WO2016080431A1 - 有機el表示装置用円偏光板および有機el表示装置 - Google Patents
有機el表示装置用円偏光板および有機el表示装置 Download PDFInfo
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- WO2016080431A1 WO2016080431A1 PCT/JP2015/082368 JP2015082368W WO2016080431A1 WO 2016080431 A1 WO2016080431 A1 WO 2016080431A1 JP 2015082368 W JP2015082368 W JP 2015082368W WO 2016080431 A1 WO2016080431 A1 WO 2016080431A1
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- 150000003839 salts Chemical class 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 238000001577 simple distillation Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical group C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
- 238000001721 transfer moulding Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/80—Constructional details
- H10K59/8793—Arrangements for polarized light emission
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
- H05B33/04—Sealing arrangements, e.g. against humidity
Definitions
- the present invention relates to a circularly polarizing plate for an organic EL display device and an organic EL display device.
- the present invention has been made to solve the above-described conventional problems, and its main purpose is circular polarization for organic EL display devices having an excellent antireflection function and an excellent organic EL panel protection function. To provide a board.
- the circularly polarizing plate of the present invention is used for an organic EL display device.
- This circularly polarizing plate includes a polarizer, a retardation layer functioning as a ⁇ / 4 plate, a barrier layer, and an adhesive layer having a barrier function in this order, and the absorption axis of the polarizer and the retardation
- the angle formed with the slow axis of the layer is 35 ° to 55 °.
- the circularly polarizing plate further includes another retardation layer functioning as a ⁇ / 2 plate between the polarizer and the retardation layer, and the absorption axis of the polarizer and the retardation layer
- the angle formed between the slow axis of the retardation layer is 65 ° to 85 °, and the angle formed between the absorption axis of the polarizer and the slow axis of the other retardation layer is 10 ° to 20 °.
- the circularly polarizing plate further includes a protective film between the polarizer and the retardation layer.
- the circularly polarizing plate further includes a protective film between the polarizer and the other retardation layer.
- the circularly polarizing plate further includes a protective film on the opposite side of the polarizer from the retardation layer.
- the polarizer is elongated and has the absorption axis in the longitudinal direction; the retardation layer is elongated and is 35 with respect to the longitudinal direction. It has the slow axis in the direction of ° to 55 °.
- the polarizer is elongated and has the absorption axis in the longitudinal direction; the retardation layer and the other retardation layer are elongated, and The retardation layer has the slow axis in the direction of 65 ° to 85 ° with respect to the longitudinal direction, and the other retardation layer has the retardation in the direction of 10 ° to 20 ° with respect to the longitudinal direction.
- the ratio K / I of potassium content (% by weight) to iodine content (% by weight) in the polarizer is 0.180 to 0.235.
- an organic EL display device is provided. This organic display device includes the circularly polarizing plate described above.
- an organic EL panel protective function can be imparted by forming a barrier layer on the surface of the retardation layer. Furthermore, since the barrier layer can be formed while maintaining the optical properties and mechanical properties of the retardation film (retardation layer) within a desired range, an excellent antireflection function and an excellent organic property can be formed. A circularly polarizing plate having both an EL panel protective function can be obtained. In addition, according to one embodiment of the present invention, since only one ⁇ / 4 plate is used as the retardation layer, and the ⁇ / 4 plate also serves as an inner protective film of the polarizer, the thickness can be significantly reduced. Can be realized.
- Refractive index (nx, ny, nz) “Nx” is the refractive index in the direction in which the in-plane refractive index is maximum (ie, the slow axis direction), and “ny” is the direction orthogonal to the slow axis in the plane (ie, the fast axis direction). “Nz” is the refractive index in the thickness direction.
- Refractive index (nx, ny, nz) “Nx” is the refractive index in the direction in which the in-plane refractive index is maximum (ie, the slow axis direction), and “ny” is the direction orthogonal to the slow axis in the plane (ie, the fast axis direction). “Nz” is the refractive index in the thickness direction.
- In-plane retardation (Re) “Re ( ⁇ )” is an in-plane retardation measured with light having a wavelength of ⁇ nm at 23 ° C.
- Re (550) is an in-plane retardation measured with light having a wavelength of 550 nm at 23 ° C.
- Thickness direction retardation (Rth) is a retardation in the thickness direction measured with light having a wavelength of ⁇ nm at 23 ° C.
- Rth (550) is a retardation in the thickness direction measured with light having a wavelength of 550 nm at 23 ° C.
- the circular polarizing plate according to the embodiment of the present invention is used in an organic EL display device.
- a circularly polarizing plate according to one embodiment of the present invention includes a polarizer, a retardation layer functioning as a ⁇ / 4 plate, a barrier layer, and an adhesive layer having a barrier function in this order.
- the circularly polarizing plate according to another embodiment of the present invention further includes another retardation layer that functions as a ⁇ / 2 plate between the polarizer and the retardation layer.
- the overall configuration of the circularly polarizing plate will be specifically described with respect to these representative embodiments, and then each layer and the optical film constituting the circularly polarizing plate will be described in detail.
- FIG. 1 is a schematic sectional view of a circularly polarizing plate according to one embodiment of the present invention.
- the circularly polarizing plate 100 of the present embodiment includes a polarizer 10, a retardation layer 20, a barrier layer 30, and an adhesive layer 40 in this order.
- the retardation layer 20 functions as a ⁇ / 4 plate
- the pressure-sensitive adhesive layer 40 has a barrier function.
- the circularly polarizing plate 100 in the illustrated example includes a protective film 50 on the side opposite to the retardation layer 20 of the polarizer.
- the circularly polarizing plate may include another protective film (also referred to as an inner protective film: not shown) between the polarizer and the retardation layer.
- the inner protective film is omitted.
- the retardation layer 20 can also function as an inner protective film. With such a configuration, the circularly polarizing plate can be further reduced in thickness.
- the angle formed by the absorption axis of the polarizer 10 and the slow axis of the retardation layer 20 is 35 ° to 55 °, preferably 38 ° to 52 °, more preferably 40 ° to It is 50 °, more preferably 42 ° to 48 °, and particularly preferably 44 ° to 46 °. If the angle is in such a range, a desired circular polarization function can be realized. Note that when an angle is referred to in this specification, the angle includes both clockwise and counterclockwise angles unless otherwise specified.
- FIG. 2 is a schematic cross-sectional view of a circularly polarizing plate according to another embodiment of the present invention.
- the circularly polarizing plate 101 of this embodiment further includes another retardation layer 60 between the polarizer 10 and the retardation layer 20.
- Another retardation layer 60 functions as a ⁇ / 2 plate.
- the retardation layer 20 may be referred to as a first retardation layer
- the other retardation layer 60 may be referred to as a second retardation layer.
- the circularly polarizing plate 101 in the illustrated example includes a protective film 50 on the side opposite to the retardation layer of the polarizer.
- the circularly polarizing plate may include another protective film (also referred to as an inner protective film: not shown) between the polarizer and the retardation layer.
- another protective film also referred to as an inner protective film: not shown
- the inner protective film is omitted.
- the second retardation layer 60 can also function as an inner protective film.
- the angle formed by the absorption axis of the polarizer 10 and the slow axis of the first retardation layer 20 is preferably 65 ° to 85 °, more preferably 72 ° to 78 °. More preferably, it is about 75 °.
- the angle formed by the absorption axis of the polarizer 10 and the slow axis of the second retardation layer 60 is preferably 10 ° to 20 °, more preferably 13 ° to 17 °, and still more preferably. About 15 °.
- Polarizer Any appropriate polarizer may be adopted as the polarizer 10.
- Specific examples include hydrophilic polymer films such as polyvinyl alcohol films, partially formalized polyvinyl alcohol films, and ethylene / vinyl acetate copolymer partially saponified films, and dichroic substances such as iodine and dichroic dyes.
- examples thereof include polyene-based oriented films such as those subjected to the dyeing treatment and stretching treatment according to the above, polyvinyl alcohol dehydrated products and polyvinyl chloride dehydrochlorinated products.
- a polarizer obtained by dyeing a polyvinyl alcohol film with iodine and uniaxially stretching is used because of excellent optical properties.
- the dyeing with iodine is performed, for example, by immersing a polyvinyl alcohol film in an aqueous iodine solution.
- the stretching ratio of the uniaxial stretching is preferably 3 to 7 times.
- the stretching may be performed after the dyeing treatment or may be performed while dyeing. Moreover, you may dye
- the polyvinyl alcohol film is subjected to swelling treatment, crosslinking treatment, washing treatment, drying treatment and the like. For example, by immersing a polyvinyl alcohol film in water and washing it before dyeing, not only can the surface of the polyvinyl alcohol film be cleaned and anti-blocking agents can be washed, but the polyvinyl alcohol film can be swollen and dyed.
- the polyvinyl alcohol-based film may be a single-layer film (ordinary film-formed film) or may be a polyvinyl alcohol-based resin layer applied and formed on a resin base material.
- Techniques for making polarizers from single-layer polyvinyl alcohol-based films are well known in the art. A technique for producing a polarizer from a polyvinyl alcohol-based resin layer formed by coating on a resin substrate is described, for example, in JP-A-2009-098653.
- the thickness of the polarizer is typically about 1 ⁇ m to 80 ⁇ m.
- the ratio K / I of potassium content (wt%) to iodine content (wt%) in the polarizer is preferably 0.180 to 0.235, more preferably 0.200. ⁇ 0.230. If K / I is in such a range, a polarizer having very excellent heat resistance can be obtained. As a result, a circularly polarizing plate capable of realizing an organic EL display device having extremely excellent durability can be obtained by a synergistic effect with the barrier properties of the barrier layer and the pressure-sensitive adhesive layer. More specifically, a circularly polarizing plate including such a polarizer having K / I typically has a small hue change due to heating. For example, the amount of change in the a value (hunter color system) after heating the circularly polarizing plate at 95 ° C. for 500 hours is, for example, 7 or less, preferably 5 or less, more preferably 3 or less.
- the polarizer preferably contains a zinc component.
- the zinc component include zinc chloride and zinc sulfate.
- the retardation layer 20 can function as a ⁇ / 4 plate as described above.
- the in-plane retardation Re (550) of such a retardation layer is 100 nm to 180 nm, preferably 110 nm to 170 nm, more preferably 120 nm to 160 nm, and particularly preferably 135 nm to 155 nm.
- the thickness of the retardation layer can be set so as to function most appropriately as a ⁇ / 4 plate. In other words, the thickness can be set so as to obtain a desired in-plane retardation. Specifically, the thickness is preferably 10 ⁇ m to 80 ⁇ m, more preferably 10 ⁇ m to 60 ⁇ m, and most preferably 30 ⁇ m to 50 ⁇ m.
- the retardation layer may exhibit reverse dispersion wavelength characteristics in which the retardation value increases with the wavelength of the measurement light, or may exhibit positive wavelength dispersion characteristics in which the retardation value decreases with the wavelength of the measurement light.
- the phase difference value may exhibit a flat chromatic dispersion characteristic that hardly changes depending on the wavelength of the measurement light. It is preferable to exhibit a flat wavelength dispersion characteristic.
- the retardation layer may be composed of any appropriate resin film that can satisfy the optical characteristics and mechanical characteristics as described above.
- Representative examples of such resins include cellulose resins, polyesters, polyvinyl alcohols, polyvinyl acetals, polycarbonates, polyamides, polyimides, polyethersulfones, polyethers, polysulfones, polystyrenes, cyclic Examples thereof include resins such as olefin-based (polynorbornene-based), polyolefin-based, acrylic-based, urethane-based, acrylic-urethane-based, and acetate-based transparent resins.
- the retardation layer 20 can be preferably formed of a polycarbonate resin.
- the polycarbonate resin that can be used in this embodiment includes at least a structural unit derived from a dihydroxy compound having a bond structure represented by the following structural formula (1), and has at least one bond structure —CH 2 in the molecule. It is produced by reacting a dihydroxy compound containing at least a dihydroxy compound having —O— with a carbonic acid diester in the presence of a polymerization catalyst.
- the dihydroxy compound having a bond structure represented by the structural formula (1) includes a structure having two alcoholic hydroxyl groups and a linking group —CH 2 —O— in the molecule, in the presence of a polymerization catalyst. Any compound having any structure can be used as long as it is a compound capable of reacting with a carbonic acid diester to form a polycarbonate, and a plurality of types of compounds may be used in combination. Moreover, you may use together the dihydroxy compound which does not have the coupling
- a dihydroxy compound having a bond structure represented by the structural formula (1) may be abbreviated as a dihydroxy compound (A), and a dihydroxy compound not having a bond structure represented by the structural formula (1) may be abbreviated as a dihydroxy compound (B). is there.
- the “linking group —CH 2 —O—” in the dihydroxy compound (A) means a structure constituting a molecule by bonding to atoms other than hydrogen atoms.
- this linking group at least an atom to which an oxygen atom can be bonded or an atom to which a carbon atom and an oxygen atom can be bonded simultaneously is most preferably a carbon atom.
- the number of “linking group —CH 2 —O—” in the dihydroxy compound (A) is 1 or more, preferably 2 to 4.
