctional monomer may be contained in the composition for forming a prepolymer, and the remainder of the polyfunctional monomer component may be added after the prepolymerization to carry out the main polymerization.
  • the polymerization rate of the prepolymer is not particularly limited, but is preferably 3% by mass or more, more preferably 5% by mass or more, and preferably 50% by mass from the viewpoint of obtaining a viscosity suitable for coating on a substrate. As mentioned above, it is more preferably 40% by mass or less.
  • the polymerization rate of the prepolymer can be adjusted by selecting the type of photopolymerization initiator and adjusting the amount used, and adjusting the irradiation intensity and irradiation time of active energy rays such as UV light.
  • the adhesive sheet may contain an oligomer in addition to the acrylic base polymer.
  • the weight average molecular weight of the acrylic oligomer is, for example, 1000 or more, and for example, 30,000 or less.
  • the acrylic oligomer contains a (meth) acrylic acid alkyl ester as a main constituent monomer component.
  • the glass transition temperature of the acrylic oligomer is preferably 60 ° C. or higher, more preferably 80 ° C. or higher, still more preferably 100 ° C. or higher, and particularly preferably 110 ° C. or higher.
  • the combined use of the low Tg acrylic base polymer introduced with the crosslinked structure and the high Tg acrylic oligomer tends to improve the adhesive strength in the pressure-sensitive adhesive layer 21, and particularly tends to improve the adhesive holding power at high temperatures. be.
  • the glass transition temperature of the acrylic oligomer is preferably 200 ° C. or lower, more preferably 180 ° C. or lower, still more preferably 160 ° C. or lower.
  • the glass transition temperature of the acrylic oligomer is calculated by the above Fox formula.
  • the acrylic oligomer having a glass transition temperature of 60 ° C. or higher preferably has a (meth) acrylic acid alkyl ester having a linear or branched alkyl group and / or an alicyclic alkyl group as a constituent monomer component. Contains (meth) acrylic acid alkyl esters. Specific examples of these are as described above as constituent monomers of the acrylic base polymer.
  • the (meth) acrylic acid alkyl ester having a linear or branched alkyl group methyl methacrylate is preferable because it has a high glass transition temperature and is excellent in compatibility with a base polymer.
  • the (meth) acrylic acid alkyl ester having an alicyclic alkyl group include dicyclopentanyl acrylate, dicyclopentanyl methacrylate, cyclohexyl acrylate, and cyclohexyl methacrylate.
  • the acrylic oligomer contains, as constituent monomer components, one or more selected from the group consisting of dicyclopentanyl acrylate, dicyclopentanyl methacrylate, cyclohexyl acrylate, and cyclohexyl methacrylate, and methyl methacrylate.
  • dicyclopentanyl acrylate dicyclopentanyl methacrylate
  • cyclohexyl acrylate cyclohexyl methacrylate
  • methyl methacrylate include.
  • the amount of the (meth) acrylic acid alkyl ester having a linear or branched alkyl group with respect to the total amount of the monomer components constituting the acrylic oligomer is preferably 10% by mass or more, more preferably 20% by mass or more, still more preferably. It is 30% by mass or more, preferably 90% by mass or less, more preferably 80% by mass or less, and further preferably 70% by mass or less.
  • the amount of the (meth) acrylic acid alkyl ester having an alicyclic alkyl group with respect to the total amount of the monomer components constituting the acrylic oligomer is preferably 10% by mass or more, more preferably 20% by mass or more, still more preferably 30% by mass. % Or more, preferably 90% by mass or less, more preferably 80% by mass or less, still more preferably 70% by mass or less.
  • the weight average molecular weight of the acrylic oligomer is preferably 1000 or more, more preferably 1500 or more, and further preferably 2000.
  • the weight average molecular weight is preferably 30,000 or less, more preferably 10,000 or less, still more preferably 8,000 or less.
  • Acrylic oligomers having a molecular weight in such a range are suitable for achieving good adhesive strength and adhesive retention in the pressure-sensitive adhesive layer 21.
