WO2022145169A1 - Optical film, production method therefor, and polarizing plate - Google Patents
Optical film, production method therefor, and polarizing plate Download PDFInfo
- Publication number
- WO2022145169A1 WO2022145169A1 PCT/JP2021/044208 JP2021044208W WO2022145169A1 WO 2022145169 A1 WO2022145169 A1 WO 2022145169A1 JP 2021044208 W JP2021044208 W JP 2021044208W WO 2022145169 A1 WO2022145169 A1 WO 2022145169A1
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- Prior art keywords
- film
- optical film
- polymer
- birefringence
- crystalline
- Prior art date
Links
- 239000012788 optical film Substances 0.000 title claims abstract description 221
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 46
- 239000010408 film Substances 0.000 claims abstract description 250
- 229920000642 polymer Polymers 0.000 claims abstract description 151
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- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 45
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- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 10
- 230000010287 polarization Effects 0.000 description 10
- 230000005540 biological transmission Effects 0.000 description 9
- OMIHGPLIXGGMJB-UHFFFAOYSA-N 7-oxabicyclo[4.1.0]hepta-1,3,5-triene Chemical group C1=CC=C2OC2=C1 OMIHGPLIXGGMJB-UHFFFAOYSA-N 0.000 description 8
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 8
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- 150000004678 hydrides Chemical class 0.000 description 7
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- PBKONEOXTCPAFI-UHFFFAOYSA-N 1,2,4-trichlorobenzene Chemical compound ClC1=CC=C(Cl)C(Cl)=C1 PBKONEOXTCPAFI-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 125000000217 alkyl group Chemical group 0.000 description 6
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 6
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- 125000004432 carbon atom Chemical group C* 0.000 description 5
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- 125000001424 substituent group Chemical group 0.000 description 4
- 238000001644 13C nuclear magnetic resonance spectroscopy Methods 0.000 description 3
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
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- OEVVKKAVYQFQNV-UHFFFAOYSA-N 1-ethenyl-2,4-dimethylbenzene Chemical compound CC1=CC=C(C=C)C(C)=C1 OEVVKKAVYQFQNV-UHFFFAOYSA-N 0.000 description 2
- GVLZQVREHWQBJN-UHFFFAOYSA-N 3,5-dimethyl-7-oxabicyclo[2.2.1]hepta-1,3,5-triene Chemical group CC1=C(O2)C(C)=CC2=C1 GVLZQVREHWQBJN-UHFFFAOYSA-N 0.000 description 2
- JLBJTVDPSNHSKJ-UHFFFAOYSA-N 4-Methylstyrene Chemical compound CC1=CC=C(C=C)C=C1 JLBJTVDPSNHSKJ-UHFFFAOYSA-N 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
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- MPMBRWOOISTHJV-UHFFFAOYSA-N but-1-enylbenzene Chemical compound CCC=CC1=CC=CC=C1 MPMBRWOOISTHJV-UHFFFAOYSA-N 0.000 description 2
- 235000011089 carbon dioxide Nutrition 0.000 description 2
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
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- 239000011630 iodine Substances 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 2
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- SBYMUDUGTIKLCR-UHFFFAOYSA-N 2-chloroethenylbenzene Chemical compound ClC=CC1=CC=CC=C1 SBYMUDUGTIKLCR-UHFFFAOYSA-N 0.000 description 1
- FZHNODDFDJBMAS-UHFFFAOYSA-N 2-ethoxyethenylbenzene Chemical compound CCOC=CC1=CC=CC=C1 FZHNODDFDJBMAS-UHFFFAOYSA-N 0.000 description 1
- KBKNKFIRGXQLDB-UHFFFAOYSA-N 2-fluoroethenylbenzene Chemical compound FC=CC1=CC=CC=C1 KBKNKFIRGXQLDB-UHFFFAOYSA-N 0.000 description 1
- CTHJQRHPNQEPAB-UHFFFAOYSA-N 2-methoxyethenylbenzene Chemical compound COC=CC1=CC=CC=C1 CTHJQRHPNQEPAB-UHFFFAOYSA-N 0.000 description 1
- DXIJHCSGLOHNES-UHFFFAOYSA-N 3,3-dimethylbut-1-enylbenzene Chemical compound CC(C)(C)C=CC1=CC=CC=C1 DXIJHCSGLOHNES-UHFFFAOYSA-N 0.000 description 1
- IWTYTFSSTWXZFU-UHFFFAOYSA-N 3-chloroprop-1-enylbenzene Chemical compound ClCC=CC1=CC=CC=C1 IWTYTFSSTWXZFU-UHFFFAOYSA-N 0.000 description 1
- CEBRPXLXYCFYGU-UHFFFAOYSA-N 3-methylbut-1-enylbenzene Chemical compound CC(C)C=CC1=CC=CC=C1 CEBRPXLXYCFYGU-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004727 Noryl Substances 0.000 description 1
- 229920001207 Noryl Polymers 0.000 description 1
- 239000005062 Polybutadiene Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- YMOONIIMQBGTDU-VOTSOKGWSA-N [(e)-2-bromoethenyl]benzene Chemical compound Br\C=C\C1=CC=CC=C1 YMOONIIMQBGTDU-VOTSOKGWSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 125000004103 aminoalkyl group Chemical group 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
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- 239000012298 atmosphere Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000000071 blow moulding Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- XZKRXPZXQLARHH-UHFFFAOYSA-N buta-1,3-dienylbenzene Chemical compound C=CC=CC1=CC=CC=C1 XZKRXPZXQLARHH-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
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- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 description 1
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
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- GCPCLEKQVMKXJM-UHFFFAOYSA-N ethoxy(diethyl)alumane Chemical compound CCO[Al](CC)CC GCPCLEKQVMKXJM-UHFFFAOYSA-N 0.000 description 1
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- 229940087305 limonene Drugs 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000001225 nuclear magnetic resonance method Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 1
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 1
- 125000002097 pentamethylcyclopentadienyl group Chemical group 0.000 description 1
- XKJCHHZQLQNZHY-UHFFFAOYSA-N phthalimide Chemical compound C1=CC=C2C(=O)NC(=O)C2=C1 XKJCHHZQLQNZHY-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920013636 polyphenyl ether polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
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- 229920005604 random copolymer Polymers 0.000 description 1
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- VIHDTGHDWPVSMM-UHFFFAOYSA-N ruthenium;triphenylphosphane Chemical compound [Ru].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 VIHDTGHDWPVSMM-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical compound C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- YOUIDGQAIILFBW-UHFFFAOYSA-J tetrachlorotungsten Chemical compound Cl[W](Cl)(Cl)Cl YOUIDGQAIILFBW-UHFFFAOYSA-J 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- MCULRUJILOGHCJ-UHFFFAOYSA-N triisobutylaluminium Chemical compound CC(C)C[Al](CC(C)C)CC(C)C MCULRUJILOGHCJ-UHFFFAOYSA-N 0.000 description 1
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-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
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3083—Birefringent or phase retarding elements
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F12/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F12/02—Monomers containing only one unsaturated aliphatic radical
- C08F12/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F12/06—Hydrocarbons
- C08F12/08—Styrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
- C08L101/12—Compositions of unspecified macromolecular compounds characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
Definitions
- the present invention relates to an optical film, a method for producing the same, and a polarizing plate.
- Patent Documents 1 to 3 Conventionally, a film manufacturing technique using a resin has been proposed (Patent Documents 1 to 3).
- a resin may be used to manufacture an optical film having anisotropy in the refractive index.
- Such an optical film having anisotropy in the refractive index may have birefringence.