- examples of the dihydroxy compound (A) include 9,9-bis (4- (2-hydroxyethoxy) phenyl) fluorene and 9,9-bis (4- (2-hydroxyethoxy) -3. -Methylphenyl) fluorene, 9,9-bis (4- (2-hydroxyethoxy) -3-isopropylphenyl) fluorene, 9,9-bis (4- (2-hydroxyethoxy) -3-isobutylphenyl) fluorene, 9,9-bis (4- (2-hydroxyethoxy) -3-tert-butylphenyl) fluorene, 9,9-bis (4- (2-hydroxyethoxy) -3-cyclohexylphenyl) fluorene, 9,9- Screw( 4- (2-hydroxyethoxy) -3-phenylphenyl) fluorene, 9,9-bis (4- (2-hydroxyethoxy) -3,5-dimethylphenyl) fluorene, 9,9-bis (4- (2-bis (4
- bis (hydroxyalkoxyaryl) alkanes 1,1-bis [4- (2-hydroxyethoxy) phenyl] silane
- 1,1-bis [3-cyclohexyl-4- (2-hydroxyethoxy) phenyl] cyclohexane 1,1-bis [4- (2-hydroxyethoxy) phenyl] cyclopentane, etc.
- dihydroxy compounds (A) may be used alone or in combination of two or more.
- dihydroxy compound represented by the formula (4) include isosorbide, isomannide and isoidet which are in a stereoisomeric relationship, and these may be used alone or in combination of two or more. May be.
- the use ratio of the dihydroxy compound represented by Formula (4) and the other dihydroxy compound is as described later as the ratio of the structural unit derived from each dihydroxy compound constituting the polycarbonate resin.
- dihydroxy compounds (A) isosorbide obtained by dehydrating condensation of sorbitol produced from various starches that are abundant as resources and are readily available is easy to obtain and produce, and optical characteristics From the viewpoint of moldability, it is most preferable.
- isosorbide Since isosorbide is apt to be gradually oxidized by oxygen, it is important to use an oxygen scavenger or in a nitrogen atmosphere in order to prevent decomposition due to oxygen during storage and handling during production. It is also necessary to prevent moisture from entering.
- decomposition products such as formic acid are generated.
- the resulting polycarbonate may be colored or the physical properties may be significantly deteriorated.
- the polymerization reaction may be affected, and a high molecular weight polymer may not be obtained.
- the resulting polycarbonate may be colored or the physical properties may be remarkably deteriorated.
- a reducing agent or an antacid is used as the stabilizer.
- the reducing agent include sodium borohydride and lithium borohydride
- examples of the antacid include sodium hydroxide. Since the alkali metal serves as a polymerization catalyst when the alkali metal salt is added, the polymerization reaction may not be controlled if it is added excessively.
- isosorbide may be distilled as necessary.
- isosorbide may be distilled as necessary in order to remove them.
- the distillation of isosorbide may be simple distillation or continuous distillation, and is not particularly limited. After the atmosphere is an inert gas atmosphere such as argon or nitrogen, distillation is performed under reduced pressure.
- the formic acid content is less than 20 ppm, preferably 10 ppm or less, more preferably 5 ppm or less, further preferably 3 ppm or less, and particularly preferably no formic acid. can do.
- the content of the alkali and / or alkaline earth metal compound is 10 ⁇ mol or less, preferably 5 ⁇ mol or less, more preferably 3 ⁇ mol or less, even more preferably 1 ⁇ mol or less as a metal conversion amount with respect to 1 mol of isosorbide.
- the purity can be made high so as not to contain any alkali and / or alkaline earth metal compound.
- a dihydroxy compound (A) having a formic acid content of less than 20 ppm for example, a dihydroxy compound represented by the general formula (1).
- the formic acid content is preferably 10 ppm or less, more preferably 5 ppm or less, still more preferably 3 ppm or less, and particularly preferably no formic acid generated by decomposition of the dihydroxy compound (A) or the like.
- the dihydroxy compound (A) having a low content of formic acid and alkali and / or alkaline earth metal compound for example, the dihydroxy compound represented by the formula (4) is specifically used for the reaction with the carbonic acid diester.
- Such means is not particularly limited, and for example, the following method can be employed.
- a high-purity dihydroxy compound (A), for example, the dihydroxy compound represented by the formula (4), is stored until immediately before the reaction with the carbonic acid diester, preferably in an inert gas atmosphere or an atmosphere free of oxygen such as a reduced pressure or vacuum atmosphere. To do. In the case of storage in an environment of 40 ° C.
- the reaction system with the carbonic acid diester usually within 2 weeks, more preferably within 1 week. If the environment is stored at 40 ° C. and 80% RH, the dihydroxy compound represented by the above formula (4) is usually polymerized within 2 weeks, preferably within 1 week, even if left in the atmosphere. Will not be disturbed. 40 ° C, 80 When the temperature and humidity are lower than% RH, the storage period can be made longer.
- the inert gas atmosphere includes an atmosphere in which one or two or more oxygen contents such as nitrogen and argon are 1000 ppm or less, and particularly an atmosphere containing no oxygen at all.
- An atmosphere with an oxygen content of 100 ppm or less at 3 kPa or less is included.
- an oxygen scavenger mainly composed of iron powder for example, an oxygen scavenger such as AGELESS (Mitsubishi Gas Chemical Co., Ltd.), Oxita (manufactured by Ueno Pharmaceutical Co., Ltd.), silica gel, A desiccant such as molecular sieve or aluminum oxide may coexist.
- the dihydroxy compound (A) for example, isosorbide
- the storage temperature is 40 ° C. or lower
- an oxygen scavenger is allowed to coexist and an environment having an oxygen concentration of 1000 ppm or lower is maintained in an inert gas atmosphere.
- the storage temperature is 40 ° C. or lower, preferably 25 ° C. or lower, more preferably 10 ° C. or lower, and particularly preferably 5 ° C. or lower.
- Powder and flaky isosorbide can be stored even under high humidity of 80% RH, but there is a change in mass due to moisture absorption. Storage in an inert gas atmosphere is preferable. Furthermore, these conditions can be used in appropriate combinations.
- the dihydroxy compound (A) for example, the dihydroxy compound represented by the formula (4), for the reaction with the carbonic acid diester described later, the form is not particularly limited, A liquid state such as a molten state or an aqueous solution may be used.
- ⁇ Dihydroxy compound (B)> In the said polycarbonate resin, you may use the dihydroxy compound (B) which is dihydroxy compounds other than a dihydroxy compound (A) as a dihydroxy compound.
- the dihydroxy compound (B) include alicyclic dihydroxy compounds, aliphatic dihydroxy compounds, oxyalkylene glycols, aromatic dihydroxy compounds, diols having a cyclic ether structure, and the like as dihydroxy compounds that constitute polycarbonate structural units.
- a dihydroxy compound (A) for example, a dihydroxy compound represented by the formula (4).
- the alicyclic dihydroxy compound that can be used for the polycarbonate resin is not particularly limited, but preferably a compound containing a 5-membered ring structure or a 6-membered ring structure is usually used.
- the 6-membered ring structure may be fixed in a chair shape or a boat shape by a covalent bond.
- the heat resistance of the obtained polycarbonate can be increased.
- the number of carbon atoms contained in the alicyclic dihydroxy compound is usually 70 or less, preferably 50 or less, more preferably 30 or less. The higher this value, the higher the heat resistance, but the synthesis becomes difficult, the purification becomes difficult, and the cost is expensive. The smaller the number of carbon atoms, the easier the purification and the easier it is to obtain.
- alicyclic dihydroxy compound containing a 5-membered ring structure or a 6-membered ring structure include alicyclic dihydroxy compounds represented by the following general formula (II) or (III).
- HOCH 2 —R 1 —CH 2 OH (II) HO—R 2 —OH (III) (Formula (II), (III), R 1, R 2, respectively, showing a cycloalkylene group having 4 to 20 carbon atoms.)
- cyclohexanedimethanol which is an alicyclic dihydroxy compound represented by the above general formula (II), in general formula (II), R 1 is represented by the following general formula (IIa) (wherein R 3 has 1 to 12 alkyl groups or hydrogen atoms are included).
- Specific examples thereof include 1,2-cyclohexanedimethanol, 1,3-cyclohexanedimethanol, 1,4-cyclohexanedimethanol and the like.
- R 1 is represented by the following general formula (IIb) (in the formula: , N represents 0 or 1).
- R 1 is represented by the following general formula (IIc) (wherein m represents 0 or 1). Specific examples thereof include 2,6-decalin dimethanol, 1,5-decalin dimethanol, 2,3-decalin dimethanol and the like.
- norbornanedimethanol which is an alicyclic dihydroxy compound represented by the above general formula (II)
- various isomers in which R 1 is represented by the following general formula (IId) in the general formula (II) include 2,3-norbornane dimethanol and 2,5-norbornane dimethanol.
- the adamantane dimethanol which is an alicyclic dihydroxy compound represented by the general formula (II), includes various isomers in which R 1 is represented by the following general formula (IIe) in the general formula (II). Specific examples thereof include 1,3-adamantane dimethanol and the like.
- cyclohexanediol which is an alicyclic dihydroxy compound represented by the general formula (III), in general formula (III), R 2 is represented by the following general formula (IIIa) (wherein, R 3 is a C1- 12 alkyl groups or hydrogen atoms are included).
- R 3 is a C1- 12 alkyl groups or hydrogen atoms are included.
- Specific examples of such compounds include 1,2-cyclohexanediol, 1,3-cyclohexanediol, 1,4-cyclohexanediol, 2-methyl-1,4-cyclohexanediol, and the like.
- R 2 represents the following general formula (IIIb) (wherein n Represents 0 or 1).
- R 2 is represented by the following general formula (IIIc) (where m is 0 , Or 1) is included. Specifically, 2,6-decalindiol, 1,5-decalindiol, 2,3-decalindiol, and the like are used.
- the norbornanediol which is an alicyclic dihydroxy compound represented by the above general formula (III) includes various isomers in which R 2 is represented by the following general formula (IIId) in the general formula (III). Specifically, 2,3-norbornanediol, 2,5-norbornanediol and the like are used.
- the adamantanediol which is an alicyclic dihydroxy compound represented by the above general formula (III) includes various isomers in which R 2 is represented by the following general formula (IIIe) in the general formula (III). Specifically, 1,3-adamantanediol or the like is used as such.
- cyclohexane dimethanols tricyclodecane dimethanols, adamantane diols, and pentacyclopentadecane dimethanols are particularly preferable, and are easily available and easy to handle. From this viewpoint, 1,4-cyclohexanedimethanol, 1,3-cyclohexanedimethanol, 1,2-cyclohexanedimethanol, and tricyclodecane dimethanol are preferable.
- Usable aliphatic dihydroxy compounds include, for example, ethylene glycol, 1,3-propanediol, 1,2-propanediol, 1,4-butanediol, 1,3-butanediol, 1,2-butanediol, Examples include 1,5-heptanediol, 1,6-hexanediol, and the like.
- Examples of usable oxyalkylene glycols include diethylene glycol, triethylene glycol, tetraethylene glycol, and polyethylene glycol.
- diols having a cyclic ether structure examples include spiroglycols and dioxane glycols.
- the above exemplary compounds are examples of alicyclic dihydroxy compounds, aliphatic dihydroxy compounds, oxyalkylene glycols, aromatic dihydroxy compounds, and diols having a cyclic ether structure that can be used in the present invention. It is not limited. These compounds can be used alone or in combination with a dihydroxy compound represented by the formula (4).
- the ratio of the dihydroxy compound (A) to the total dihydroxy compound constituting the polycarbonate resin is not particularly limited, but is preferably 10 mol% or more, more preferably 40 mol% or more, and further Preferably it is 60 mol% or more, Preferably it is 90 mol% or less, More preferably, it is 80 mol% or less, More preferably, it is 70 mol% or less.
- the content ratio of structural units derived from other dihydroxy compounds is too large, performance such as optical characteristics may be deteriorated.
- the dihydroxy compound (A) for all dihydroxy compounds constituting the polycarbonate for example, the dihydroxy compound represented by the formula (4) and the alicyclic dihydroxy compound
- the total ratio is not particularly limited, but is preferably 80 mol% or more, more preferably 90 mol% or more, and particularly preferably 95 mol% or more.
- the content rate of the structural unit derived from the dihydroxy compound (A), for example, the dihydroxy compound represented by Formula (4), and the structural unit derived from an alicyclic dihydroxy compound in polycarbonate resin it is arbitrary ratios.
- the structural unit derived from the alicyclic dihydroxy compound is preferably 10:90 to 90:10 (mol%).
- dihydroxy compounds (A) for all dihydroxy compounds constituting the polycarbonate for example, represented by the formula (4)
- the ratio of the total of the dihydroxy compound and each of these dihydroxy compounds is not particularly limited, and can be selected at an arbitrary ratio.
- the content rate of the structural unit derived from the dihydroxy compound (A), for example, the dihydroxy compound represented by the formula (4) and the structural unit derived from each of these dihydroxy compounds is not particularly limited, and is selected at an arbitrary ratio. it can.