  • the acrylic oligomer is obtained by polymerizing the above-mentioned monomer components by various polymerization methods.
  • Various polymerization initiators may be used in the polymerization of the acrylic oligomer.
  • a chain transfer agent may be used in the polymerization reaction from the viewpoint of adjusting the molecular weight.
  • the amount of the acrylic oligomer in the pressure-sensitive adhesive layer 21 with respect to 100 parts by mass of the base polymer is preferably 0.5 parts by mass or more, more preferably 0.8 parts by mass or more. More preferably, it is 1 part by mass or more.
  • the amount of the acrylic oligomer in the pressure-sensitive adhesive layer 21 is 1.3 parts by mass or more and 1.5 parts by mass or more and 1.8 parts by mass or more and 2 parts by mass or more and 2.3 parts by mass with respect to 100 parts by mass of the base polymer. It may be 2 parts or more, or 2.5 parts by mass or more.
  • the amount of the acrylic oligomer added to the pressure-sensitive adhesive layer 21 is excessively large, the haze of the pressure-sensitive adhesive layer 21 tends to increase due to the decrease in compatibility, and the transparency tends to decrease.
  • the optical adhesive sheet arranged on the visual side of the image display panel is required to have high transparency, the amount of the acrylic oligomer in the optical adhesive sheet 20 (adhesive layer 21) is based on 100 parts by mass of the base polymer. It is preferably 10 parts by mass or less, more preferably 7 parts by mass or less, still more preferably 6 parts by mass or less, and particularly preferably 5 parts by mass or less.
  • the acrylic base polymer (or prepolymer composition) is mixed with the acrylic oligomer, a cross-linking agent and / or a polyfunctional compound for introducing a cross-linking structure, and other additives to be blended as needed.
  • a thickening additive or the like may be used for the purpose of adjusting the viscosity.
  • the tacky composition contains a prepolymer composition and a polyfunctional compound
  • a photopolymerization initiator and a chain transfer agent for the main polymerization it is preferable to add a photopolymerization initiator and a chain transfer agent for the main polymerization to the tacky composition.
  • a polymerization initiator for the main polymerization may be added to the prepolymer composition. If the polymerization initiator during the prepolymerization remains in the prepolymer composition without being deactivated, the addition of the polymerization initiator for the main polymerization may be omitted.
  • the tacky composition may contain a chain transfer agent.
  • the content of the acrylic base polymer (or prepolymer composition) in the adhesive composition is preferably 50% by mass or more, more preferably 70% by mass, and 80% by mass or more with respect to the total amount of the non-volatile content. It is more preferable, and it is particularly preferable that it is 90% by mass or more.
  • the amount of the cross-linking agent and / or the polyfunctional compound in the adhesive composition is adjusted so that the gel fraction is within the above range.
  • the amount of the cross-linking agent is preferably 0.005 part by mass or more, more preferably 0.01 part by mass or more, still more preferably, with respect to 100 parts by mass of the acrylic base polymer. Is 0.02 parts by mass.
  • the amount of the cross-linking agent is preferably 0.5 parts by mass or less, more preferably 0.3 parts by mass or less, and further preferably 0.1 parts by mass or less.
  • the amount of the polyfunctional (meth) acrylate is preferably 0.005 part by mass or more, more preferably 0.005 part by mass with respect to 100 parts by mass of the acrylic base polymer (prepolymer). It is 0.01 part by mass or more, more preferably 0.02 part by mass or more.
  • the amount of the polyfunctional (meth) acrylate is preferably 0.3 parts by mass or less, more preferably 0.2 parts by mass or less, and further preferably 0.1 part by mass or less.
  • a silane coupling agent may be added to the pressure-sensitive adhesive composition.
  • the amount of the silane coupling agent added is preferably 0.01 part by mass or more, more preferably 0.03 part by mass with respect to 100 parts by mass of the base polymer. It is more than parts, preferably 5.0 parts by mass or less, and more preferably 2.0 parts by mass or less.
  • the adhesive composition may contain components other than the above.