- the optical film having birefringence can be provided in the display device as a film such as a reflection suppression film and a viewing angle compensation film.
- the optical film When the optical film is provided in the display device, it is required to appropriately adjust the balance between the birefringence in the thickness direction and the birefringence in the in-plane direction perpendicular to the thickness direction.
- the balance between the birefringence in the thickness direction and the birefringence in the in-plane direction can be expressed by the NZ coefficient of the optical film. For example, if an optical film having an NZ coefficient of more than 0.0 and less than 1.0 is obtained, the optical film makes it possible to improve the display quality when the display surface is viewed from an inclined direction.
- the optical film is required to have reverse wavelength dispersibility.
- An optical film having a reverse wavelength dispersibility can usually exhibit its optical function in a wide wavelength range.
- a wave plate as an optical film having anti-wavelength dispersibility can be used as a wide-band wave plate capable of functioning in a wide wavelength range.
- an optical film having an NZ coefficient of more than 0.0 and less than 1.0 Conventionally, a method for manufacturing an optical film having an NZ coefficient of more than 0.0 and less than 1.0 is known. Further, an optical film having a reverse wavelength dispersibility is conventionally known. However, it has not been conventionally achieved to realize an optical film having an NZ coefficient of more than 0.0 and less than 1.0 and having anti-wavelength dispersibility by a film having negative birefringence characteristics.
- the present invention was devised in view of the above problems, and is an optic having a negative birefringence characteristic, a reverse wavelength dispersibility, and an NZ coefficient larger than 0.0 and less than 1.0. It is an object of the present invention to provide a film and a method for producing the same; and a polarizing plate provided with the above-mentioned optical film;
- the present inventor has diligently studied to solve the above-mentioned problems. As a result, the present inventor has used a method including a step of bringing a resin film containing a crystalline polymer into contact with a solvent to change birefringence in the thickness direction and a step of stretching the resin film in this order. For example, they have found that the above-mentioned problems can be solved, and have completed the present invention. That is, the present invention includes the following.
- An optical film containing a crystalline polymer The optical film has a negative birefringence characteristic and The in-plane retardations Re (450), Re (550) and Re (650) of the optical film at the measurement wavelengths of 450 nm, 550 nm and 650 nm satisfy the formula (1).
- the optical film according to [1] wherein the optical film has a single-layer structure.
- the crystalline polymer having a negative intrinsic birefringence is a polystyrene-based polymer.
- a polarizing plate comprising the optical film according to any one of [1] to [8] and a polarizing film.
- a step of preparing a resin film made of a resin containing a crystalline polymer having a negative intrinsic birefringence and a thermoplastic polymer having a positive intrinsic birefringence comprising the steps of stretching the resin film in this order.
- a polarizing plate provided with an optical film; can be provided.
- the birefringence in the in-plane direction of the film is a value represented by (nx-ny), and is therefore represented by Re / d, unless otherwise specified.
- the birefringence in the thickness direction of the film is a value represented by [ ⁇ (nx + ny) / 2 ⁇ -nz], and is therefore represented by Rth / d, unless otherwise specified.
- the NZ coefficient of the film is a value represented by (nx-nz) / (nx-ny) unless otherwise specified.
- nx represents the refractive index in the direction perpendicular to the thickness direction of the film (in-plane direction) and in the direction giving the maximum refractive index.
- ny represents the refractive index in the in-plane direction of the film and perpendicular to the direction of nx.
- nz represents the refractive index in the thickness direction of the film.
- d represents the thickness of the film.
- the measurement wavelength is 550 nm unless otherwise specified.
- the material having positive intrinsic birefringence means a material in which the refractive index in the stretching direction is larger than the refractive index in the direction perpendicular to it, unless otherwise specified. Therefore, a polymer having positive intrinsic birefringence means a polymer in which the refractive index in the stretching direction is larger than the refractive index in the direction perpendicular to the refractive index, unless otherwise specified.
- the material having negative birefringence means a material in which the refractive index in the stretching direction is smaller than the refractive index in the direction perpendicular to the refractive index, unless otherwise specified. Therefore, a polymer having negative intrinsic birefringence means a polymer in which the refractive index in the stretching direction is smaller than the refractive index in the direction perpendicular to the refractive index, unless otherwise specified.
- the "long" shape means a shape having a length of 5 times or more, preferably 10 times or more, and specifically a roll. It refers to the shape of a film that has a length that allows it to be rolled up and stored or transported. There is no particular limitation on the upper limit of the length, but it is usually 100,000 times or less with respect to the width.
- the directions of the elements are "parallel”, “vertical” and “orthogonal”, and include errors within a range that does not impair the effect of the present invention, for example, within a range of ⁇ 5 °, unless otherwise specified. You may go out.
- the angle formed by the optical axis (absorption axis, transmission axis, slow phase axis, etc.) of each film in the member including a plurality of films represents the angle when the film is viewed from the thickness direction.
- the "polarizing plate”, “circular polarizing plate”, “wave plate” and “negative C plate” are not only rigid members but also flexible members such as resin films. Also includes. It was
- optical film contains a crystalline polymer. This optical film meets the following requirements (A) to (C) in combination.
- Requirement (A) The optical film has negative birefringence characteristics.
- optical film has been difficult to manufacture in the past, but it can be easily manufactured when a specific manufacturing method described later is used.
- the optical film according to this embodiment has a negative birefringence characteristic.
- the film has negative birefringence characteristics means that when the film is stretched in one stretching direction, the amount of increase in the refractive index in the direction perpendicular to the stretching direction is larger than the amount of increase in the refractive index in the stretching direction. , Say big. Further, the film "has a positive birefringence characteristic” means that when the film is stretched in one stretching direction, the amount of increase in the refractive index in the stretching direction is the amount of increase in the refractive index in the direction perpendicular to the stretching direction. It means that it is bigger than.
- the stretching direction is usually perpendicular to the thickness direction, and thus may be in-plane.
- the birefringence characteristics of the optical film can be examined by stretching the optical film.
- the birefringence characteristics of an optical film usually depend on the composition of the optical film. Therefore, when a resin film having the same composition as an optical film is stretched to produce an optical film as in the manufacturing method described later, the birefringence characteristics of the optical film are usually examined by stretching the resin film as well. be able to. Specifically, when the resin film is stretched in one stretching direction, if the amount of increase in the refractive index in the direction perpendicular to the stretching direction is larger than the amount of increase in the refractive index in the stretching direction, it is obtained from the resin film.
- the birefringence characteristic of the optical film to be obtained can be negative.
- the optical film of the present embodiment having a negative birefringence characteristic and an NZ coefficient satisfying the formula (2) is an optical film that has never existed before. Its industrial value is high.
- the in-plane retardation Re (450) at a measurement wavelength of 450 nm, the in-plane retardation Re (550) at a measurement wavelength of 550 nm, and the in-plane retardation Re (650) at a measurement wavelength of 650 nm according to the present embodiment are Equation (1) is satisfied.
- An optical film having an in-plane retardation satisfying the formula (1) usually has a reverse wavelength dispersibility. Therefore, the in-plane retardation of this optical film can be larger as the measurement wavelength is longer. Therefore, the optical film can exhibit its optical function in a wide wavelength range. For example, when the optical film can function as a 1/4 wave plate at one wavelength, the optical film can also function as a 1/4 wave plate in a wide wavelength range other than the one wavelength. Further, for example, when the optical film can function as a 1/2 wave plate at one wavelength, the optical film can also function as a 1/2 wave plate in a wide wavelength range other than the one wavelength.
- NZ coefficient of optical film The NZ coefficient Nz of the optical film according to the present embodiment satisfies the formula (2).