- the degree of polymerization of a polycarbonate resin having a structural unit derived from the above-mentioned dihydroxy compound (hereinafter sometimes referred to as “polycarbonate copolymer”) is phenol, 1,1,2,2-tetrachloroethane as a solvent.
- polycarbonate copolymer phenol, 1,1,2,2-tetrachloroethane as a solvent.
- the polycarbonate concentration was precisely adjusted to 1.00 g / dl, and the reduced viscosity measured at a temperature of 30.0 ° C. ⁇ 0.1 ° C. (hereinafter simply referred to as “reduced viscosity of polycarbonate”).
- the polymerization is preferably 0.40 dl / g or more, more preferably 0.43 dl / g or more, and usually polymerization of 2.00 dl / g or less, preferably 1.60 dl / g or less.
- the mechanical strength at the time of molding is often weak.
- the reduced viscosity of the polycarbonate is increased, the fluidity at the time of molding is lowered, the cycle characteristics are lowered, the molding cycle is lengthened, and the birefringence of the obtained molded product tends to be increased.
- the Abbe number of the polycarbonate resin is preferably 20 or more, more preferably 50 or more, and particularly preferably 55 or more.
- the larger this value the smaller the wavelength dispersion of the refractive index and the smaller the aberration, making it suitable as an optical film.
- the upper limit is not particularly limited.
- the 5% heat loss temperature of the polycarbonate resin is preferably 340 ° C. or higher, more preferably 345 ° C. or higher.
- the higher the 5% heat loss temperature the higher the thermal stability and the better the use at higher temperatures.
- the manufacturing temperature can be increased, and the control range at the time of manufacturing can be widened.
- the lower the temperature the lower the thermal stability, making it difficult to use at high temperatures.
- the allowable control width at the time of manufacture becomes narrow and difficult to make. Accordingly, the upper limit of the 5% heat loss temperature is not particularly limited, and the higher the better, the higher the decomposition temperature of the copolymer.
- the Izod impact strength of the polycarbonate resin is preferably 30 J / m 2 or more. The greater the Izod impact strength, the higher the strength of the molded body and the less likely it will break, so the upper limit is not particularly limited.
- the polycarbonate resin preferably has a generated gas amount other than the phenol component per unit area at 110 ° C. (hereinafter sometimes simply referred to as “generated gas amount”) of 5 ng / cm 2 or less. More preferably, the amount of generated gas derived from a dihydroxy compound other than the dihydroxy compound represented by formula (4) is 0.5 ng / cm 2 or less.
- the polycarbonate resin gives a single glass transition temperature when differential scanning calorimetry (DSC) is performed, but adjusts the type and mixing ratio of the dihydroxy compound and the alicyclic dihydroxy compound represented by the formula (4).
- the glass transition temperature can be obtained as a polymer having an arbitrary glass transition temperature from about 45 ° C. to about 155 ° C., for example, depending on the application.
- the glass transition temperature of the polycarbonate resin is preferably adjusted to 45 ° C. or higher, for example, 45 to 130 ° C.
- the polycarbonate resin preferably has at least two of the above physical properties, and more preferably has other physical properties.
- the polycarbonate resin can be produced by a melt polymerization method in which a dihydroxy compound containing the dihydroxy compound (A) is reacted with a carbonic acid diester in the presence of a polymerization catalyst.
- a carbonic acid diester used in the method for producing a polycarbonate resin include diphenyl carbonate, substituted diphenyl carbonate typified by ditolyl carbonate, dimethyl carbonate, diethyl carbonate, and di-t-butyl carbonate. Particularly preferred is diphenyl carbonate. And carbonates and substituted diphenyl carbonates. These carbonic acid diesters may be used alone or in combination of two or more.
- the carbonic acid diester is preferably used in a molar ratio of 0.90 to 1.10, more preferably 0.96 to 1.04, based on all dihydroxy compounds used in the reaction.
- this molar ratio is less than 0.90, the terminal OH group of the produced polycarbonate increases, and the thermal stability of the polymer may deteriorate, or the desired high molecular weight product may not be obtained.
- the molar ratio exceeds 1.10, the rate of the transesterification reaction decreases under the same conditions, and it becomes difficult to produce a polycarbonate having a desired molecular weight.
- the amount of residual carbonic acid diester in the coalescence increases, and this residual carbonic acid diester may cause odor during molding or in the molded product.
- the retardation layer 20 can be preferably formed of a cyclic olefin resin.
- the cyclic olefin-based resin is a general term for resins that are polymerized using a cyclic olefin as a polymerization unit, and is described in, for example, JP-A-1-240517, JP-A-3-14882, JP-A-3-122137, and the like. Resin.
- ring-opening (co) polymers of cyclic olefins include ring-opening (co) polymers of cyclic olefins, addition polymers of cyclic olefins, copolymers of cyclic olefins and ⁇ -olefins such as ethylene and propylene (typically random copolymers). And graft modified products in which these are modified with an unsaturated carboxylic acid or a derivative thereof, and hydrides thereof.
- the cyclic olefin include norbornene monomers.
- norbornene-based monomer examples include norbornene and alkyl and / or alkylidene substituted products thereof such as 5-methyl-2-norbornene, 5-dimethyl-2-norbornene, 5-ethyl-2-norbornene, 5-butyl- 2-Norbornene, 5-ethylidene-2-norbornene, etc.
- Polar group substitution products such as halogens; dicyclopentadiene, 2,3-dihydrodicyclopentadiene, etc .; dimethanooctahydronaphthalene, alkyl and / or alkylidene substitution thereof
- polar group substituents such as halogen, for example, 6-methyl-1,4: 5,8-dimethano-1,4,4a, 5,6,7,8,8a-octahydronaphthalene, 6-ethyl -1,4: 5,8-dimethano-1,4,4a, 5,6,7,8,8a-octahi Lonaphthalene, 6-ethylidene-1,4: 5,8-dimethano-1,4,4a, 5,6,7,8,8a-octahydronaphthalene, 6-chloro-1,4: 5,8-dimethano -1,4,4a, 5,6,7,8,8a-octahydronaphthalene, 6-cyano
- cycloolefins capable of ring-opening polymerization can be used in combination as long as the object of the present invention is not impaired.
- cycloolefins include compounds having one reactive double bond such as cyclopentene, cyclooctene, and 5,6-dihydrodicyclopentadiene.
- the cyclic olefin resin preferably has a number average molecular weight (Mn) measured by a gel permeation chromatograph (GPC) method using a toluene solvent, preferably 25,000 to 200,000, more preferably 30,000 to 100,000. 000, most preferably 40,000 to 80,000.
- Mn number average molecular weight measured by a gel permeation chromatograph (GPC) method using a toluene solvent, preferably 25,000 to 200,000, more preferably 30,000 to 100,000. 000, most preferably 40,000 to 80,000.
- the retardation layer 20 is obtained, for example, by stretching a film formed from the resin.
- Any appropriate forming method can be adopted as a method of forming a film from the resin. Specific examples include compression molding methods, transfer molding methods, injection molding methods, extrusion molding methods, blow molding methods, powder molding methods, FRP molding methods, cast coating methods (for example, casting methods), calendar molding methods, and hot presses. Law. Extrusion molding or cast coating is preferred. This is because the smoothness of the resulting film can be improved and good optical uniformity can be obtained.
- the molding conditions can be appropriately set according to the composition and type of the resin used, the properties desired for the retardation layer, and the like. In addition, since many film products are marketed for the said resin, you may use the said commercial film as it is for a extending
- the stretching ratio of the film can vary depending on the in-plane retardation value and thickness desired for the retardation layer, the type of resin used, the thickness of the film used, the stretching temperature, and the like. Specifically, the draw ratio is preferably 1.75 times to 3.00 times, more preferably 1.80 times to 2.80 times, and most preferably 1.85 times to 2.60 times. By stretching at such a magnification, a retardation layer having an in-plane retardation capable of appropriately exhibiting the effects of the present invention can be obtained.
- the stretching temperature of the film can vary depending on the in-plane retardation value and thickness desired for the retardation layer, the type of resin used, the thickness of the film used, the stretching ratio, and the like. Specifically, the stretching temperature is preferably 125 ° C. to 150 ° C., more preferably 130 ° C. to 140 ° C., and most preferably 130 ° C. to 135 ° C. By extending
- any appropriate stretching method can be adopted as the stretching method of the film.
- various stretching methods such as free end stretching, fixed end stretching, free end contraction, and fixed end contraction can be used singly or simultaneously or sequentially.
- the stretching direction can also be performed in various directions and dimensions such as a horizontal direction, a vertical direction, a thickness direction, and a diagonal direction.
- the retardation layer is formed by stretching a resin film uniaxially at a free end or uniaxially at a fixed end.
- a resin film uniaxially at a free end or uniaxially at a fixed end there is a method of stretching between rolls having different peripheral speeds while running the resin film in the longitudinal direction.
- a specific example of the fixed end uniaxial stretching there is a method of stretching in the width direction (lateral direction) while running the resin film in the longitudinal direction.
- the retardation layer is produced by continuously stretching a long resin film obliquely in a direction at a predetermined angle with respect to the longitudinal direction.
- a long stretched film having an orientation angle of a predetermined angle with respect to the longitudinal direction of the film (slow axis in the direction of the predetermined angle) is obtained.
- a roll toe roll means the system laminated
- Examples of the stretching machine used for the oblique stretching include a tenter type stretching machine capable of adding feed forces, pulling forces, or pulling forces at different speeds in the lateral and / or longitudinal directions.
- the tenter type stretching machine includes a horizontal uniaxial stretching machine, a simultaneous biaxial stretching machine, and the like, but any suitable stretching machine can be used as long as a long resin film can be continuously stretched obliquely.
- Another Retardation Layer (second retardation layer) 60 can function as a ⁇ / 2 plate as described above.
- the in-plane retardation Re (550) of such a retardation layer is 180 nm to 320 nm, more preferably 200 nm to 290 nm, and further preferably 230 nm to 280 nm.
- the Nz coefficient of the other retardation layer is, for example, 0.9 to 2, preferably 1 to 1.5, and more preferably 1 to 1.3.
- the thickness of another retardation layer can be set so as to function most appropriately as a ⁇ / 2 plate.
- the thickness can be set so as to obtain a desired in-plane retardation.
- the thickness is preferably 10 ⁇ m to 60 ⁇ m, more preferably 30 ⁇ m to 50 ⁇ m.
- the other retardation layer preferably has an absolute value of the photoelastic coefficient of 2.0 ⁇ 10 ⁇ 11 m 2 / N or less, more preferably 2.0 ⁇ 10 ⁇ 13 m 2 / N to 1.5 ⁇ 10 ⁇ . 11 m 2 / N, more preferably includes a resin of 1.0 ⁇ 10 -12 m 2 /N ⁇ 1.2 ⁇ 10 -11 m 2 / N.
- the photoelastic coefficient is within such a range, a change in phase difference is unlikely to occur when shrinkage stress is generated during heating. Therefore, by forming the retardation layer using a resin having such a photoelastic coefficient, the thermal unevenness of the obtained organic EL display device can be satisfactorily prevented.
- the other retardation layer may exhibit a reverse dispersion wavelength characteristic in which the retardation value increases according to the wavelength of the measurement light, and exhibits a positive chromatic dispersion characteristic in which the retardation value decreases according to the wavelength of the measurement light.
- it may exhibit a flat wavelength dispersion characteristic in which the phase difference value hardly changes depending on the wavelength of the measurement light. It is preferable to exhibit a flat wavelength dispersion characteristic.
- Re (450) / Re (550) of the retardation layer is preferably from 0.99 to 1.03, and Re (650) / Re (550) is preferably from 0.98 to 1.02.
- Another retardation layer can be preferably formed of a cyclic olefin-based resin. The method for forming the cyclic olefin-based resin and the second retardation layer is as described in the above section A-3 for the first retardation layer.
- the barrier layer 30 has a barrier property against moisture and gas (for example, oxygen).
- a water vapor transmission rate of at 90% RH conditions is preferably not more than 0.2g / m 2 / 24hr, more preferably be less 0.1g / m 2 / 24hr , more preferably not more than 0.05g / m 2 / 24hr.
- the lower limit of the moisture permeability for example, a 0.001g / m 2 / 24hr, preferably 0.005g / m 2 / 24hr. 60 ° C.
- the gas barrier layer the gas barrier properties 90% RH conditions, and preferably 1.0 ⁇ 10 -7 g / m 2 /24hr ⁇ 0.5g/m 2 / 24hr, more preferably 1.0 ⁇ a 10 -7 g / m 2 /24hr ⁇ 0.1g/m 2 / 24hr.
- the gas barrier layer preferably has a total light transmittance of 70% or more, more preferably 75% or more, and further preferably 80% or more from the viewpoint of optical properties.
- the barrier layer 30 includes a laminated structure of an inorganic thin film and an anchor coat layer.
- the barrier layer 30 can be formed on the retardation layer such that the inorganic thin film is on the organic EL panel side (the side far from the polarizer).