  • Other components include, for example, tackifiers, plasticizers, softeners, antioxidants, fillers, colorants, UV absorbers, antioxidants, surfactants, and antistatic agents.
  • the optical adhesive sheet 20 can be manufactured, for example, by applying the above-mentioned adhesive composition on a separator 10 (separator 10A) to form a coating film, and then drying the coating film.
  • Examples of the method of applying the adhesive composition include roll coat, kiss roll coat, gravure coat, reverse coat, roll brush, spray coat, dip roll coat, bar coat, knife coat, air knife coat, curtain coat, and lip coat. , And die coat.
  • the drying temperature of the coating film is, for example, 50 ° C to 200 ° C.
  • the drying time is, for example, 5 seconds to 20 minutes.
  • the cross-linking reaction proceeds at the same time as the above-mentioned drying or by aging thereafter.
  • the aging conditions are appropriately set depending on the type of the cross-linking agent.
  • the aging temperature is, for example, 20 ° C to 160 ° C.
  • the aging time is, for example, 1 minute to 7 days.
  • separator 10 separator 10B
  • separator 10B laminates the separator 10 on the pressure-sensitive adhesive layer 21 on the separator 10A before or after aging.
  • the adhesive composition is a photopolymerizable composition containing a prepolymer composition, a polyfunctional compound, or the like
  • the adhesive composition is applied in layers on the separator 10 and then photocured by irradiating with active light. Is done.
  • a cover sheet may be attached to the surface of the coating layer, and the adhesive composition may be irradiated with active light while sandwiched between the two sheets to prevent polymerization inhibition due to oxygen. preferable.
  • the active light is selected according to the type of monomer component, polymerizable component (eg, polyfunctional (meth) acrylate), and type of photopolymerization initiator. Generally, ultraviolet light and / or short wavelength visible light is used.
  • the integrated light amount of the irradiation light is, for example, about 100 to 5000 mJ / cm 2 .
  • the light source for light irradiation a light source capable of irradiating light in a wavelength range in which the photopolymerization initiator contained in the adhesive composition has sensitivity is used. Examples of the light source include an LED light source, a high pressure mercury lamp, an ultrahigh pressure mercury lamp, a metal halide lamp, and a xenon lamp.
  • the optical adhesive sheet X with a separator can be manufactured.
  • the optical pressure-sensitive adhesive sheet X with a separator is preferably manufactured in a clean room.
  • the air cleanliness of the production line is preferably class 3 or less, more preferably class 2 or less, still more preferably class 1 in the ISO 146444-1 standard.
  • the thickness of the pressure-sensitive adhesive layer 21 is preferably 10 ⁇ m or more, more preferably 15 ⁇ m or more, from the viewpoint of ensuring sufficient adhesiveness to the adherend. From the viewpoint of handleability of the optical pressure-sensitive adhesive sheet 20, the thickness of the pressure-sensitive adhesive layer 21 is preferably 300 ⁇ m or less, more preferably 200 ⁇ m or less.
  • the haze of the pressure-sensitive adhesive layer 21 is preferably 3% or less, more preferably 2% or less.
  • the haze of the pressure-sensitive adhesive layer 21 can be measured using a haze meter in accordance with JIS K7136 (2000). Examples of the haze meter include "NDH2000" manufactured by Nippon Denshoku Kogyo Co., Ltd. and "HM-150 type” manufactured by Murakami Color Technology Research Institute.
  • the transmittance of the light emitted from the white LED light source in the pressure-sensitive adhesive layer 21 is, for example, 50% or more, preferably 80% or more, and more preferably 90% or more. Such a configuration is preferable from the viewpoint of appropriately performing a foreign matter inspection using a white LED light source.
  • the infrared transmittance of the pressure-sensitive adhesive layer 21 is, for example, 50% or more, preferably 80% or more, and more preferably 90% or more. Such a configuration is preferable from the viewpoint of appropriately performing a foreign matter inspection using infrared rays.
  • the present invention will be specifically described below with reference to examples, but the present invention is not limited to the examples.