- the three-dimensional birefringence nx, ny and nz of the optical film having the NZ coefficient Nz satisfying this equation (2) can satisfy nx>nz> ny. 0 ⁇ Nz ⁇ 1 (2)
- the NZ coefficient Nz of the optical film is usually greater than 0.0, preferably greater than 0.1, more preferably greater than 0.2, and usually less than 1.0, preferably less than 0.9. , More preferably less than 0.8.
- An optical film having an NZ coefficient satisfying the formula (2) is not only in the polarized state of light passing through the optical film in the thickness direction, but also in the polarized state of light passing in an inclined direction that is neither parallel nor perpendicular to the thickness direction. Can be changed appropriately. Therefore, the optical film can exert its optical function not only for light in the thickness direction but also for light in the tilt direction. For example, when the optical film can give a phase difference of 1/4 wavelength to the light passing in the thickness direction, the optical film also gives a phase difference of 1/4 wavelength to the light passing in the tilt direction. sell. Further, for example, when the optical film can give a phase difference of 1/2 wavelength to the light passing in the thickness direction, the optical film has a phase difference of 1/2 wavelength to the light passing in the tilt direction. Can be given.
- the optical film according to an embodiment of the present invention contains a crystalline polymer.
- the crystalline polymer represents a polymer having crystallinity.
- the crystalline polymer represents a polymer having a melting point Tm. That is, the crystalline polymer represents a polymer whose melting point Tm can be observed with a differential scanning calorimeter (DSC).
- a resin containing a crystalline polymer may be referred to as a "crystalline resin”.
- This crystalline resin is preferably a thermoplastic resin.
- the optical film preferably contains a crystalline resin, and more preferably consists only of the crystalline resin.
- the crystalline polymer preferably has a negative intrinsic birefringence.
- a crystalline polymer having negative intrinsic birefringence When a crystalline polymer having negative intrinsic birefringence is stretched, it can exhibit a large refractive index in the direction perpendicular to the stretching direction. Therefore, when a crystalline polymer having a negative intrinsic birefringence is used, an optical film having a negative birefringence characteristic can be easily obtained. Further, when the crystalline polymer having negative intrinsic birefringence is used as described above, the in-plane retardation satisfying the formula (1) and the NZ coefficient satisfying the formula (2) can be easily achieved. ..
- crystalline polystyrene-based polymer As the crystalline polymer having negative intrinsic birefringence, a polymer containing an aromatic ring is preferable, and examples thereof include polystyrene-based polymers.
- the polystyrene-based polymer having crystallinity may be referred to as "crystalline polystyrene-based polymer”.
- the crystalline polystyrene-based polymer can be a polymer of a styrene-based monomer. Therefore, the crystalline polystyrene-based polymer can be a polymer containing a structural unit having a structure formed by polymerizing a styrene-based monomer (hereinafter, appropriately referred to as “styrene-based unit”).
- the styrene-based monomer may be an aromatic vinyl compound such as styrene or a styrene derivative.
- the styrene derivative include compounds in which the benzene ring of styrene or the ⁇ -position or ⁇ -position is substituted with a substituent.
- styrene-based monomer examples include styrene, alkylstyrene, halogenated styrene, halogenated alkylstyrene, alkoxystyrene, vinyl benzoic acid ester, and hydrogenated polymers thereof.
- alkyl styrene examples include methyl styrene, ethyl styrene, isopropyl styrene, t-butyl styrene, 2,4-dimethyl styrene, phenyl styrene, vinyl naphthalene, and vinyl styrene.
- halogenated styrene examples include chlorostyrene, bromostyrene, and fluorostyrene.
- halogenated alkyl styrenes examples include chloromethyl styrene.
- alkoxystyrene examples include methoxystyrene and ethoxystyrene.
- styrene-based monomers styrene, methylstyrene, ethylstyrene, and 2,4-dimethylstyrene are preferable. Further, one type of styrene-based monomer may be used, or two or more types may be used in combination.
- the crystalline polystyrene-based polymer preferably has an isotactic structure or a syndiotactic structure, and more preferably has a syndiotactic structure.
- the fact that the crystalline polystyrene-based polymer has a syndiotactic structure means that the stereochemical structure of the crystalline polystyrene-based polymer has a syndiotactic structure.
- the syndiotactic structure is a three-dimensional structure in which phenyl groups, which are side chains, are alternately located in opposite directions with respect to the main chain formed by a carbon-carbon bond in the Fischer projection formula. Compared with the polystyrene-based polymer having an atactic structure, the polystyrene-based polymer having a syndiotactic structure usually has a low specific density and is excellent in hydrolysis resistance, heat resistance and chemical resistance.
- the tacticity of a crystalline polystyrene-based polymer can be quantified by a nuclear magnetic resonance method ( 13 C-NMR method) using isotope carbon.
- 13 C-NMR method nuclear magnetic resonance method
- the tacticity measured by the C-NMR method can be indicated by the abundance ratio of a plurality of consecutive constituent units. In general, for example, when there are two consecutive building blocks, it is a diad, when there are three, it is a triad, and when there are five, it is a pentad.
- the crystalline polystyrene-based polymer having a syndiotactic structure may have a syndiotacticity of usually 75% or more, preferably 85% or more in diad (racemic diad), or pentad (racemic pen).
- (Tad) may have a syndiotacticity of usually 30% or more, preferably 50% or more.
- the crystalline polystyrene-based polymer may be a homopolymer or a copolymer. Therefore, the crystalline polystyrene-based polymer may be a homopolymer of one kind of styrene-based monomer, or may be a copolymer of two or more kinds of styrene-based monomers.
- the ratio of each styrene-based unit to 100% by weight of the entire crystalline polystyrene-based polymer is preferably 5% by weight. As described above, it is more preferably 10% by weight or more, preferably 95% by weight or less, and more preferably 90% by weight or less.
- the crystalline polystyrene-based polymer may be a copolymer of one or more types of styrene-based monomers and a monomer other than the styrene-based monomers.
- the proportion of the styrene-based unit contained in the crystalline polystyrene-based polymer is preferably 80% by weight or more, more preferably 83% by weight or more, still more preferably 85% by weight or more from the viewpoint of obtaining an optical film having desired optical properties. Is.
- the ratio of a certain structural unit contained in the crystalline polystyrene-based polymer can match the ratio of the monomer corresponding to the structural unit to all the monomers of the crystalline polystyrene-based polymer. Therefore, the ratio of the styrene-based unit contained in the crystalline polystyrene-based polymer may match the ratio of the styrene-based monomer to all the monomers of the crystalline polystyrene-based polymer.
- the crystalline polystyrene-based polymer is obtained, for example, by polymerizing a styrene-based monomer in an inert hydrocarbon solvent or in the absence of a solvent, using a titanium compound and a condensation product of water and trialkylaluminum as a catalyst. It can be manufactured (see Japanese Patent Application Laid-Open No. 62-187708).
- one type may be used alone, or two or more types may be used in combination at any ratio.
- the weight average molecular weight Mw of the crystalline polymer is preferably 130,000 or more, more preferably 140,000 or more, particularly preferably 150,000 or more, preferably 500,000 or less, and more preferably 450,000 or less. Particularly preferably, it is 400,000 or less. Since the crystalline polymer having such a weight average molecular weight Mw can have a high glass transition temperature Tg, the heat resistance of the optical film can be enhanced.
- the weight average molecular weight (Mw) of the polymer can be measured as a polystyrene-equivalent value by gel permeation chromatography (GPC) using 1,2,4-trichlorobenzene as a developing solvent.