- the inorganic thin film may be formed directly on the retardation layer.
- the inorganic thin film is formed of any appropriate inorganic compound.
- the inorganic thin film preferably contains at least one inorganic compound selected from the group consisting of oxides, nitrides, hydrides and complex compounds thereof.
- the inorganic compound may be a complex compound of oxide, nitride and / or hydride as well as an oxide, nitride or hydride alone. By using such a compound, the transparency can be further improved.
- the inorganic compound that forms the inorganic thin film may have any suitable structure. Specifically, it may have a complete crystal structure or an amorphous structure.
- the elements constituting the inorganic compound include carbon (C), silicon (Si), aluminum (Al), magnesium (Mg), calcium (Ca), potassium (K), zinc (Zn), tin (Sn), Nickel (Ni), sodium (Na), boron (B), titanium (Ti), lead (Pb), zirconium (Zr), yttrium (Y), hydrocarbons, and their oxides, carbides, nitrides and A mixture thereof may be mentioned. These may be used alone or in combination of two or more. Among these, carbon, silicon, and aluminum are preferably used.
- the inorganic compound examples include diamond-like carbon (DLC), silicon nitride (SiNx), silicon oxide (SiOy), aluminum oxide (AlOz), aluminum nitride, and the like.
- the value x of SiNx is preferably 0.3-2.
- the y value of SiOy is preferably 1.3 to 2.5.
- the value of z of AlOz is preferably 0.7 to 2.3.
- Particularly preferred are silicon oxide and aluminum oxide. This is because high gas barrier properties can be stably maintained.
- the inorganic thin film may be formed of a single layer or a multi-layer laminate.
- the inorganic thin film is a laminate include a three-layer structure of inorganic oxide layer / inorganic nitride layer / inorganic oxide layer (for example, SiOy layer / SiNx layer / SiOy layer).
- Arbitrary appropriate methods can be employ
- Specific examples include a vapor deposition method and a coating method.
- the vapor deposition method is preferable in that a uniform thin film having a high barrier property can be obtained.
- the vapor deposition method includes PVD (physical vapor deposition method) such as vacuum vapor deposition, ion plating and sputtering, and CVD (chemical vapor deposition method).
- the thickness of the inorganic thin film is preferably 0.1 nm to 5000 nm, more preferably 0.5 nm to 1000 nm, still more preferably 10 nm to 1000 nm, particularly preferably 30 nm to 500 nm, and particularly preferably 50 nm to 200 nm. If it is such a range, it will have sufficient barrier property, a crack and peeling will not generate
- any appropriate material can be adopted as a material for forming the anchor coat layer.
- Such materials include resins, hydrocarbons, metals, metal oxides and metal nitrides.
- the anchor coat layer is formed of, for example, a resin composition.
- the resin used in the resin composition may be solvent-based or water-based.
- the resin may be a thermoplastic resin, a thermosetting resin, or a photocurable resin.
- Specific examples of the resin include polyester resin, urethane resin, acrylic resin, nitrocellulose resin, silicon resin, alcoholic hydroxyl group-containing resin (vinyl alcohol resin, ethylene vinyl alcohol resin, etc.), vinyl modified Examples include resins, isocyanate group-containing resins, carbodiimide resins, alkoxyl group-containing resins, epoxy resins, oxazoline group-containing resins, modified styrene resins, modified silicon resins, and alkyl titanates.
- the resin composition includes a thermosetting resin or a photocurable resin.
- the thermosetting resin include resins that can be cured by applying thermal energy and that can form a transparent and flat surface after curing.
- Representative examples include polycarbonate, polymethyl methacrylate, polyacrylate, methyl phthalate homopolymer or copolymer, polyethylene terephthalate, polystyrene, diethylene glycol bisallyl carbonate, acrylonitrile / styrene copolymer, poly (-4-methylpentene-1 ), Phenol resin, epoxy resin, cyanate resin, maleimide resin, polyimide resin, etc., and those modified with polyvinyl butyral, acrylonitrile-butadiene rubber, polyfunctional acrylate compound, etc., crosslinked polyethylene resin, Modified with thermoplastic resin such as crosslinked polyethylene / epoxy resin, crosslinked polyethylene / cyanate resin, polyphenylene ether / epoxy resin, polyphenylene ether / /
- the photocurable resin examples include a resin composition composed of an acrylate compound having a radical reactive unsaturated compound, a resin composition composed of a mercapto compound having an acrylate compound and a thiol group, epoxy acrylate, urethane acrylate, polyester acrylate, poly Examples thereof include a resin composition obtained by dissolving an oligomer such as ether acrylate in a polyfunctional acrylate monomer. These may be used alone or in combination of two or more.
- the resin composition includes a polyester resin, a urethane resin, an acrylic resin, an isocyanate group-containing resin, an oxazoline group-containing resin, a carbodiimide resin, an alcoholic hydroxyl group-containing resin, and a gas barrier property. It contains at least one resin selected from the group consisting of copolymers of these resins. Polyester resins are preferred.
- the polyester resin can be obtained by reacting a polyvalent carboxylic acid component and a polyhydric alcohol component.
- the polyvalent carboxylic acid component include terephthalic acid, isophthalic acid, adipic acid, sebacic acid, azelaic acid, orthophthalic acid, diphenylcarboxylic acid, and dimethylphthalic acid.
- the polyhydric alcohol component include ethylene glycol, 1, Examples include 2-propylene glycol, 1,3-propylene glycol, 1,4-butanediol, diethylene glycol, neopentyl glycol, dipropylene glycol, 1,6-hexanediol, bisphenol A, and the like.
- the molecular weight of the resin constituting the anchor coat layer is preferably a number average molecular weight of 3,000 to 30,000, more preferably 4,000 to 28,000, and still more preferably 5, from the viewpoints of gas barrier properties and adhesion. 000 to 25,000.
- silane coupling agent it is preferable to add a silane coupling agent to the resin composition forming the anchor coat layer from the viewpoint of improving the adhesion between the layers.
- silane coupling agent include epoxy group-containing silanes such as ⁇ - (3,4-epoxycyclohexyl) ethyltrimethoxysilane, ⁇ -glycidoxypropylmethyldiethoxylane, and ⁇ -glycidoxypropyltrimethoxysilane.
- Coupling agent ⁇ -aminopropyltrimethoxysilane, N- ⁇ (aminoethyl) ⁇ -aminopropylmethyljetoxylan, N- ⁇ (aminoethyl) ⁇ -aminopropyltrimethoxylane, N- ⁇ (aminoethyl) ⁇ -Amino group-containing silane coupling agents such as aminopropyltriethoxylane, and mixtures thereof.
- preferred silane coupling agents include ⁇ -glycidoxypropyltrimethoxysilane and ⁇ -aminopropyltrimethoxysilane. These silane coupling agents may be used alone or in combination of two or more.
- the silane coupling agent is preferably added at a ratio of 0.1 to 80% by mass, and more preferably 1 to 50% by mass with respect to the resin forming the anchor coat layer.
- the resin composition forming the anchor coat layer preferably contains a curing agent, and it is preferable to use polyisocyanate as the curing agent.
- polyisocyanate include aliphatic polyisocyanates such as hexamethylene diisocyanate and dicyclohexylmethane diisocyanate, and aromatic polyisocyanates such as xylene diisocyanate, tolylene diisocyanate, diphenylmethane diisocyanate, polymethylene polyphenylene diisocyanate, tolidine diisocyanate, and naphthalene diisocyanate. It is done.
- a bifunctional or higher polyisocyanate is preferable from the viewpoint of improving barrier properties.
- any appropriate additive can be blended in the resin composition forming the anchor coat layer as necessary.
- additives include polyhydric alcohols such as glycerin, ethylene glycol, polyethylene glycol and polypropylene glycol, aqueous epoxy resins, lower alcohols such as methanol, ethanol, normal propanol and isopropanol, ethylene glycol monomethyl ether, propylene glycol monomethyl ether.
- Ethers such as propylene glycol diethyl ether, diethylene glycol monoethyl ether, propylene glycol monoethyl ether, esters such as propylene glycol monoacetate and ethylene glycol monoacetate, antioxidants, weathering stabilizers, UV absorbers, antistatic agents , Pigments, dyes, antibacterial agents, lubricants, inorganic fillers, antiblocking agents, adhesives, plasticizers and the like.
- an appropriate resin or additive may be added for the purpose of improving film formability and preventing pinholes.
- the metal forming the anchor coat layer is preferably chromium, aluminum, silicon, nickel, titanium, tin, iron, molybdenum, or an alloy of two or more of these from the viewpoint of barrier properties and adhesion.
- the said metal oxide and nitride are mentioned preferably from a viewpoint of barrier property and adhesiveness.
- Preferred are chromium, silicon oxide, aluminum oxide, titanium oxide, silicon nitride, aluminum nitride, and titanium nitride, and more preferred are silicon oxide and silicon nitride.
- Examples of the hydrocarbon forming the anchor coat layer include diamond-like carbon.
- the thickness of the anchor coat layer is preferably 0.1 nm to 5000 nm, more preferably 10 nm to 2000 nm, still more preferably 100 nm to 1000 nm, and particularly preferably 300 nm to 600 nm.
- any appropriate method can be adopted as a method for forming the anchor coat layer.
- a coating and immersion are mentioned, for example.
- Specific examples of the coating method include reverse roll coater, gravure coater, rod coater, air doctor coater, spray and brush.
- a uniform anchor coat layer can be formed by subjecting the coating layer or the layer formed by dipping to any suitable drying treatment to evaporate the solvent.
- the drying treatment include heat drying such as hot air drying and hot roll drying, and infrared drying. The heating temperature is, for example, about 80 ° C. to 200 ° C.
- the formed anchor coat layer may be subjected to a crosslinking treatment by irradiation with energy rays.
- examples of the forming method include vapor deposition and coating. Vapor deposition is preferred in that a uniform thin film with high adhesion can be obtained.
- Typical examples of the vapor deposition method include PVD (physical vapor deposition method) such as vacuum vapor deposition, ion plating, and sputtering, and CVD (chemical vapor deposition method).
- any appropriate surface treatment for example, chemical treatment
- Discharge treatment is applied to the anchor coat layer before forming the barrier layer.
- a protective layer may be formed on the surface side (inorganic thin film side, pressure-sensitive adhesive layer side) of the barrier layer.
- the protective layer is typically formed of a resin.
- the resin forming the protective layer may be solvent-borne or water-based. Specific examples include polyester resins, urethane resins, acrylic resins, polyvinyl alcohol resins, ethylene / unsaturated carboxylic acid copolymers, ethylene vinyl alcohol resins, vinyl modified resins, nitrocellulose resins, silicon resins. , Isocyanate resins, epoxy resins, oxazoline group-containing resins, modified styrene resins, modified silicon resins, and alkyl titanates. These may be used alone or in combination.
- inorganic particles may be added to improve barrier properties, abrasion resistance, and slipperiness.
- examples of the inorganic particles include silica sol, alumina sol, particulate inorganic filler, and layered inorganic filler. These may be used alone or in combination.
- the inorganic particles may be added by mixing, or may be added by polymerizing the monomer of the resin in the presence of the inorganic particles.
- the resin forming the protective layer is preferably an aqueous resin from the viewpoint of improving the gas barrier properties of the inorganic thin film, and more preferably a vinyl alcohol resin or an ethylene vinyl alcohol resin.
- a blend of polyvinyl alcohol and an ethylene / unsaturated carboxylic acid copolymer is also suitable.
- the method for forming the protective layer is the same as the method for forming the anchor coat layer using the resin composition described above.
- the thickness of the protective layer is preferably 0.05 ⁇ m to 10 ⁇ m, more preferably 0.1 ⁇ m to 3 ⁇ m.
- the barrier layer 30 may be a single layer or a plurality of layers.
- “one barrier layer” means that the constituent unit layer composed of an anchor coat layer, an inorganic thin film, and a protective layer as necessary is one layer.
- the barrier layer is composed of a plurality of layers, the number of structural unit layers is preferably 1 to 10 layers, and more preferably 1 to 5 layers. In this case, each structural unit layer may be the same or different.
- the adhesive layer 40 has a barrier function as described above. By imparting a barrier function to the pressure-sensitive adhesive layer of the circularly polarizing plate, a circularly polarizing plate having an excellent organic EL panel protective function can be obtained due to a synergistic effect with the barrier layer. Furthermore, compared with the case where a barrier layer is formed on an organic EL panel, an organic EL display device can be produced with excellent production efficiency.
- the pressure-sensitive adhesive having a barrier function include a rubber-based pressure-sensitive adhesive composition having a rubber-based polymer as a base polymer.
- Examples of the rubber polymer include a conjugated diene polymer obtained by polymerizing one kind of conjugated diene compound, a conjugated diene copolymer obtained by polymerizing two or more kinds of conjugated diene compounds, and a conjugated diene.
- Examples thereof include conjugated diene copolymers obtained by copolymerizing a compound and an aromatic vinyl compound, and hydrogenated products thereof.
- the conjugated diene compound is not particularly limited as long as it is a monomer having a polymerizable conjugated diene.