  • the specific numerical values such as the compounding amount (content), the physical property value, the parameter, etc. described below are the compounding amounts corresponding to them described in the above-mentioned "form for carrying out the invention” (forms for carrying out the invention). It can be replaced with an upper limit (numerical value defined as “less than or equal to” or “less than”) or a lower limit (numerical value defined as "greater than or equal to” or “greater than or equal to”) such as content), physical property value, and parameter.
  • Example 1 by forming a silicone-based release layer on one side of a cycloolefin polymer (COP) film (trade name "Zeonoa film ZF16", thickness 50 ⁇ m, manufactured by Zeon Corporation) as a base film in a clean room. (Two separators were made in this way).
  • the air cleanliness in the clean room is class 3 in the ISO 14644-1 standard.
  • silicone-based release layer In the formation of the silicone-based release layer, first, 30 parts by mass of an additive-type silicone composition (trade name "LTC761", manufactured by Toray Dow Corning) and a silicone dispersion (trade name "BY 24-850", Toray Co., Ltd.) A mixture of 0.9 parts by mass of Dow Corning and 2 parts by mass of a platinum catalyst for curing silicone (trade name "SRX 212", manufactured by Toray Dow Corning) is mixed with a mixed solvent of toluene and hexane (toluene and hexane). The volume ratio was diluted by 1: 1) to prepare a release agent solution.
  • an additive-type silicone composition trade name "LTC761”
  • silicone dispersion trade name "BY 24-850”, Toray Co., Ltd.
  • a mixture of 0.9 parts by mass of Dow Corning and 2 parts by mass of a platinum catalyst for curing silicone (trade name "SRX 212”, manufactured by Toray Dow Corning) is mixed with a mixed solvent of to
  • the separator of Example 1 includes a COP film as a base film and a silicone release layer on one surface thereof.
  • an ultraviolet curable adhesive composition is applied to a release layer forming surface in one of the separators of Example 1 (the first separator as a support release film) to coat a coating film (thickness). 50 ⁇ m) was formed.
  • the other separator of Example 1 (the second separator as a cover release film) was laminated on the exposed surface of the coating film to obtain a laminated body.
  • the laminated body was irradiated with ultraviolet rays from the second separator side to photo-cure the adhesive composition coating film to form an adhesive layer.
  • the optical pressure-sensitive adhesive sheet with a separator of Example 1 As the light source for ultraviolet irradiation, a black light whose position was adjusted so that the irradiation intensity on the irradiation surface directly under the lamp was 5 mW / cm 2 was used. As described above, the optical pressure-sensitive adhesive sheet with a separator of Example 1 was produced.
  • the optical pressure-sensitive adhesive sheet with a separator has a photocurable pressure-sensitive adhesive layer and separators arranged on both sides.
  • Example 2 With the separator of Example 1 except that a filler-less polyethylene terephthalate (PET) film (trade name "38-U41", thickness 38 ⁇ m, manufactured by Toray Industries, Inc.) was used as the base film of the separator instead of the COP film.
  • PET polyethylene terephthalate
  • the optical pressure-sensitive adhesive sheet with a separator of Example 2 was produced in the same manner as the optical pressure-sensitive adhesive sheet.
  • Comparative Example 1 Examples except that a biaxially stretched polyester film (trade name "Lumirror XD500P", thickness 75 ⁇ m, filler-containing PET film, manufactured by Toray Advanced Materials Korea) was used as the base film of the separator instead of the COP film.
  • the optical pressure-sensitive adhesive sheet with a separator of Comparative Example 1 was produced in the same manner as the optical pressure-sensitive adhesive sheet with a separator of 1.
  • Example 2 Example 1 except that a biaxially stretched polypropylene film (trade name "Trefan # 30-2500H", thickness 75 ⁇ m, filler-containing film, manufactured by Toray Industries, Inc.) was used as the base film for the separator instead of the COP film.
  • the optical pressure-sensitive adhesive sheet with a separator of Comparative Example 2 was produced in the same manner as the optical pressure-sensitive adhesive sheet with a separator.