- the glass transition temperature Tg of the crystalline polymer is preferably 85 ° C. or higher, more preferably 90 ° C. or higher, and particularly preferably 95 ° C. or higher.
- the glass transition temperature of the crystalline polymer is preferably 160 ° C. or lower, more preferably 155 ° C. or lower, and particularly preferably 150 ° C. or lower.
- the melting point Tm of the crystalline polymer is preferably 200 ° C. or higher, more preferably 210 ° C. or higher, particularly preferably 220 ° C. or higher, preferably 300 ° C. or lower, more preferably 290 ° C. or lower, and particularly preferably 280 ° C. or lower. Is.
- Tm of the crystalline polymer is within the above range, when the crystalline resin is molded to obtain a resin film, unintended progress of crystallization of the crystalline polymer and generation of foreign substances due to thermal decomposition are suppressed. can. Therefore, an optical film having good appearance and optical characteristics can be easily obtained.
- the glass transition temperature Tg and melting point Tm of the polymer can be measured by the following methods. First, the polymer is melted by heating, and the melted polymer is rapidly cooled with dry ice. Subsequently, using this polymer as a test piece, the glass transition temperature Tg and melting point Tm of the polymer were measured at a heating rate of 10 ° C./min (heating mode) using a differential scanning calorimeter (DSC). Can be measured.
- the amount of the crystalline polymer in 100% by weight of the crystalline resin is preferably 30% by weight or more, more preferably 40% by weight or more, and particularly preferably 45% by weight or more from the viewpoint of obtaining an optical film having desired optical properties. It is preferably 80% by weight or less, more preferably 70% by weight or less, and particularly preferably 65% by weight or less.
- the crystallinity of the crystalline polymer contained in the optical film is usually higher than a certain level.
- the specific range of crystallinity is preferably 10% or more, more preferably 15% or more, and particularly preferably 30% or more.
- the crystallinity of the crystalline polymer can be measured by X-ray diffraction.
- the crystalline resin may contain an amorphous polymer having no crystallinity in combination with the crystalline polymer.
- a thermoplastic polymer is usually used. Above all, this amorphous thermoplastic polymer preferably has a positive intrinsic birefringence. When a polymer having positive intrinsic birefringence is used in combination with the above-mentioned crystalline polymer having negative intrinsic birefringence, the inverse wavelength dispersibility of the optical film can be easily obtained.
- polyphenylene ether is preferable from the viewpoint of transparency and toughness.
- Polyphenylene ethers can usually have excellent compatibility with crystalline polystyrene-based polymers.
- Polyphenylene ether represents a polymer having a phenylene ether skeleton. Substituents may or may not be attached to the benzene ring of the phenylene ether skeleton. Polyphenylene ether usually has a phenylene ether skeleton in its backbone. As the polyphenylene ether, a polymer containing a phenylene ether unit represented by the following formula (I) is preferable.
- Q 1 is independently a halogen atom, a lower alkyl group (for example, an alkyl group having 1 or more and 7 or less carbon atoms), a phenyl group, a haloalkyl group, an aminoalkyl group, a hydrocarbon oxy group, or Represents a halohydrocarbon oxy group (where the halogen atom and the oxygen atom are separated by at least two carbon atoms).
- a halogen atom for example, an alkyl group having 1 or more and 7 or less carbon atoms
- a phenyl group for example, an alkyl group having 1 or more and 7 or less carbon atoms
- a phenyl group for example, a phenyl group, a haloalkyl group, an aminoalkyl group, a hydrocarbon oxy group, or Represents a halohydrocarbon oxy group (where the halogen atom and the oxygen atom are separated by at least two carbon atoms
- Q 2 is independently a hydrogen atom, a halogen atom, a lower alkyl group (for example, an alkyl group having 1 or more and 7 or less carbon atoms), a phenyl group, a haloalkyl group, a hydrocarbon oxy group, or a halo.
- a hydrocarbon oxy group where the halogen atom and the oxygen atom are separated by at least two carbon atoms.
- a hydrogen atom is preferable as Q2 .
- the polyphenylene ether may be a homopolymer having one kind of structural unit or a copolymer having two or more kinds of structural units.
- the polymer containing the structural unit represented by the formula (I) is a homopolymer
- a preferred example of the homopolymer is 2,6-dimethyl-1,4-phenylene ether unit ("-(”.
- Examples thereof include homopolymers having a structural unit (represented by C 6 H 2 (CH 3 ) 2 -O)-”.
- the polymer containing the structural unit represented by the formula (I) is a copolymer
- preferred examples of the copolymer include 2,6-dimethyl-1,4-phenylene ether unit and 2,3. , 6-trimethyl-1,4-phenylene ether unit (structural unit represented by "-(C 6 H (CH 3 ) 3 -O-)-”) and a random copolymer having a combination thereof.
- the polyphenylene ether may contain structural units other than the phenylene ether unit.
- the polyphenylene ether can be a copolymer having a phenylene ether unit and other structural units.
- the ratio of structural units other than the phenylene ether unit in the polyphenylene ether is preferably small as long as the desired optical properties can be obtained.
- the content of the phenylene ether unit in 100% by weight of the polyphenylene ether is preferably 50% by weight or more, more preferably 70% by weight or more, still more preferably 80% by weight or more, still more preferably 90% by weight or more. Particularly preferably, it is 95% by weight or more.
- polyphenylene ethers having other substituents grafted on the polymer chain can also be mentioned.
- Such polyphenylene ethers can be synthesized, for example, by grafting another substituent onto the polyphenylene ether by an appropriate method.
- Specific examples include polyphenylene ether grafted with a polymer such as polystyrene, polybutadiene, or other vinyl-containing polymer.
- polyphenylene ether may be produced by the method described in JP-A-11-302259.
- amorphous polymer one type may be used alone, or two or more types may be used in combination at any ratio.
- the weight average molecular weight Mw of the amorphous polymer such as polyphenylene ether is preferably 15,000 or more, more preferably 25,000 or more, particularly preferably 35,000 or more, and preferably 100,000 or less. It is preferably 85,000 or less, and particularly preferably 70,000 or less.
- the weight average molecular weight Mw of the amorphous polymer is not more than the lower limit of the above range, the mechanical strength of the optical film can be increased. Further, when the weight average molecular weight Mw of the amorphous polymer is not more than the upper limit of the above range, the crystalline polymer and the amorphous polymer can be uniformly mixed at a high level.
- the glass transition temperature of an amorphous polymer such as polyphenylene ether is preferably 100 ° C. or higher, more preferably 110 ° C. or higher, particularly preferably 120 ° C. or higher, preferably 350 ° C. or lower, more preferably 300 ° C. or lower. Particularly preferably, it is 250 ° C. or lower.
- the glass transition temperature of the amorphous polymer is at least the lower limit of the above range, the heat resistance of the optical film can be enhanced. Further, when the glass transition temperature of the amorphous polymer is not more than the upper limit of the above range, stretching in the manufacturing process of the optical film can be smoothly performed.
- the amount of the amorphous polymer in 100% by weight of the crystalline resin is preferably 20% by weight or more, more preferably 30% by weight or more, and particularly preferably 35% by weight from the viewpoint of obtaining an optical film having desired optical properties. % Or more, preferably 70% by weight or less, more preferably 60% by weight or less, and particularly preferably 55% by weight or less.
- the weight ratio (thermoplastic polymer / crystalline polymer) is , Preferably within a specific range. Specifically, the weight ratio (thermoplastic polymer / crystalline polymer) is preferably 3/7 or more, more preferably 3.5 / 6.5 or more, and particularly preferably 4/6 or more. Is 8/2 or less, more preferably 7.5 / 2.5 or less, and particularly preferably 7/3 or less.