- Specific examples of the conjugated diene compound include 1,3-butadiene, isoprene, 2,3-dimethyl-1,3-butadiene, 1,3-pentadiene, 3-methyl-1,3-pentadiene, and 1,3-heptadiene. 1,3-hexadiene.
- 1,3-butadiene and isoprene are preferable from the viewpoint of industrial availability.
- Conjugated diene compounds may be used alone or in combination.
- the aromatic vinyl compound is not particularly limited as long as it is a monomer having an aromatic vinyl structure copolymerizable with a conjugated diene compound.
- Specific examples of the aromatic vinyl compound include styrene, p-methylstyrene, ⁇ -methylstyrene, vinylethylbenzene, vinylxylene, vinylnaphthalene, diphenylethylene and the like. Among these, styrene is preferable from the viewpoint of industrial availability.
- Aromatic vinyl compounds may be used alone or in combination.
- the diene copolymer may be a random copolymer or a block copolymer. Moreover, compounds other than a conjugated diene compound and an aromatic vinyl compound may be copolymerized to obtain a diene copolymer.
- conjugated diene (co) polymers include butadiene rubber (BR), isoprene rubber (IR), styrene-butadiene copolymer (SBR), butadiene-isoprene-styrene random copolymer, isoprene.
- BR butadiene rubber
- IR isoprene rubber
- SBR styrene-butadiene copolymer
- SIS styrene-isoprene block copolymer
- SEBS styrene-ethylene-butadiene block copolymer
- NBR acrylonitrile-butadiene rubber
- isoprene-styrene copolymers are preferred.
- these hydrogenated materials can also be used suitably.
- rubber polymers include isobutylene (IB), styrene-isobutylene-styrene block copolymer (SIBS), styrene-ethylenepropylene copolymer-styrene block copolymer, etc. Can also be used.
- the rubber-based polymers may be used alone or in combination.
- the rubber-based polymer that can be used in the present invention is preferably 50% by weight or more, more preferably 70% by weight or more, and still more preferably 80% by weight or more of the conjugated diene-based (co) polymer in the whole rubber-based polymer. Especially preferably, it contains 90% by weight or more.
- the upper limit of the content of the conjugated diene (co) polymer is not particularly limited, and may be 100% by weight (that is, a rubber polymer composed only of the conjugated diene (co) polymer).
- the pressure-sensitive adhesive composition contains a rubber-based polymer as a base polymer.
- the content of the rubber-based polymer in the pressure-sensitive adhesive composition is preferably 40% by weight or more, more preferably 50% by weight or more, and further preferably 60% by weight or more.
- the upper limit of content of a rubber-type polymer is not specifically limited, For example, it is 90 weight% or less.
- the pressure-sensitive adhesive composition may further contain any appropriate additive in addition to the rubber-based polymer.
- additives include cross-linking agents (for example, polyisocyanates, epoxy compounds, alkyl etherified melamine compounds), tackifiers (for example, rosin derivative resins, polyterpene resins, petroleum resins, oil-soluble phenol resins, vinyltoluenes). Resin), plasticizers, fillers (eg, layered silicates, clay materials, etc.), and anti-aging agents.
- the kind, combination, addition amount, and the like of the additive added to the pressure-sensitive adhesive composition can be appropriately set according to the purpose.
- the content (total amount) of the additive in the pressure-sensitive adhesive composition is preferably 60% by weight or less, more preferably 50% by weight or less, and still more preferably 40% by weight or less.
- the thickness of the pressure-sensitive adhesive layer 40 is, for example, about 1 ⁇ m to 300 ⁇ m, preferably 1 ⁇ m to 200 ⁇ m, more preferably 2 ⁇ m to 100 ⁇ m, and further preferably 25 ⁇ m to 100 ⁇ m.
- the pressure-sensitive adhesive layer 40 has a barrier property as described above, and typically has a barrier property against moisture and gas (for example, oxygen).
- a water vapor transmission rate of at 90% RH conditions is preferably not more than 200g / m 2 / 24hr, more preferably be less 150g / m 2 / 24hr , more preferably less 100g / m 2 / 24hr, most preferably not more than 70g / m 2 / 24hr.
- the lower limit of the moisture permeability for example, 5g / m 2 / 24hr, and preferably from 15g / m 2 / 24hr.
- the moisture permeability of the pressure-sensitive adhesive layer is in such a range, when the circularly polarizing plate is bonded to the organic EL panel due to a synergistic effect with the barrier property of the barrier layer, the organic EL panel is in the air. Good protection from moisture and oxygen.
- a release film is bonded to the surface of the pressure-sensitive adhesive layer until it is used.
- the protective film 50 is formed of any appropriate film that can be used as a protective layer of a polarizer.
- the material as the main component of the film include cellulose resins such as triacetyl cellulose (TAC), polyester-based, polyvinyl alcohol-based, polycarbonate-based, polyamide-based, polyimide-based, polyethersulfone-based, and polysulfone-based materials.
- transparent resins such as polystyrene, polynorbornene, polyolefin, (meth) acryl, and acetate.
- thermosetting resins such as (meth) acrylic, urethane-based, (meth) acrylurethane-based, epoxy-based, and silicone-based or ultraviolet curable resins are also included.
- a glassy polymer such as a siloxane polymer is also included.
- a polymer film described in JP-A-2001-343529 (WO01 / 37007) can also be used.
- a resin composition containing a thermoplastic resin having a substituted or unsubstituted imide group in the side chain and a thermoplastic resin having a substituted or unsubstituted phenyl group and nitrile group in the side chain for example, a resin composition having an alternating copolymer of isobutene and N-methylmaleimide and an acrylonitrile / styrene copolymer can be mentioned.
- the polymer film can be, for example, an extruded product of the resin composition.
- Tg glass transition temperature
- Tg glass transition temperature
- the upper limit of Tg of the said (meth) acrylic-type resin is not specifically limited, From viewpoints of a moldability etc., Preferably it is 170 degrees C or less.
- poly (meth) acrylate such as polymethyl methacrylate, methyl methacrylate- (meth) acrylic acid copolymer, methyl methacrylate- (meth) acrylic acid ester copolymer, methyl methacrylate-acrylic acid ester -(Meth) acrylic acid copolymer, (meth) acrylic acid methyl-styrene copolymer (MS resin, etc.), polymer having alicyclic hydrocarbon group (for example, methyl methacrylate-cyclohexyl methacrylate copolymer) And methyl methacrylate- (meth) acrylate norbornyl copolymer).
- poly (meth) acrylate such as polymethyl methacrylate, methyl methacrylate- (meth) acrylic acid copolymer, methyl methacrylate- (meth) acrylic acid ester copolymer, methyl methacrylate-acrylic acid ester -(Meth) acrylic acid copolymer, (meth) acrylic acid
- poly (meth) acrylate C 1-6 alkyl such as poly (meth) acrylate methyl is used. More preferred is a methyl methacrylate resin containing methyl methacrylate as a main component (50 to 100% by weight, preferably 70 to 100% by weight).
- the (meth) acrylic resin examples include (meth) acrylic resins having a ring structure in the molecule described in, for example, Acrypet VH and Acrypet VRL20A manufactured by Mitsubishi Rayon Co., Ltd., and JP-A-2004-70296.
- the resin examples include high Tg (meth) acrylic resins obtained by intramolecular crosslinking or intramolecular cyclization reaction.
- a (meth) acrylic resin having a lactone ring structure is particularly preferable in that it has high heat resistance, high transparency, and high mechanical strength.
- Examples of the (meth) acrylic resin having the lactone ring structure include JP 2000-230016, JP 2001-151814, JP 2002-120326, JP 2002-254544, and JP 2005. Examples thereof include (meth) acrylic resins having a lactone ring structure described in JP-A-146084.
- the (meth) acrylic resin having a lactone ring structure has a mass average molecular weight (sometimes referred to as a weight average molecular weight), preferably 1,000 to 2,000,000, more preferably 5,000 to 1,000,000, still more preferably 10,000 to 500,000. Preferably it is 50,000 to 500,000.
- the (meth) acrylic resin having a lactone ring structure has a Tg (glass transition temperature) of preferably 115 ° C. or higher, more preferably 125 ° C. or higher, still more preferably 130 ° C. or higher, particularly preferably 135 ° C., most preferably. Is 140 ° C. or higher. It is because it can be excellent in durability.
- the upper limit of Tg of the (meth) acrylic resin having the lactone ring structure is not particularly limited, but is preferably 170 ° C. or less from the viewpoint of moldability and the like.
- (meth) acrylic refers to acrylic and / or methacrylic.
- the protective film 40 may be subjected to a surface treatment such as a hard coat treatment, an antireflection treatment, an antisticking treatment, and an antiglare treatment as necessary.
- the thickness of the protective film is typically 5 mm or less, preferably 1 mm or less, more preferably 1 ⁇ m to 500 ⁇ m, and still more preferably 5 ⁇ m to 150 ⁇ m.
- the inner protective film is preferably optically isotropic.
- “optically isotropic” means that the in-plane retardation Re (550) is 0 nm to 10 nm and the thickness direction retardation Rth (550) is ⁇ 10 nm to +10 nm.
- Re (550) of the inner protective film is preferably 0 nm to 8 nm, more preferably 0 nm to 6 nm, and further preferably 0 nm to 3 nm.
- Rth (550) of the inner protective film is preferably ⁇ 8 nm to +8 nm, more preferably ⁇ 6 nm to +6 nm, and further preferably ⁇ 3 nm to +3 nm. If the inner protective film is optically isotropic, the viewing angle of the display device can be further expanded and the color shift can be further reduced.
- a retardation film constituting the retardation layer 20 is prepared.
- the retardation film is long and has a slow axis in a direction at a predetermined angle with respect to the long direction.
- the material, characteristics, manufacturing method, and the like of such a retardation film are as described in the above section A-3.
- a reinforcing film is bonded to one surface of the retardation film by a roll-to-roll through an adhesive to obtain a retardation film / reinforcing film laminate.
- a reinforcing film provided with an adhesive and a retardation film are bonded together by roll-to-roll.
- the reinforcing film may be composed of one kind of material or may be composed of two or more kinds of materials. For example, you may be comprised from 2 or more types of plastics.
- plastic examples include polyester resins, polyamide resins, and polyolefin resins.
- polyester resin examples include polyethylene terephthalate, polybutylene terephthalate, and polyethylene naphthalate.
- polyolefin resin examples include olefin monomer homopolymers, olefin monomer copolymers, and the like. Specific examples of polyolefin resins include homopolypropylene; block-type, random-type, and graft-type propylene copolymers having an ethylene component as a copolymer component; reactor TPO; low density, high density, linear Low density, ultra-low density, etc.
- ethylene polymers ethylene / propylene copolymer, ethylene / vinyl acetate copolymer, ethylene / methyl acrylate copolymer, ethylene / ethyl acrylate copolymer, ethylene / acrylic acid And ethylene copolymers such as butyl copolymer, ethylene / methacrylic acid copolymer, and ethylene / methyl methacrylate copolymer.
- Polyester resins are preferred, and polyethylene terephthalate is more preferred.
- Such a resin has an advantage that it has high dimensional stability, toughness, and heat resistance, and is excellent in versatility from the viewpoint of becoming a secondary material.
- the reinforcing film may contain any appropriate additive as required.
- the additive include an antioxidant, an ultraviolet absorber, a light stabilizer, an antistatic agent, a filler, and a pigment.
- the kind, number, and amount of the additive can be appropriately set depending on the purpose.
- the material of the reinforcing film is plastic, it is preferable to contain a plurality of the above additives for the purpose of preventing deterioration and the like.
- any appropriate antioxidant can be adopted as the antioxidant.
- antioxidants include phenol-based antioxidants, phosphorus-based processing heat stabilizers, lactone-based processing heat stabilizers, sulfur-based heat-resistant stabilizers, phenol-phosphorus-based antioxidants, and the like.
- the content of the antioxidant is preferably 1 part by weight or less, more preferably 100 parts by weight or less, more preferably 100 parts by weight of the base resin of the reinforcing film (when the reinforcing film is a blend, the blend is the base resin). Is 0.5 parts by weight or less, more preferably 0.01 to 0.2 parts by weight.
- any appropriate UV absorber can be adopted as the UV absorber.
- UV absorbers include benzotriazole UV absorbers, triazine UV absorbers, and benzophenone UV absorbers.
- the content of the ultraviolet absorber is preferably 2 parts by weight or less, more preferably 1 part by weight or less, and still more preferably 0.01 to 0.5 parts by weight with respect to 100 parts by weight of the base resin of the reinforcing film. Part.
- any appropriate light stabilizer can be adopted as the light stabilizer.
- Examples of such light stabilizers include hindered amine light stabilizers and benzoate light stabilizers.
- the content of the light stabilizer is preferably 2 parts by weight or less, more preferably 1 part by weight or less, further preferably 0.01 to 0.5 parts by weight with respect to 100 parts by weight of the base resin of the reinforcing film. Part.
- any suitable filler can be adopted as the filler.
- suitable fillers include inorganic fillers.
- Specific examples of the inorganic filler include carbon black, titanium oxide, and zinc oxide.