  • Example 3 Example 1 except that a biaxially stretched polyester film (trade name "Diafoil T100C50", thickness 50 ⁇ m, filler-containing PET film, manufactured by Mitsubishi Chemical Corporation) was used as the base film for the separator instead of the COP film.
  • the optical pressure-sensitive adhesive sheet with a separator of Comparative Example 3 was produced in the same manner as the optical pressure-sensitive adhesive sheet with a separator.
  • Light source White LED light source for irradiating the evaluation sample with inspection light
  • Camera device The sample transmitted light and sample reflected light of the inspection light are arranged so as to be able to be imaged, and have a resolution of 2.8 ⁇ m. Camera device
  • an optical adhesive sheet with a separator having a plan view size of 50 mm ⁇ 50 mm was prepared as a sample for evaluation.
  • the sample was set in the evaluation device in a state where the inner region (30 mm ⁇ 30 mm) surrounded by the outer region of the sample could be imaged by the camera device.
  • the sample is set in the evaluation device by having the chuck mechanism provided in the evaluation device grip the outer region of the sample.
  • ⁇ Second step> The sample set in the evaluation device was irradiated with the inspection light from the white LED light source, and the sample transmitted light and the sample reflected light were received by the camera device over the entire inner region. As a result, the received light data was acquired over the inner region.
  • the position information derived in the third step includes XY coordinate information with the projection plane as the XY plane and Z coordinate information with the thickness direction orthogonal to the XY plane as the Z direction. Is done.
  • the projection image information derived in the third step is information that can derive the total area of the foreign matter, the size of each foreign matter, and the size distribution of the foreign matter based on the projection image information.
  • Foreign matter area ratio R1 is the ratio of the total projected area of foreign matter on the projection surface of the plan view projection by the above evaluation method. Regarding the foreign matter area ratio R1, when it is 10% or less, it is evaluated as “excellent”, when it exceeds 10% and 20% or less, it is evaluated as “good”, and when it exceeds 20%, it is evaluated as “bad”. evaluated. The evaluation results are shown in Table 1.
  • Bubble area ratio R2 is the ratio of the total projected area of bubbles on the projection plane of the plan view projection. Regarding the bubble area ratio R2, when it is 5% or less, it is evaluated as “excellent”, when it exceeds 5% and 10% or less, it is evaluated as “good”, and when it exceeds 10%, it is evaluated as “bad”. evaluated. The evaluation results are shown in Table 1.
  • the maximum foreign matter length L1 is the maximum length of the maximum foreign matter in the plan view projection. Regarding the maximum foreign matter length L1, when it is 20 ⁇ m or less, it is evaluated as “excellent”, when it is more than 20 ⁇ m and 30 ⁇ m or less, it is evaluated as “good”, and when it is more than 30 ⁇ m and 50 ⁇ m or less, it is “possible”. It was evaluated as "defective” when it exceeded 50 ⁇ m. The evaluation results are shown in Table 1.
  • the maximum foreign matter length L2 is the maximum length of the maximum foreign matter between the separator and the optical adhesive sheet (adhesive layer) in the plan view projection. Regarding the maximum foreign matter length L2, the case of 20 ⁇ m or less is evaluated as “excellent”, the case of exceeding 20 ⁇ m and 30 ⁇ m or less is evaluated as “good”, and the case of exceeding 30 ⁇ m and 50 ⁇ m or less is “possible”. It was evaluated as "defective" when it exceeded 50 ⁇ m. The evaluation results are shown in Table 1.
  • Foreign matter area ratio R3 is the ratio of the total projected area of foreign matter on the projection surface of the plan view projection by the above evaluation method for the separator. Regarding the foreign matter area ratio R3, when it is 10% or less, it is evaluated as “excellent”, when it exceeds 10% and 20% or less, it is evaluated as “good”, and when it exceeds 20%, it is evaluated as "bad”. evaluated. The evaluation results are shown in Table 2.