- the weight ratio (thermoplastic polymer / crystalline polymer) is in the above range, the inverse wavelength dispersibility of the optical film can be easily obtained.
- the crystalline resin may contain any component in combination with the above-mentioned crystalline polymer and amorphous polymer.
- Optional components include, for example, lubricants; layered crystal compounds; fine particles such as inorganic fine particles; antioxidants, heat stabilizers, light stabilizers, weathering stabilizers, ultraviolet absorbers, stabilizers such as near-infrared absorbers; plastics. Agents; colorants such as dyes and pigments; antistatic agents; and the like. Any component may be used alone or in combination of two or more. The amount of any component can be appropriately determined as long as the effect of the present invention is not significantly impaired. The amount of any component may be, for example, in the range where the total light transmittance of the optical film can be maintained at 85% or more.
- the optical film may have a multi-layer structure including a plurality of layers, but preferably has a single-layer structure.
- the single-layer structure represents a structure having only a single layer having the same composition and not having a layer having a composition different from the above-mentioned composition. Therefore, it is preferable that the optical film has a single layer formed of the crystalline resin.
- the optical film preferably has an in-plane retardation in an appropriate range according to the application.
- the specific in-plane retardation Re of the optical film may be preferably 100 nm or more, more preferably 110 nm or more, particularly preferably 120 nm or more, and preferably 180 nm or less, more preferably 170 nm or less at a measurement wavelength of 550 nm. Particularly preferably, it may be 160 nm or less.
- the optical film can function as a 1/4 wave plate.
- the specific in-plane retardation Re of the optical film may be preferably 245 nm or more, more preferably 265 nm or more, particularly preferably 270 nm or more, and preferably 320 nm or less, more preferably 300 nm at a measurement wavelength of 550 nm.
- it may be particularly preferably 295 nm or less.
- the optical film can function as a 1/2 wave plate.
- the film retardation can be measured using a phase difference meter (for example, "AXoScan OPMF-1" manufactured by AXOMETRICS).
- a phase difference meter for example, "AXoScan OPMF-1" manufactured by AXOMETRICS.
- the optical film preferably has high transparency.
- the specific total light transmittance of the optical film is preferably 80% or more, more preferably 85% or more, and particularly preferably 88% or more.
- the total light transmittance of the film can be measured in the wavelength range of 400 nm to 700 nm using an ultraviolet / visible spectrometer.
- the optical film preferably has a small haze.
- the haze of the optical film is preferably less than 1.0%, more preferably less than 0.8%, particularly preferably less than 0.5%, ideally 0.0%.
- the haze of the film can be measured using a haze meter (for example, "NDH5000" manufactured by Nippon Denshoku Kogyo Co., Ltd.).
- the optical film may contain a solvent.
- This solvent may be incorporated into the film in the step of bringing the resin film into contact with the solvent in the production method described later. Specifically, all or part of the solvent incorporated into the film upon contact with the resin film can enter the interior of the polymer. Therefore, it is difficult to completely remove the solvent even if the drying is performed above the boiling point of the solvent. Therefore, the optical film may contain a solvent.
- the optical film is preferably a stretched film.
- the stretched film represents a film produced through a stretching treatment.
- the optical film is preferably a uniaxially stretched film.
- the uniaxially stretched film represents a film that is positively stretched only in one direction and is not positively stretched in any other direction. Since the uniaxially stretched film can be manufactured by stretching in only one direction, the manufacturing process can be simplified, and thus simple manufacturing can be realized.
- the optical film may be a single-wafer film or a long film having a long shape.
- the optical film has a long shape, it is possible to continuously manufacture a polarizing plate by laminating the optical film and the long polarizing film.
- the thickness of the optical film can be set appropriately according to the application of the optical film.
- the specific thickness of the optical film is preferably 5 ⁇ m or more, more preferably 10 ⁇ m or more, particularly preferably 30 ⁇ m or more, preferably 400 ⁇ m or less, more preferably 300 ⁇ m or less, and particularly preferably 200 ⁇ m or less.
- the above-mentioned optical film is The step (i) of preparing a resin film made of a crystalline resin containing a crystalline polymer having a negative intrinsic birefringence and a thermoplastic polymer having a positive intrinsic birefringence; The step (ii) of bringing the resin film into contact with a solvent to change the birefringence in the thickness direction; The step of stretching the resin film (iii) and Can be manufactured by a manufacturing method containing the above in this order.
- the resin film before being brought into contact with the solvent in step (ii) is referred to as "raw film”, and the resin film after being brought into contact with the solvent in step (ii) is referred to as "pre-stretched film”. ".
- the present inventor presumes that the mechanism for obtaining the above-mentioned optical film by the above-mentioned manufacturing method is as follows. However, the technical scope of the present invention is not limited by the following mechanism.
- an optical film is manufactured using a resin film containing a crystalline polymer having a negative intrinsic birefringence.
- a crystalline polymer having a negative intrinsic birefringence When a crystalline polymer having a negative intrinsic birefringence is oriented in a certain orientation direction, it can exhibit a small refractive index in the orientation direction and a large refractive index in the direction perpendicular to the orientation direction. Therefore, the resin film and the optical film containing this crystalline polymer can have negative birefringence characteristics as represented by the requirement (A).
- the optical film may contain a thermoplastic polymer having a positive intrinsic birefringence in combination with a crystalline polymer having a negative intrinsic birefringence.
- a thermoplastic polymer having positive intrinsic birefringence When oriented in a certain orientation direction, a large refractive index may be developed in the orientation direction, and a small refractive index may be developed in the direction perpendicular to the orientation direction. Therefore, when oriented in a certain orientation direction, the direction in which the refractive index of the crystalline polymer is maximized and the direction in which the refractive index of the thermoplastic polymer is maximized can be perpendicular to each other.
- the entire birefringence of the optical film containing the combination of the crystalline polymer and the thermoplastic polymer may reflect the difference between the birefringence of the crystalline polymer and the birefringence of the thermoplastic polymer.
- the difference between the birefringence of the crystalline polymer and the birefringence of the thermoplastic polymer is small at a short measurement wavelength and large at a long measurement wavelength. Therefore, the optical film obtained by the above-mentioned manufacturing method can have a reverse wavelength dispersibility as represented by the requirement (B).
- the solvent infiltrates into the raw fabric film.
- the action of the infiltrated solvent causes microBrownian motion in the molecules of the crystalline polymer in the film, and the molecular chains are oriented. According to the study of the present inventor, it is considered that the solvent-induced crystallization phenomenon of the crystalline polymer may proceed when the molecular chain is oriented.
- the surface area of the film is large on the front surface and the back surface, which are the main surfaces. Therefore, as for the infiltration rate of the solvent, the infiltration rate in the thickness direction through the front surface or the back surface is high. Then, the orientation of the molecules of the crystalline polymer can proceed so that the molecules of the polymer are oriented in the thickness direction. Therefore, in the step (ii), the molecules of the crystalline polymer can be oriented in the thickness direction.
- the pre-stretched film as a resin film in which the molecules of the crystalline polymer are oriented in the thickness direction in the step (ii) is stretched in the step (iii).
- the molecules of the polymer contained in the pre-stretched film can be oriented in a direction perpendicular to the thickness direction. Therefore, by combining the orientation in the thickness direction in the step (iii) and the orientation in the direction perpendicular to the thickness direction in the step (iii), the orientation direction of the polymer molecules can be three-dimensionally adjusted. can. Therefore, the optical film obtained by the above-mentioned manufacturing method can have an NZ coefficient in an appropriate range as represented by the requirement (C).