- the content of the filler is preferably 20 parts by weight or less with respect to 100 parts by weight of the base resin that forms the reinforcing film (when the reinforcing film is a blend, the blend is the base resin).
- the amount is preferably 10 parts by weight or less, and more preferably 0.01 to 10 parts by weight.
- inorganic, low molecular weight and high molecular weight antistatic agents such as surfactants, inorganic salts, polyhydric alcohols, metal compounds, carbon and the like are also preferred.
- a high molecular weight antistatic agent and carbon are preferable from the viewpoint of contamination and adhesiveness maintenance.
- the thickness of the reinforcing film is preferably 5 to 300 ⁇ m, more preferably 10 to 250 ⁇ m, still more preferably 15 to 200 ⁇ m, and particularly preferably 20 to 150 ⁇ m. Furthermore, the total thickness of the reinforcing film and the pressure-sensitive adhesive described later is preferably 1 to 4 times the thickness of the retardation film.
- the reinforcing film may be a single layer or a laminate of two or more layers.
- the reinforcing film has a product (GPa ⁇ ⁇ m) of a tensile elastic modulus (GPa) and a thickness ( ⁇ m) at 23 ° C. of preferably 20 to 500, more preferably 30 to 300.
- This value can be controlled by adjusting the forming material of the reinforcing film, the type and amount of the additive, and the ratio of the thicknesses of the respective layers when the reinforcing film is a laminate.
- the product is less than 20 (GPa ⁇ ⁇ m)
- the reinforcing film is insufficiently stiff, and there is a case where wrinkles are formed during lamination with the retardation film and the appearance is impaired.
- the said product exceeds 500 (GPa * micrometer), the waist of a reinforcement film is too strong and the handleability at the time of peeling from a retardation film may become inadequate.
- the linear expansion coefficient of the reinforcing film is preferably as small as possible.
- the linear expansion coefficient is preferably 5 ppm / ° C. to 50 ppm / ° C., more preferably 10 ppm / ° C. to 30 ppm / ° C.
- the rate of dimensional change due to heating of the reinforcing film is also preferably as small as possible.
- the dimensional change after heating at 180 ° C. for 5 minutes is preferably 0.1% to 5.0%, more preferably 0.5% to 3.0%.
- the dimensional change of the retardation film can be suppressed even in a high-temperature environment during the barrier layer formation process, and the molecular orientation change can be reduced. can do.
- the optical properties (such as the slow axis direction and the retardation value) of the retardation film can be maintained well.
- the reinforcing film is stretched in one embodiment.
- the stretching conditions can vary depending on the purpose, desired linear expansion coefficient, and the like.
- the draw ratio is preferably 1.5 to 10 times, more preferably 3.0 to 5.0 times.
- the stretching temperature is preferably the glass transition temperature (Tg) to (Tg + 50 ° C.) of the reinforcing film.
- Stretching is preferably biaxial stretching. This is because the in-plane anisotropy of thermal properties and mechanical properties can be reduced.
- the biaxial stretching method either a tenter simultaneous biaxial stretching method or a sequential biaxial stretching method using a roll and a tenter may be used. Further, a tubular method may be used.
- the retardation film / reinforcing film laminate is subjected to a vapor deposition method (for example, sputtering) for forming a barrier layer by using the retardation film as described in the section A-3 and the reinforcing film as described above.
- a vapor deposition method for example, sputtering
- the retardation film obtained by oblique stretching tends to have a large variation in orientation (slow axis direction) and is oriented by thermal and / or mechanical stimulation.
- the variation in the slow axis direction is further increased.
- the film may crack or deform.
- the optical and mechanical properties of the retardation film are maintained within an allowable range even when subjected to a high temperature environment such as vapor deposition. can do. Therefore, a barrier layer can be formed on the surface while maintaining the properties of the retardation film obtained by oblique stretching. As a result, the retardation film in which the barrier layer is formed can be used for roll-to-roll.
- any appropriate pressure-sensitive adhesive can be used as the pressure-sensitive adhesive for reinforcing film.
- the base polymer of the pressure-sensitive adhesive include (meth) acrylic polymers, rubber polymers, silicone polymers, polyurethane polymers, and polyester polymers.
- the pressure-sensitive adhesive preferably contains a (meth) acrylic polymer having a (meth) acrylic acid alkyl ester having an alkyl group having 1 to 20 carbon atoms as a main component (monomer unit).
- the “main component” means a monomer having the highest constituent ratio among the monomer units (components) constituting the (meth) acrylic polymer. Details of such an adhesive are described in, for example, Japanese Patent Application Laid-Open No. 2014-141649, and the corresponding description is incorporated herein by reference.
- a barrier layer is formed on the surface of the retardation film of the retardation film / reinforcing film laminate. More specifically, an anchor coat layer is formed on the surface of the retardation film, an inorganic thin film is formed on the surface of the anchor coat layer, and a protective layer is formed on the surface of the inorganic thin film as necessary.
- the materials, formation methods, etc. of the anchor coat layer, inorganic thin film and protective layer are as described in the above section A-5.
- the inorganic thin film is formed, and / or after the protective layer is formed, heat treatment may be performed.
- heat treatment By performing the heat treatment, the barrier properties and film quality of the obtained barrier layer can be stabilized, and bubbles can be finely dispersed in the obtained barrier layer, and adverse effects due to the bubbles can be prevented. .
- Any appropriate method can be adopted as a heating method in the heat treatment. Specific examples include a method of storing in an oven or temperature-controlled room set to a predetermined temperature, a method of blowing hot air, a method of heating with an infrared heater, a method of irradiating light with a lamp, and direct contact with a hot roll or hot plate.
- a heating device can be incorporated in a part of a film production apparatus such as a coater or slitter, and heat treatment can be carried out during the production process.
- the temperature of the heat treatment is typically a temperature below the melting point of the retardation film, and preferably a temperature that does not adversely affect the optical properties and mechanical properties of the retardation film.
- the temperature of the heat treatment is preferably 60 ° C. or higher, more preferably 70 ° C. or higher, because a treatment time necessary for the effect of the heat treatment to be manifested can be set appropriately.
- the upper limit of the heat treatment temperature is, for example, 200 ° C., preferably 160 ° C., from the viewpoint of preventing a decrease in barrier properties.
- the heat treatment time can depend on the heat treatment temperature. For example, when the heat treatment temperature is 150 ° C., the heat treatment time can be about 3 to 60 minutes.
- an optical laminate (intermediate body for circularly polarizing plate) having a configuration of barrier layer / retardation film / reinforcing film is produced.
- the optical layered body in the present embodiment has a long shape (roll shape in the description example).
- a specific retardation film and a specific reinforcing film are used in combination to form a barrier layer on the surface while maintaining the optical and mechanical properties of the retardation film obtained by oblique stretching. can do. Therefore, the retardation film in which the barrier layer is formed can be used for roll-to-roll. That is, the optical layered body thus obtained is one of the results actually obtained in the present invention, and is one of means for realizing the circularly polarizing plate of the present invention and its excellent effects. is there.
- the reinforcing film is peeled from the optical laminate, and a polarizer is bonded to the peeled surface by roll-to-roll.
- the barrier layer / retardation film laminate obtained by peeling the reinforcing film and the polarizing plate are adjacent to the retardation film. In this way, they are bonded together by roll-to-roll.
- the barrier layer / retardation film laminate, the polarizer, and the protective film are bonded together by roll-to-roll.
- the barrier layer / retardation film laminate and the polarizer are bonded together by roll-to-roll, and then the protective film is bonded by roll-to-roll.
- the polarizing plate or the polarizer has a long shape (roll shape in the description example) and has an absorption axis in the long direction.
- a barrier layer can be formed on a retardation film having a slow axis in an oblique direction (a direction at a predetermined angle with respect to the longitudinal direction). Lamination by roll-to-roll can be performed using a polarizer obtained by uniaxial stretching.
- the pressure-sensitive adhesive constituting the pressure-sensitive adhesive layer is as described in the above section A-6.
- the circularly polarizing plate of the present invention is obtained.
- the retardation layer 20 As a typical example of a method for manufacturing a circularly polarizing plate by roll-to-roll, the case where the retardation layer 20 is used alone has been described. However, the first retardation layer 20 and the second retardation layer 60 are used in combination. It will be apparent to those skilled in the art that a similar procedure applies to. Specifically, instead of the retardation film constituting the retardation layer 20, a laminate of the retardation film constituting the first retardation layer 20 and the retardation film constituting the second retardation layer 60. May be used.
- the circularly polarizing plate of the present invention may be manufactured by a so-called batch method. That is, the retardation film on which the barrier layer is formed and the polarizing plate (polarizer / protective film laminate) may be cut into a predetermined size and bonded together. Alternatively, the retardation film, the polarizer, and the protective film on which the barrier layer is formed may be cut into a predetermined size and bonded together. If it is a batch type, it is not necessary to control the angle between the absorption axis of the polarizer and the slow axis of the retardation film in the roll state, so that a retardation film obtained by longitudinal stretching or transverse stretching can be used. .
- the organic EL display device of the present invention includes the circularly polarizing plate described in the above section A on the viewing side.
- the circularly polarizing plate is laminated so that the pressure-sensitive adhesive layer is on the organic EL panel side (so that the polarizer is on the viewing side).
- the present invention will be specifically described by way of examples, but the present invention is not limited to these examples.
- the measuring method of each characteristic is as follows.
- Example 1 After a commercially available polyvinyl alcohol (PVA) film (“VF-PS” manufactured by Kuraray Co., Ltd.) is dyed in an aqueous solution containing iodine, it is uniaxially about 6 times between rolls having different speed ratios in an aqueous solution containing boric acid. Stretched to obtain a long polarizer (thickness 30 ⁇ m). The ratio K / I of iodine concentration (% by weight) and potassium concentration (% by weight) in the polarizer was 0.402.
- PVA polyvinyl alcohol
- TAC film (“TD80UL” manufactured by Fuji Photo Film Co., Ltd., thickness 80 ⁇ m) as a protective film is bonded to one side of this polarizer using a PVA adhesive, and a polarizer having a polarizer / protective film configuration Got.
- This polarizing plate was punched into a length of 20 cm ⁇ width of 30 cm. At this time, the absorption axis of the polarizer was set in the vertical direction.
- Re (550) 140 nm retardation film (thickness 35 ⁇ m) by stretching a commercially available long norbornene resin film (“ZEONOR” manufactured by Nippon Zeon Co., Ltd., thickness 50 ⁇ m) by 1.52 times.
- ZEONOR commercially available long norbornene resin film
- a barrier layer (thickness: 150 nm) was formed on the retardation film to obtain a barrier layer / retardation layer laminate.
- a SiOx film was formed by a sputtering method using a SiO target.
- Moisture permeability of the barrier layer was 0.05g / m 2 / 24hr.
- the polarizing plate and the barrier layer / retardation layer laminate obtained above were bonded together via an acrylic pressure-sensitive adhesive so that the polarizer and the retardation layer were adjacent to each other. At this time, the slow axis of the retardation layer was set to 45 ° counterclockwise with respect to the absorption axis of the polarizer.
- a pressure-sensitive adhesive layer (thickness 50 ⁇ m) having a barrier function is formed on the surface of the barrier layer, and a circle having a configuration of protective film / polarizer / retardation layer ( ⁇ / 4 plate) / barrier layer / pressure-sensitive adhesive layer A polarizing plate was obtained.
- the pressure-sensitive adhesive constituting the pressure-sensitive adhesive layer is a polybutene with respect to 100 parts by weight of a styrene / ethylene propylene copolymer / styrene block copolymer (Kuraray Co., Ltd., trade name “Septon 2063”, styrene content: 13% by weight).
- ZEONOR manufactured by ZEON Corporation, thickness 75 ⁇ m
- a circularly polarizing plate having the structure of layer / adhesive layer was obtained. The obtained circularly polarizing plate was subjected to the evaluations (1) and (2) above. The results are shown in Table 1.
- Example 3 Protective film / polarizer / second retardation layer ( ⁇ / 2 plate) / first retardation layer in the same manner as in Example 2 except that a polarizer having K / I of 0.210 was used.
- the circularly polarizing plates of the examples of the present invention have very excellent barrier properties (moisture permeability). Further, as is clear from comparison between Example 2 and Example 3, a polarizing plate satisfying both excellent moisture permeability and heat resistance by adjusting K / I and improving the heat resistance of the polarizer can be obtained. can get.
- the circularly polarizing plate of the present invention is suitably used for an organic EL display device.