  • the maximum foreign matter length L3 is the maximum length of the foreign matter that is the largest in the plan view projection of the separator. Regarding the maximum foreign matter length L3, when it is 15 ⁇ m or less, it is evaluated as “excellent”, when it is more than 15 ⁇ m and 30 ⁇ m or less, it is evaluated as “good”, and when it is more than 30 ⁇ m and 50 ⁇ m or less, it is “possible”. It was evaluated as "defective" when it exceeded 50 ⁇ m. The evaluation results are shown in Table 2.
  • the number N1 is the number of foreign substances having a maximum length of 20 ⁇ m or more and 30 ⁇ m or less in the plan view projection of the separator.
  • the number N2 is the number of foreign substances having a maximum length of 15 ⁇ m or more and 30 ⁇ m or less in the plan view projection of the separator. These are shown in Table 2. In each separator in Comparative Examples 1 to 3, N1 exceeded 20 and N2 exceeded 100.
  • ⁇ Surface roughness of separator> The surface roughness of each separator in Examples 1 and 2 and Comparative Examples 1 to 3 was examined. Specifically, first, the surface roughness Ra (arithmetic mean roughness) of the exposed surface of the release layer of the separator is set to 0.7 mm ⁇ 0 by a scanning white interferometer (trade name “NewView7300”, manufactured by Zyg Congress). It was obtained from an observation image of .52 mm. Further, the surface roughness Rz (ten-point average roughness) of the exposed surface of the release layer of the separator was obtained from an observation image of 0.7 mm ⁇ 0.52 mm by the scanning white meter. Table 2 shows each surface roughness Ra and Rz (nm).
  • the optical adhesive sheet with a separator of the present invention can be used for manufacturing an optical article such as a display panel, for example.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Adhesive Tapes (AREA)
  • Laminated Bodies (AREA)

Abstract

Cette feuille adhésive sensible à la pression (X) est une feuille adhésive sensible à la pression optique recouverte d'un séparateur comprenant une couche d'adhésif sensible à la pression (20) et un séparateur (10) disposé sur un côté d'épaisseur de la couche d'adhésif sensible à la pression (20). La feuille adhésive sensible à la pression (X), lorsqu'elle est examinée selon un procédé d'évaluation donné, présente une proportion de la surface projetée totale de substances étrangères dans la zone projetée d'une vue en plan inférieure ou égale à 20 %.
PCT/JP2021/035339 2020-09-30 2021-09-27 Feuille adhésive sensible à la pression optique avec séparateur WO2022071212A1 (fr)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005154689A (ja) * 2003-11-28 2005-06-16 Hitachi Chem Co Ltd セパレータ付き感圧型接着シート及び光学部材組立体並びにその組立方法
JP2008302580A (ja) * 2007-06-07 2008-12-18 Nitto Denko Corp 光学フィルム用粘着シート、その製造方法、粘着型光学フィルムおよび画像表示装置
JP2013060555A (ja) * 2011-09-14 2013-04-04 Lintec Corp 離型フィルム及びその製造方法
JP2015078251A (ja) * 2013-10-15 2015-04-23 三菱樹脂株式会社 基材レス両面粘着シート
JP2020083908A (ja) * 2018-11-15 2020-06-04 王子ホールディングス株式会社 積層シート

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4790472B2 (ja) 2006-03-31 2011-10-12 三井化学株式会社 粘着フィルム用セパレーター

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005154689A (ja) * 2003-11-28 2005-06-16 Hitachi Chem Co Ltd セパレータ付き感圧型接着シート及び光学部材組立体並びにその組立方法
JP2008302580A (ja) * 2007-06-07 2008-12-18 Nitto Denko Corp 光学フィルム用粘着シート、その製造方法、粘着型光学フィルムおよび画像表示装置
JP2013060555A (ja) * 2011-09-14 2013-04-04 Lintec Corp 離型フィルム及びその製造方法
JP2015078251A (ja) * 2013-10-15 2015-04-23 三菱樹脂株式会社 基材レス両面粘着シート
JP2020083908A (ja) * 2018-11-15 2020-06-04 王子ホールディングス株式会社 積層シート

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