- Step of preparing a resin film includes a step of preparing a raw film as a resin film before contacting with a solvent.
- a crystalline resin containing a crystalline polymer can be used as the material of the raw film prepared in the step (i).
- the raw film is preferably made of only crystalline resin.
- the crystalline resin contained in the raw film may be the same as the crystalline resin contained in the optical film.
- the crystallinity of the crystalline polymer contained in the raw film is preferably small.
- the specific crystallinity is preferably less than 10%, more preferably less than 5%, and particularly preferably less than 3%. If the crystallinity of the crystalline polymer contained in the raw film before contact with the solvent is low, many molecules of the crystalline polymer can be oriented in the thickness direction by contact with the solvent, so that in a wide range.
- the NZ coefficient can be adjusted.
- the raw film preferably has optical isotropic properties. Therefore, the raw film preferably has a small birefringence Re / d in the in-plane direction, and preferably has a small absolute value
- the birefringence Re / d of the raw film in the in-plane direction is preferably less than 1.0 ⁇ 10 -3 , more preferably less than 0.5 ⁇ 10 -3 , and particularly preferably 0.3 ⁇ . It is less than 10 -3 .
- of the birefringence in the thickness direction of the raw film is preferably less than 1.0 ⁇ 10 -3 , more preferably less than 0.5 ⁇ 10 -3 , and particularly preferably 0.3. It is less than ⁇ 10 -3 .
- Having optical isotropic properties as described above indicates that the molecular orientation of the crystalline polymer contained in the raw film is low and is substantially non-oriented.
- the raw film preferably has a small solvent content, and more preferably does not contain a solvent.
- the ratio (solvent content) of the solvent contained in the raw film to 100% by weight of the raw film is preferably 1% or less, more preferably 0.5% or less, and particularly preferably 0.1% or less. Ideally, it is 0.0%. Since the amount of the solvent contained in the raw film before contact with the solvent is small, many molecules of the crystalline polymer can be oriented in the thickness direction by the contact with the solvent, so that the NZ coefficient can be adjusted in a wide range. Is possible.
- the solvent content of the raw film can be measured by the density.
- the haze of the raw film is preferably less than 1.0%, preferably less than 0.8%, more preferably less than 0.5%, and ideally 0.0%.
- the thickness of the raw film is set according to the thickness of the optical film to be manufactured.
- the thickness is increased by contacting with the solvent in the step (ii).
- the thickness becomes smaller. Therefore, the thickness of the raw film may be set in consideration of the change in thickness in the step (ii) and the step (iii) as described above.
- the raw film may be a single-wafer film, but it is preferably a long film.
- a long raw film it is possible to continuously produce an optical film by a roll-to-roll method, so that the productivity of the optical film can be effectively increased.
- a method for producing the raw fabric film since a raw fabric film containing no solvent can be obtained, an injection molding method, an extrusion molding method, a press molding method, an inflation molding method, a blow molding method, a calendar molding method, and a casting molding method.
- a resin molding method such as a compression molding method is preferable.
- the extrusion molding method is preferable because the thickness can be easily controlled.
- the manufacturing conditions in the extrusion molding method are preferably as follows.
- the cylinder temperature (molten resin temperature) is preferably Tm or higher, more preferably “Tm + 20 ° C” or higher, preferably “Tm + 100 ° C” or lower, and more preferably “Tm + 50 ° C” or lower.
- the cooling body that the molten resin extruded into a film comes into contact with first is not particularly limited, but a cast roll is usually used.
- the cast roll temperature is preferably "Tg-50 ° C.” or higher, preferably "Tg + 70 ° C.” or lower, and more preferably "Tg + 40 ° C.” or lower.
- the raw fabric film When the raw fabric film is manufactured under such conditions, the raw fabric film having a thickness of 1 ⁇ m to 1 mm can be easily manufactured.
- Tm represents the melting point of the crystalline polymer
- Tg represents the glass transition temperature of the crystalline polymer.
- the method for producing an optical film includes a step (ii) in which a resin film as a raw film is brought into contact with a solvent after the step (i). By this step (ii), the birefringence in the thickness direction of the raw film is changed, and a pre-stretched film having a birefringence in the thickness direction different from that of the raw film is obtained.
- an organic solvent is usually used.
- a solvent that can penetrate into the resin film without dissolving the crystalline polymer contained in the resin film can be used, and for example, a hydrocarbon solvent such as cyclohexane, toluene, limonene, and decalin can be used. ; Carbon disulfide;
- the type of the solvent may be one type or two or more types.
- the contact method between the resin film and the solvent there are no restrictions on the contact method between the resin film and the solvent.
- Examples of the contact method include a spray method in which a solvent is sprayed on a resin film; a coating method in which a solvent is applied to a resin film; a dipping method in which a resin film is immersed in a solvent; and the like. Above all, the dipping method is preferable because continuous contact can be easily performed.
- the temperature of the solvent in contact with the resin film is arbitrary as long as the solvent can maintain the liquid state, and therefore can be set in the range of the melting point or more and the boiling point or less of the solvent.
- the contact time is preferably 0.5 seconds or longer, more preferably 1.0 seconds or longer, and particularly preferably 5.0 seconds or longer.
- the upper limit is not particularly limited and may be, for example, 24 hours or less. However, since the degree of progress of orientation tends not to change significantly even if the contact time is lengthened, it is preferable that the contact time is short as long as the desired optical characteristics can be obtained.
- the birefringence Rth / d in the thickness direction of the resin film changes.
- the amount of change in birefringence Rth / d in the thickness direction caused by contact with the solvent is preferably 0.1 ⁇ 10 -3 or more, more preferably 0.2 ⁇ 10 -3 or more, and particularly preferably 0.3 ⁇ 10 It is -3 or more, preferably 50.0 ⁇ 10 -3 or less, more preferably 30.0 ⁇ 10 -3 or less, and particularly preferably 20.0 ⁇ 10 -3 or less.
- the amount of change in the birefringence Rth / d in the thickness direction represents an absolute value of the change in the birefringence Rth / d in the thickness direction of the resin film.
- the specific amount of change in the birefringence Rth / d in the thickness direction is obtained by subtracting the birefringence Rth / d in the thickness direction of the original film from the birefringence Rth / d in the thickness direction of the unstretched film and obtaining it as an absolute value. Be done.
- the birefringence Rth / d in the thickness direction is increased by contact between the resin film and the solvent.
- the birefringence Re / d in the in-plane direction of the resin film may or may not change due to contact with the solvent. From the viewpoint of simplifying the control of the in-plane retardation Re of the optical film, it is preferable that the change in the birefringence Re / d in the in-plane direction caused by the contact with the solvent is small, and it is more preferable that the change does not occur. preferable.
- the amount of change in birefringence Re / d in the in-plane direction caused by contact with the solvent is preferably 0.0 ⁇ 10 -3 to 0.2 ⁇ 10 -3 , more preferably 0.0 ⁇ 10 -3 to 0.
- the amount of change in the birefringence Re / d in the in-plane direction represents an absolute value of the change in the birefringence Re / d in the in-plane direction of the resin film.
- the specific amount of change in the in-plane birefringence Re / d is obtained by subtracting the in-plane birefringence Re / d of the raw film from the in-plane birefringence Re / d of the unstretched film. Obtained as a value.
- the pre-stretched film as the resin film after contact with the solvent is a negative C plate. Therefore, it is preferable that the refractive index nz in the thickness direction of the unstretched film is smaller than the refractive indexes nx and ny in the in-plane direction. Further, it is preferable that the refractive indexes nx and ny in the in-plane direction of the unstretched film are the same value or close to each other.