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Abstract
Description
1つの実施形態においては、上記円偏光板は、上記偏光子と上記位相差層との間に、λ/2板として機能する別の位相差層をさらに備え、該偏光子の吸収軸と該位相差層の遅相軸とのなす角度が65°~85°であり、該偏光子の吸収軸と該別の位相差層の遅相軸とのなす角度が10°~20°である。
1つの実施形態においては、上記円偏光板は、上記偏光子と上記位相差層との間に保護フィルムをさらに備える。
1つの実施形態においては、上記円偏光板は、上記偏光子と上記別の位相差層との間に保護フィルムをさらに備える。
1つの実施形態においては、上記円偏光板は、上記偏光子の上記位相差層と反対側に保護フィルムをさらに備える。
1つの実施形態においては、上記偏光子は長尺状であり、かつ、長尺方向に上記吸収軸を有し;上記位相差層は長尺状であり、かつ、長尺方向に対して35°~55°の方向に上記遅相軸を有する。
1つの実施形態においては、上記偏光子は長尺状であり、かつ、長尺方向に上記吸収軸を有し;上記位相差層および上記別の位相差層は長尺状であり、かつ、該位相差層は長尺方向に対して65°~85°の方向に上記遅相軸を有し、該別の位相差層は長尺方向に対して10°~20°の方向に上記遅相軸を有する。
1つの実施形態においては、上記偏光子におけるヨウ素含有量(重量%)に対するカリウム含有量(重量%)の比K/Iは0.180~0.235である。
本発明の別の局面によれば、有機EL表示装置が提供される。この有機表示装置は、上記の円偏光板を備える。
本明細書における用語および記号の定義は下記の通りである。
(1)屈折率(nx、ny、nz)
「nx」は面内の屈折率が最大になる方向(すなわち、遅相軸方向)の屈折率であり、「ny」は面内で遅相軸と直交する方向(すなわち、進相軸方向)の屈折率であり、「nz」は厚み方向の屈折率である。
(2)面内位相差(Re)
「Re(λ)」は、23℃における波長λnmの光で測定した面内位相差である。例えば、「Re(550)」は、23℃における波長550nmの光で測定した面内位相差である。Re(λ)は、層(フィルム)の厚みをd(nm)としたとき、式:Re=(nx-ny)×dによって求められる。
(3)厚み方向の位相差(Rth)
「Rth(λ)」は、23℃における波長λnmの光で測定した厚み方向の位相差である。例えば、「Rth(550)」は、23℃における波長550nmの光で測定した厚み方向の位相差である。Rth(λ)は、層(フィルム)の厚みをd(nm)としたとき、式:Rth=(nx-nz)×dによって求められる。
(4)Nz係数
Nz係数は、Nz=Rth/Reによって求められる。
A-1.円偏光板の全体構成
本発明の実施形態による円偏光板は、有機EL表示装置に用いられる。本発明の1つの実施形態による円偏光板は、偏光子と、λ/4板として機能する位相差層と、バリア層と、バリア機能を有する粘着剤層と、をこの順に備える。本発明の別の実施形態による円偏光板は、偏光子と位相差層との間にλ/2板として機能する別の位相差層をさらに備える。以下、これらの代表的な実施形態について円偏光板の全体的な構成を具体的に説明し、その後で、円偏光板を構成する各層および光学フィルムを詳細に説明する。
偏光子10としては、任意の適切な偏光子が採用され得る。具体例としては、ポリビニルアルコール系フィルム、部分ホルマール化ポリビニルアルコール系フィルム、エチレン・酢酸ビニル共重合体系部分ケン化フィルム等の親水性高分子フィルムに、ヨウ素や二色性染料等の二色性物質による染色処理および延伸処理が施されたもの、ポリビニルアルコールの脱水処理物やポリ塩化ビニルの脱塩酸処理物等ポリエン系配向フィルム等が挙げられる。好ましくは、光学特性に優れることから、ポリビニルアルコール系フィルムをヨウ素で染色し一軸延伸して得られた偏光子が用いられる。
位相差層20は、上記のとおりλ/4板として機能し得る。このような位相差層の面内位相差Re(550)は、100nm~180nmであり、好ましくは110nm~170nmであり、さらに好ましくは120nm~160nmであり、特に好ましくは135nm~155nmである。位相差層20は、代表的にはnx>ny=nzまたはnx>ny>nzの屈折率楕円体を有する。なお、本明細書において例えば「ny=nz」は、厳密に等しいのみならず、実質的に等しいものを包含する。したがって、位相差層のNz係数は、例えば0.9~2であり、好ましくは1~1.5であり、より好ましくは1~1.3である。
構造式(1)で表される結合構造を有するジヒドロキシ化合物をジヒドロキシ化合物(A)、構造式(1)で表される結合構造を有さないジヒドロキシ化合物をジヒドロキシ化合物(B)と略記することがある。
ジヒドロキシ化合物(A)における「連結基-CH2-O-」とは、水素原子以外の原子と互いに結合して分子を構成する構造を意味する。この連結基において、少なくとも酸素原子が結合し得る原子又は炭素原子と酸素原子が同時に結合し得る原子としては、炭素原子が最も好ましい。ジヒドロキシ化合物(A)中の「連結基-CH2-O-」の数は1以上であり、好ましくは2~4である。
4-(2-ヒドロキシエトキシ)-3-フェニルフェニル)フルオレン、9,9-ビス(4-(2-ヒドロキシエトキシ)-3,5-ジメチルフェニル)フルオレン、9,9-ビス(4-(2-ヒドロキシエトキシ)-3-tert-ブチル-6-メチルフェニル)フルオレン、9,9-ビス(4-(3-ヒドロキシ-2,2-ジメチルプロポキシ)フェニル)フルオレン等で例示されるような、側鎖に芳香族基を有し、主鎖に芳香族基に結合したエーテル基を有する化合物、ビス[4-(2-ヒドロキシエトキシ)フェニル]メタン、ビス[4-(2-ヒドロキシエトキシ)フェニル]ジフェニルメタン、1,1-ビス[4-(2-ヒドロキシエトキシ)フェニル]エタン、1,1-ビス[4-(2-ヒドロキシエトキシ)フェニル]-1-フェニルエタン、2,2-ビス[4-(2-ヒドロキシエトキシ)フェニル]プロパン、2,2-ビス[4-(2-ヒドロキシエトキシ)-3-メチルフェニル]プロパン、2,2-ビス[3,5-ジメチル-4-(2-ヒドロキシエトキシ)フェニル]プロパン、1,1-ビス[4-(2-ヒドロキシエトキシ)フェニル]-3,3,5-トリメチルシクロヘキサン、1,1-ビス[4-(2-ヒドロキシエトキシ)フェニル]シクロヘキサン、1,4-ビス[4-(2-ヒドロキシエトキシ)フェニル]シクロヘキサン、1,3-ビス[4-(2-ヒドロキシエトキシ)フェニル]シクロヘキサン、2,2-ビス[4-(2-ヒドロキシエトキシ)-3-フェニルフェニル]プロパン、2,2-ビス[(2-ヒドロキシエトキシ)-3-イソプロピルフェニル]プロパン、2,2-ビス[3-tert-ブチル-4-(2-ヒドロキシエトキシ)フェニル]プロパン、2,2-ビス[4-(2-ヒドロキシエトキシ)フェニル]ブタン、2,2-ビス[4-(2-ヒドロキシエトキシ)フェニル]-4-メチルペンタン、2,2-ビ
ス[4-(2-ヒドロキシエトキシ)フェニル]オクタン、1,1-ビス[4-(2-ヒドロキシエトキシ)フェニル]デカン、2,2-ビス[3-ブロモ-4-(2-ヒドロキシエトキシ)フェニル]プロパン、2,2-ビス[3-シクロヘキシル-4-(2-ヒドロキシエトキシ)フェニル]プロパン等で例示されるような、ビス(ヒドロキシアルコキシアリール)アルカン類、1,1-ビス[4-(2-ヒドロキシエトキシ)フェニル]シクロヘキサン、1,1-ビス[3-シクロヘキシル-4-(2-ヒドロキシエトキシ)フェニル]シクロヘキサン、1,1-ビス[4-(2-ヒドロキシエトキシ)フェニル]シ
クロペンタン等で例示されるような、ビス(ヒドロキシアルコキシアリール)シクロアルカン類、4,4’-ビス(2-ヒドロキシエトキシ)ジフェニルエ-テル、4,4’-ビス(2-ヒドロキシエトキシ)-3,3’-ジメチルジフェニルエ-テル等で例示されるような、ジヒドロキシアルコキシジアリールエーテル類、4,4’-ビス(2-ヒドロキエトキシフェニル)スルフィド、4,4’-ビス[4-(2-ジヒドロキシエトキシ)-3-メチルフェニル]スルフィド等で例示されるような、ビスヒドロキシアルコキシアリールスルフィド類、4,4’-ビス(2-ヒドロキエトキシフェニル)スルホキシド、4,4’-ビス[4-(2-ジヒドロキシエトキシ)-3-メチルフェニル]スルホキシド等で例示されるような、ビスヒドロキシアルコキシアリールスルホキシド類、4,4’-ビス(2-ヒドロキエトキシフェニル)スルホン、4,4’-ビス[4-(2-ジヒドロキシエトキシ)-3-メチルフェニル]スルホン等で例示されるような、ビスヒドロキシアルコキシアリールスルホン類、1,4-ビスヒドロキシエトキシベンゼン、1,3-ビスヒドロキシエトキシベンゼン、1,2-ビスヒドロキシエトキシベンゼン、1,3-ビス[2-[4-(2-ヒドロキシエトキシ)フェニル]プロピル]ベンゼン、1,4-ビス[2-[4-(2-ヒドロキシエトキシ)フェニル]プロピル]ベンゼン、4,4’-ビス(2-ヒドロキシエトキシ)ビフェニル、1,3-ビス[4-(2-ヒドロキシエトキシ)フェニル]-5,7-ジメチルアダマンタン、下記式(4)で表されるジヒドロキシ化合物に代表される無水糖アルコール、および下記一般式(6)で表されるスピログリコール等の環状エーテル構造を有する化合物が挙げられ、これらは単独で用いても良く、2種以上を組み合わせて用いても良い。
高純度のジヒドロキシ化合物(A)、例えば式(4)で表されるジヒドロキシ化合物を炭酸ジエステルとの反応直前まで、好ましくは不活性ガス雰囲気又は減圧ないし真空雰囲気といった、酸素の存在しない雰囲気下に保管する。この保管状態から取り出した後、40℃、80%RHの環境の保管の場合、通常2週間以内に、より好ましくは1週間以内に、炭酸ジエステルとの反応系に供給することが好ましい。40℃、80%RHの環境の保管であれば、通常2週間以内、好ましくは1週間以内の間、上記式(4)で表されるジヒドロキシ化合物を、大気中に放置しておいても重合を阻害することがない。40℃、80
%RHより温度、湿度が低い場合には、保管期間をより長くすることができる。
保管温度は40℃以下なら、脱酸素剤を共存させ、不活性ガス雰囲気下で酸素濃度1000ppm以下の環境を保つと、1ヶ月は重合に供することができる。保管温度は40℃以下、好ましくは、25℃以下、さらに好ましくは、10℃以下、特に好ましくは5℃以下である。
さらに、これら条件は、適宜組合せて用いることができる。
なお、ジヒドロキシ化合物(A)、例えば式(4)で表されるジヒドロキシ化合物を、後述する炭酸ジエステルとの反応に供する場合、その形態は特に限定されず、粉末状、フレーク状であっても、溶融状態や水溶液などの液状であってもよい。
上記ポリカーボネート樹脂においては、ジヒドロキシ化合物としてジヒドロキシ化合物(A)以外のジヒドロキシ化合物である、ジヒドロキシ化合物(B)を用いてもよい。ジヒドロキシ化合物(B)としては、例えば、脂環式ジヒドロキシ化合物、脂肪族ジヒドロキシ化合物、オキシアルキレングリコール類、芳香族ジヒドロキシ化合物、環状エーテル構造を有するジオール類等を、ポリカーボネートの構成単位となるジヒドロキシ化合物として、ジヒドロキシ化合物(A)、例えば式(4)で表されるジヒドロキシ化合物とともに用いることができる。
HOCH2-R1-CH2OH (II)
HO-R2-OH (III)
(式(II)、(III)中、R1、R2はそれぞれ、炭素数4~20のシクロアルキレン基を示す。)
上記一般式(II)で表される脂環式ジヒドロキシ化合物であるシクロヘキサンジメタノールとしては、一般式(II)において、R1が下記一般式(IIa)(式中、R3は炭素数1~12のアルキル基又は水素原子を示す。)で表される種々の異性体を包含する。このようなものとしては、具体的には、1,2-シクロヘキサンジメタノール、1,3-シクロヘキサンジメタノール、1,4-シクロヘキサンジメタノールなどが挙げられる。
使用可能なオキシアルキレングリコール類としては、例えば、ジエチレングリコール、トリエチレングリコール、テトラエチレングリコール、ポリエチレングリコール等が挙げられる。
ニルメタン、ビス(4-ヒドロキシフェニル)メタン、ビス(4-ヒドロキシ-5-ニトロフェニル)メタン、1,1-ビス(4-ヒドロキシフェニル)エタン、3,3-ビス(4-ヒドロキシフェニル)ペンタン、1,1-ビス(4-ヒドロキシフェニル)シクロヘキサン、ビス(4-ヒドロキシフェニル)スルホン、2,4’-ジヒドロキシジフェニルスルホン、ビス(4-ヒドロキシフェニル)スルフィド、4,4’-ジヒドロキシジフェニルエーテル、4,4’-ジヒドロキシ-3,3’-ジクロロジフェニルエーテル、4,4’-ジヒドロキシ-2,5-ジエトキシジフェニルエーテル、9,9-ビス[4-(2