- the difference between the refractive index nx and the refractive index ny is relatively small, the difference between the refractive index nz and the refractive index nz is relatively large, and the difference between the refractive index ny and the refractive index nz is relatively large. It is preferably relatively large.
- the difference between the rate nz and the in-plane refractive indexes nx and ny can be expressed.
- the birefringence Rth / d in the thickness direction of the unstretched film is preferably 0.05 ⁇ 10 -3 or more, preferably 0.1 ⁇ 10 -3 or more, and particularly preferably 0.2 ⁇ 10 -3 or more. It is preferably 10 ⁇ 10 -3 or less, more preferably 6.0 ⁇ 10 -3 or less, and particularly preferably 4.0 ⁇ 10 -3 or less.
- the birefringence Re / d in the in-plane direction of the pre-stretched film may be smaller than the birefringence Rth / d in the thickness direction of the pre-stretched film.
- the specific range of birefringence Re / d in the in-plane direction of the unstretched film is preferably 0.01 ⁇ 10 -3 or more, preferably 0.05 ⁇ 10 -3 or more, and particularly preferably 0.1 ⁇ 10. It is -3 or more, preferably 1.0 ⁇ 10 -3 or less, more preferably 0.5 ⁇ 10 -3 or less, and particularly preferably 0.2 ⁇ 10 -3 or less.
- the pre-stretched film as the resin film after contact with the solvent has an NZ coefficient greater than 1.0.
- the specific NZ coefficient of the pre-stretched film is preferably greater than 1.0, more preferably greater than 5.0, particularly preferably greater than 10, and preferably less than 50, more preferably less than 40, particularly preferred. Is less than 30.
- the thickness of the resin film is usually increased due to the infiltration of the solvent in contact with the resin film into the resin film.
- the lower limit of the rate of change in the thickness of the resin film at this time may be, for example, 1% or more, 2% or more, or 3% or more.
- the upper limit of the change rate of the thickness may be, for example, 80% or less, 50% or less, or 40% or less.
- the rate of change in the thickness of the resin film is a ratio obtained by dividing the difference in thickness between the raw film and the unstretched film by the thickness of the raw film.
- the method for producing an optical film includes a step (iii) of stretching a resin film as a pre-stretching film after the step (iii).
- the molecules of the polymer contained in the resin film can be oriented in a direction corresponding to the stretching direction. Therefore, according to the stretching in the step (iii), the in-plane birefringence Re / d, the in-plane retardation Re, the thickness direction birefringence Rth / d, the thickness direction birefringence Rth, and the NZ coefficient
- the above-mentioned optical film can be obtained by adjusting the optical characteristics such as.
- the stretching direction there is no limitation on the stretching direction, and examples thereof include a longitudinal direction, a width direction, and an oblique direction.
- the diagonal direction is a direction perpendicular to the thickness direction and is neither parallel nor perpendicular to the width direction.
- the stretching direction may be one direction or two or more directions, but one direction is preferable. Further, among the stretching in one direction, free uniaxial stretching in which no binding force is applied in a direction other than the stretching direction is further preferable. According to these stretchings, the above-mentioned optical film can be easily manufactured.
- the pre-stretched film usually has negative birefringence characteristics
- an optical film having a slow axis in the direction perpendicular to the stretching direction can be obtained. Therefore, since the slow phase axis direction of the optical film can be adjusted by the stretching direction, the stretching direction may be selected according to the direction of the slow phase axis to be expressed in the optical film.
- a long polarizing film has an absorption axis in its longitudinal direction and a transmission axis in its width direction.
- the pre-stretched film is stretched in the longitudinal direction to obtain an optical film having a slow phase axis in the width direction. You may get it. In this case, it is possible to efficiently manufacture a polarizing plate by roll-to-roll using a long optical film and a long polarizing film.
- the draw ratio is preferably 1.1 times or more, more preferably 1.2 times or more, preferably 20.0 times or less, more preferably 10.0 times or less, still more preferably 5.0 times or less, particularly. It is preferably 2.0 times or less. It is desirable to appropriately set the specific draw ratio according to factors such as the optical characteristics, thickness, and mechanical strength of the optical film to be manufactured.
- the stretching ratio is equal to or higher than the lower limit of the above range, the birefringence can be significantly changed by stretching. Further, when the draw ratio is not more than the upper limit of the above range, the direction of the slow phase axis can be easily controlled and the film breakage can be effectively suppressed.
- the stretching temperature is preferably "Tg R " or higher, more preferably “Tg R + 10 ° C” or higher, preferably “Tg R + 100 ° C” or lower, and more preferably “Tg R + 90 ° C” or lower.
- Tg R represents the glass transition temperature of the crystalline resin.
- the stretching temperature is equal to or higher than the lower limit of the above range, the resin film can be sufficiently softened and stretched uniformly. Further, when the stretching temperature is not more than the upper limit of the above range, the curing of the resin film due to the progress of crystallization of the crystalline polymer can be suppressed, so that the stretching can be smoothly performed, and the stretching causes a large birefringence. Can be expressed. In addition, the haze of the resulting optical film can usually be reduced to increase transparency.
- an optical film can be obtained as a stretched resin film.
- the balance between the birefringence Rth / d in the thickness direction and the birefringence Re / d in the in-plane direction can be adjusted to obtain a desired NZ coefficient. ..
- the optical properties such as retardation are exhibited by the orientation of the polymer due to the contact with the solvent in the step (iii) and the orientation of the polymer due to the stretching in the step (iii), so that the optical film is desired. It can have optical properties.
- the method for producing an optical film may be combined with the above-mentioned steps (i) to (iii) and further include any step.
- a step of preheating the pre-stretched film before the step (iii) a step of heat-treating the optical film obtained in the step (iii) to promote the crystallization of the crystalline polymer, and the like.
- Examples thereof include a step of drying the optical film to reduce the amount of the solvent in the film, a step of heat-shrinking the optical film to remove residual stress in the film, and the like.
- a long optical film can be manufactured by using a long raw film.
- the method for producing an optical film may include a step of winding the long optical film thus produced into a roll shape. Further, the method for producing an optical film may include a step of cutting a long optical film into a desired shape.
- the polarizing plate according to the embodiment of the present invention includes the above-mentioned optical film and a polarizing film.
- the polarizing film can usually function as a linear splitter. Therefore, the polarizing plate can transmit a part of the polarized light and block the other polarized light.
- the polarizing film usually has an absorption axis and a transmission axis perpendicular to the absorption axis. Then, it is possible to absorb the linear polarization having a vibration direction parallel to the absorption axis and transmit the linear polarization having a vibration direction parallel to the transmission axis.
- the vibration direction of linearly polarized light means the vibration direction of the electric field of linearly polarized light. At this time, it is preferable that the absorption axis of the polarizing film and the slow axis of the optical film form a specific angle.
- the angle formed by the absorption axis of the polarizing film and the slow axis of the optical film is preferably 80 ° or more, more preferably 85 ° or more, particularly preferably 88 ° or more, and preferably 100 ° or less. It is more preferably 95 ° or less, and particularly preferably 92 ° or less.
- the optical film preferably has an in-plane retardation that can function as a 1/2 wave plate.
- the polarizing plate according to this example can be used as a polarizing plate capable of compensating the viewing angle when provided in an image display device.
- the angle formed by the absorption axis of the polarizing film and the slow axis of the optical film is preferably 40 ° or more, more preferably 42 ° or more, particularly preferably 44 ° or more, and preferably 50 °. Below, it is more preferably 48 ° or less, and particularly preferably 46 ° or less.