-ヒドロキシエトキシ)フェニル]フルオレン、9,9-ビス[4-(2-ヒドロキシエトキシ-2-メチル)フェニル]フルオレン、9,9-ビス(4-ヒドロキシフェニル)フルオレン、9,9-ビス(4-ヒドロキシ-2-メチルフェニル)フルオレン等が挙げられる。
なお、上記例示化合物は、本発明に使用し得る脂環式ジヒドロキシ化合物、脂肪族ジヒドロキシ化合物、オキシアルキレングリコール類、芳香族ジヒドロキシ化合物、環状エーテル構造を有するジオール類の一例であって、何らこれらに限定されるものではない。これらの化合物は、1種又は2種以上を式(4)で表されるジヒドロキシ化合物とともに用いることができる。
また、ポリカーボネート樹脂は、110℃での単位面積あたりのフェノール成分以外の発生ガス量(以下、単に「発生ガス量」と称す場合がある。)が5ng/cm2以下であることが好ましく、また、式(4)で表されるジヒドロキシ化合物以外のジヒドロキシ化合物由来の発生ガス量は0.5ng/cm2以下であることがより好ましい。
ポリカーボネート樹脂において、上記物性は、少なくとも二つを同時に有するものが好ましく、さらに他の物性を併せもつものがより好ましい。
<炭酸ジエステル>
ポリカーボネート樹脂の製造方法で用いられる炭酸ジエステルとしては、例えば、ジフェニルカーボネート、ジトリルカーボネートに代表される置換ジフェニルカーボネート、ジメチルカーボネート、ジエチルカーボネート及びジ-t-ブチルカーボネート等が例示され、特に好ましくはジフェニルカーボネート及び置換ジフェニルカーボネートが挙げられる。これらの炭酸ジエステルは、1種を単独で用いても良く、2種以上を混合して用いても良い。
別の位相差層(第2の位相差層)60は、上記のとおりλ/2板として機能し得る。このような位相差層の面内位相差Re(550)は、180nm~320nmであり、より好ましくは200nm~290nmであり、さらに好ましくは230nm~280nmである。別の位相差層60は、代表的にはnx>ny=nzまたはnx>ny>nzの屈折率楕円体を有する。別の位相差層のNz係数は、例えば0.9~2であり、好ましくは1~1.5であり、より好ましくは1~1.3である。
バリア層30は、水分およびガス(例えば酸素)に対するバリア性を有する。バリア層の40℃、90%RH条件下での水蒸気透過率(透湿度)は、好ましくは0.2g/m2/24hr以下であり、より好ましくは0.1g/m2/24hr以下であり、さらに好ましくは0.05g/m2/24hr以下である。一方、透湿度の下限は、例えば0.001g/m2/24hrであり、好ましくは0.005g/m2/24hrである。バリア層の60℃、90%RH条件下でのガスバリア性は、好ましくは1.0×10-7g/m2/24hr~0.5g/m2/24hrであり、より好ましくは1.0×10-7g/m2/24hr~0.1g/m2/24hrである。透湿度およびガスバリア性がこのような範囲であれば、円偏光板を有機ELパネルに貼り合わせた場合に、有機ELパネルを空気中の水分および酸素から良好に保護し得る。また、ガスバリア層は、光学特性の点から、全光線透過率が好ましくは70%以上であり、より好ましくは75%以上であり、さらに好ましくは80%以上である。
粘着剤層40は、上記のとおりバリア機能を有する。円偏光板の粘着剤層にバリア機能を付与することにより、バリア層との相乗的な効果により、優れた有機ELパネル保護機能を有する円偏光板を得ることができる。さらに、有機ELパネルにバリア層を形成する場合に比べて、優れた製造効率で有機EL表示装置を作製することができる。バリア機能を有する粘着剤としては、例えば、ゴム系ポリマーをベースポリマーとするゴム系粘着剤組成物が挙げられる。
保護フィルム50は、偏光子の保護層として使用できる任意の適切なフィルムで形成される。当該フィルムの主成分となる材料の具体例としては、トリアセチルセルロース(TAC)等のセルロース系樹脂や、ポリエステル系、ポリビニルアルコール系、ポリカーボネート系、ポリアミド系、ポリイミド系、ポリエーテルスルホン系、ポリスルホン系、ポリスチレン系、ポリノルボルネン系、ポリオレフィン系、(メタ)アクリル系、アセテート系等の透明樹脂等が挙げられる。また、(メタ)アクリル系、ウレタン系、(メタ)アクリルウレタン系、エポキシ系、シリコーン系等の熱硬化型樹脂または紫外線硬化型樹脂等も挙げられる。この他にも、例えば、シロキサン系ポリマー等のガラス質系ポリマーも挙げられる。また、特開2001-343529号公報(WO01/37007)に記載のポリマーフィルムも使用できる。このフィルムの材料としては、例えば、側鎖に置換または非置換のイミド基を有する熱可塑性樹脂と、側鎖に置換または非置換のフェニル基ならびにニトリル基を有する熱可塑性樹脂を含有する樹脂組成物が使用でき、例えば、イソブテンとN-メチルマレイミドからなる交互共重合体と、アクリロニトリル・スチレン共重合体とを有する樹脂組成物が挙げられる。当該ポリマーフィルムは、例えば、上記樹脂組成物の押出成形物であり得る。
以下、本発明の円偏光板の製造方法の代表的な実施形態について説明する。本実施形態は、偏光子と位相差層とをロールトゥロールにより連続的に積層する方式であり、非常に優れた製造効率で円偏光板を製造することができる。
本発明の有機EL表示装置は、その視認側に上記A項に記載の円偏光板を備える。円偏光板は、粘着剤層が有機ELパネル側となるように(偏光子が視認側となるように)積層されている。
実施例および比較例で得られた円偏光板を50mm×50mmサイズに切断し、測定試料とした。この測定試料を石英ガラスに貼りあわせ、95℃のオーブンに500時間保管し、保管前後の色相値の変化量を計測した。色相値は、村上色彩技術研究所製「DOT-3」で測定した。
(2)透湿度
実施例および比較例で得られた円偏光板を10cmΦの円状に切り出し、測定試料とした。この測定試料について、テクノロックス社製「DELTAPERM」を用いて、40℃、90%RHの試験条件で透湿度を測定した。なお、比較例2の円偏光板については測定上限値を超えたため、MOCON社製「PERMTRAN」を用いて、40℃、90%RHの試験条件で透湿度を測定した。
市販のポリビニルアルコール(PVA)フィルム(クラレ社製「VF-PS」)を、ヨウ素を含む水溶液中で染色した後、ホウ酸を含む水溶液中で速比の異なるロール間にて約6倍に一軸延伸して長尺の偏光子(厚さ30μm)を得た。偏光子におけるヨウ素濃度(重量%)とカリウム濃度(重量%)との比K/Iは0.402であった。この偏光子の片面に保護フィルムとして市販のTACフィルム(富士写真フィルム社製「TD80UL」、厚さ80μm)を、PVA系接着剤を用いて貼り合わせ、偏光子/保護フィルムの構成を有する偏光板を得た。この偏光板を縦20cm×横30cmに打ち抜いた。このとき、偏光子の吸収軸が縦方向となるようにした。
一方、市販の長尺状のノルボルネン系樹脂フィルム(日本ゼオン社製「ゼオノア」、厚さ50μm)を1.52倍に延伸することによってRe(550)=140nmの位相差フィルム(厚さ35μm)を得た。この位相差フィルムにバリア層(厚さ150nm)を形成し、バリア層/位相差層の積層体を得た。なお、バリア層として、SiOターゲットを用いたスパッタ法によりSiOx膜を形成した。バリア層の透湿度は、0.05g/m2/24hrであった。
上記で得られた偏光板とバリア層/位相差層の積層体とを、偏光子と位相差層とが隣接するように、アクリル系粘着剤を介して貼り合わせた。このとき、位相差層の遅相軸が偏光子の吸収軸に対して反時計回りで45°となるようにした。
最後に、バリア層表面にバリア機能を有する粘着剤層(厚さ50μm)を形成し、保護フィルム/偏光子/位相差層(λ/4板)/バリア層/粘着剤層の構成を有する円偏光板を得た。なお、粘着剤層を構成する粘着剤としてスチレン・エチレンプロピレン共重合体・スチレンのブロックコポリマー(クラレ社製、商品名「セプトン2063」、スチレン含有量:13重量%)100重量部に対してポリブテン(JX日鉱日石エネルギー社製、「商品名「日石ポリブテンHV-300」」10重量部、テルペンフェノール粘着付与剤(ヤスハラケミカル社製、商品名「YSポリスターTH130」)40重量部、および芳香族粘着付与剤(イーストマンケミカル社製、商品名「ピコラスチックA5」)を配合し作製した粘着剤を用いた。粘着剤層の透湿度は、10g/m2/24hr(50μm換算)であった。得られた円偏光板を上記(1)および(2)の評価に供した。結果を表1に示す。
市販の長尺状のノルボルネン系樹脂フィルム(日本ゼオン社製「ゼオノア」、厚さ75μm)を2.55倍に延伸することによってRe(550)=270nmの位相差フィルム(厚さ45μm)を得た。この位相差フィルム(第2の位相差層)と実施例1で得られた位相差フィルム(第1の位相差層)とを積層し、次いで、実施例1と同様にして第1の位相差層表面にバリア層を形成し、バリア層/第1の位相差層/第2の位相差層の積層体を得た。この積層体を用いたこと以外は実施例1と同様にして、保護フィルム/偏光子/第2の位相差層(λ/2板)/第1の位相差層(λ/4板)/バリア層/粘着剤層の構成を有する円偏光板を得た。得られた円偏光板を上記(1)および(2)の評価に供した。結果を表1に示す。
K/Iが0.210である偏光子を用いたこと以外は実施例2と同様にして、保護フィルム/偏光子/第2の位相差層(λ/2板)/第1の位相差層(λ/4板)/バリア層/粘着剤層の構成を有する円偏光板を得た。得られた円偏光板を上記(1)および(2)の評価に供した。結果を表1に示す。
バリア層を形成しなかったこと、および、通常のアクリル系粘着剤層を形成したこと以外は実施例2と同様にして、保護フィルム/偏光子/第2の位相差層(λ/2板)/第1の位相差層(λ/4板)/粘着剤層の構成を有する円偏光板を得た。得られた円偏光板を上記(1)および(2)の評価に供した。結果を表1に示す。
バリア層を形成しなかったこと以外は実施例2と同様にして、保護フィルム/偏光子/第2の位相差層(λ/2板)/第1の位相差層(λ/4板)/粘着剤層の構成を有する円偏光板を得た。得られた円偏光板を上記(1)および(2)の評価に供した。結果を表1に示す。
20 位相差層
30 バリア層
40 粘着剤層
50 保護フィルム
60 別の位相差層
100 円偏光板
Claims (9)
- 偏光子と、λ/4板として機能する位相差層と、バリア層と、バリア機能を有する粘着剤層と、をこの順に備え、
該偏光子の吸収軸と該位相差層の遅相軸とのなす角度が35°~55°である、
有機EL表示装置用円偏光板。 - 前記偏光子と前記位相差層との間に、λ/2板として機能する別の位相差層をさらに備え、
該偏光子の吸収軸と該位相差層の遅相軸とのなす角度が65°~85°であり、該偏光子の吸収軸と該別の位相差層の遅相軸とのなす角度が10°~20°である、
請求項1に記載の有機EL表示装置用円偏光板。 - 前記偏光子と前記位相差層との間に保護フィルムをさらに備える、請求項1に記載の有機EL表示装置用円偏光板。
- 前記偏光子と前記別の位相差層との間に保護フィルムをさらに備える、請求項2に記載の有機EL表示装置用円偏光板。
- 前記偏光子の前記位相差層と反対側に保護フィルムをさらに備える、請求項1から4のいずれかに記載の有機EL表示装置用円偏光板。
- 前記偏光子が長尺状であり、かつ、長尺方向に前記吸収軸を有し、
前記位相差層が長尺状であり、かつ、長尺方向に対して35°~55°の方向に前記遅相軸を有し、
請求項1、3または5に記載の有機EL表示装置用円偏光板。 - 前記偏光子が長尺状であり、かつ、長尺方向に前記吸収軸を有し、
前記位相差層および前記別の位相差層が長尺状であり、かつ、該位相差層が長尺方向に対して65°~85°の方向に前記遅相軸を有し、該別の位相差層が長尺方向に対して10°~20°の方向に前記遅相軸を有する、
請求項2、4または5に記載の有機EL表示装置用円偏光板。 - 前記偏光子におけるヨウ素含有量(重量%)に対するカリウム含有量(重量%)の比K/Iが0.180~0.235である、請求項1から7のいずれかに記載の有機EL表示装置用円偏光板。
- 請求項1から8のいずれかに記載の有機EL表示装置用円偏光板を備える、有機EL表示装置。
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