- the optical film preferably has an in-plane retardation that can function as a 1/4 wave plate.
- the polarizing plate according to this example can be used as a circular polarizing plate capable of transmitting circular polarization in one rotation direction and blocking circular polarization in the other rotation direction. By providing this circularly polarizing plate on the display surface of the display device, it is possible to suppress the reflection of external light. It was
- any polarizing film can be used as the polarizing film.
- An example of a polarizing film is a film obtained by adsorbing iodine or a dichroic dye on a polyvinyl alcohol film and then uniaxially stretching it in a boric acid bath; adsorbing iodine or a dichroic dye on the polyvinyl alcohol film. Examples thereof include a film obtained by stretching and further modifying a part of polyvinyl alcohol units in the molecular chain to polyvinylene units. Of these, the polarizing film preferably contains polyvinyl alcohol. It was
- the degree of polarization of this polarizing film is not particularly limited, but is preferably 98% or more, more preferably 99% or more.
- the thickness of the polarizing film is preferably 5 ⁇ m to 80 ⁇ m. It was
- the above-mentioned polarizing plate may further include an arbitrary layer.
- the optional layer may be, for example, a polarizing element protective film layer; an adhesive layer for bonding a polarizing film and an optical film; a hard coat layer such as an impact-resistant polymethacrylate resin layer; a matte layer for improving the slipperiness of the film; Examples thereof include a reflection suppressing layer; an antifouling layer; an antistatic layer; and the like. Any of these layers may be provided with only one layer, or may be provided with two or more layers.
- the glass transition temperature Tg and the melting point Tm of the polymer were measured as follows. First, the polymer was melted by heating, and the melted polymer was rapidly cooled with dry ice. Subsequently, using this polymer as a test piece, the glass transition temperature Tg and melting point Tm of the polymer were measured at a heating rate of 10 ° C./min (heating mode) using a differential scanning calorimeter (DSC). It was measured.
- the weight average molecular weight of this polymer was measured by gel permeation chromatography at 135 ° C. using 1,2,4-trichlorobenzene as a solvent. As a result, the weight average molecular weight Mw of this polymer was 350,000. Further, it was confirmed by measuring the melting point Tm and 13 C-NMR that the obtained polymer was crystalline polystyrene having a syndiotactic structure. The melting point Tm of crystalline polystyrene was 270 ° C., and the glass transition temperature was 100 ° C. By repeating this operation, crystalline polystyrene having the syndiotactic structure required for evaluation was prepared.
- 0.014 parts of the tetrachlorotungsten phenylimide (tetrahydrofuran) complex was dissolved in 0.70 parts of toluene to prepare a solution.
- 0.061 part of a diethylaluminum ethoxide / n-hexane solution having a concentration of 19% was added and stirred for 10 minutes to prepare a catalytic solution.
- This catalyst solution was added to a pressure resistant reactor to initiate a ring-opening polymerization reaction. Then, the reaction was carried out for 4 hours while maintaining 53 ° C. to obtain a solution of a ring-opening polymer of dicyclopentadiene.
- the number average molecular weight (Mn) and weight average molecular weight (Mw) of the obtained ring-opening polymer of dicyclopentadiene are 8,750 and 28,100, respectively, and the molecular weight distribution (Mw / Mn) obtained from these. was 3.21.
- the hydride and the solution contained in the reaction solution were separated using a centrifuge and dried under reduced pressure at 60 ° C. for 24 hours to open dicyclopentadiene as a crystalline polymer having positive intrinsic birefringence. 28.5 parts of the hydride of the ring polymer was obtained.
- the hydrogenation rate of this hydride was 99% or more, the glass transition temperature Tg was 93 ° C., the melting point Tm was 262 ° C., and the ratio of racemo diad was 89%.
- Crystalline resin pellets are melt-extruded using a thermal melt extrusion film forming machine equipped with a T-die (“Measuring Extruder Type Me-20 / 2800V3” manufactured by Optical Control Systems) and rolled at a speed of 1.5 m / min. A long raw film was obtained as a resin film having a width of about 120 mm before contacting with a solvent.
- the operating conditions of the film forming machine are itemized below.
- the thickness of the original film was 158 ⁇ m.
- a pre-stretched film was obtained. The pre-stretched film was taken out from cyclohexane, the cyclohexane adhering to the film surface was wiped off, and then the film was naturally dried in the air. The thickness of the obtained pre-stretched film was 160 ⁇ m.
- the unstretched film was cut into a rectangle of 100 mm x 100 mm. Both ends of this rectangular pre-stretched film were gripped by the five clips of the stretching device, respectively.
- the pre-stretched film was pulled with a clip and freely uniaxially stretched in the longitudinal direction of the long raw film obtained in the extrusion film formation step.
- the stretching temperature was 138 ° C. and the stretching ratio was 1.2 times. By this stretching, an optical film as a uniaxially stretched film was obtained.
- the direction of the slow axis of the optical film was perpendicular to the stretching direction. Further, the NZ coefficient at the measurement wavelength of 550 nm was 0.45.
- step (1-2) The line speed in step (1-2) was changed to change the thickness of the long raw film to 115 ⁇ m.
- the raw film was not immersed in the solvent in step (1-3).
- step (1-4) the raw film was stretched instead of the pre-stretched film, the stretching temperature was changed to 132 ° C., and the stretching ratio was changed to 2.2 times.
- the optical film was manufactured by the same method as in Example 1 except for the above items.
- a mixture of a hydride of a ring-opening polymer of dicyclopentadiene and an antioxidant was formed into a strand by hot melt extrusion molding, and then shredded with a strand cutter to obtain pellets of a crystalline resin.
- a polarizing film (“HLC2-5618S” manufactured by Sanritz Co., Ltd., a polarizing element having a thickness of 180 ⁇ m and a polarization transmission axis in the width direction) was prepared. With respect to one surface of the polarizing film and the optical films obtained in Examples 1 to 3 and Comparative Examples 1 and 2, the polarization transmission axis of the polarizing film and the slow axis of the optical film form an angle of 45 °.
- a circular polarizing plate was obtained by laminating with a pressure-sensitive adhesive layer (“CS9621” manufactured by Nitto Denko).
- a mirror was prepared and the prepared circular polarizing plate was placed on the mirror so that the optical film was on the mirror side.
- the circularly polarizing plate was illuminated with a fluorescent lamp, and the reflected light from the mirror was observed in the front direction and in the tilt direction with a polar angle of about 60 °.
- the front direction is the front direction of the mirror and represents a direction parallel to the thickness direction of the circularly polarizing plate. In each observation direction, " ⁇ " if the coloring is not visible, “ ⁇ ” if the coloring is visible but very slight, and " ⁇ " if the coloring is visible at an unacceptable level. And said.
- Example 4 [Evaluation of Optical Film Obtained in Example 4] Two polarizing films (“HLC2-5618S” manufactured by Sanritz, 180 ⁇ m in thickness, and a polarizing element having a polarizing transmission axis in the width direction) were prepared and placed on a cross Nicol.
- Cross Nicol means that the polarization transmission axis is vertical when viewed from the thickness direction.
- the optical film obtained in Example 4 is placed on the polarizing transmission axis of the polarizing film on the viewing side (that is, the polarizing film on the viewing side when installed in a backlight described later) and the slow axis of the optical film. It was installed so that it matches.
- a polarizing film and an optical film were bonded to each other via an adhesive layer (“CS9621” manufactured by Nitto Denko) to obtain a laminated body.
- a backlight was prepared in a dark room, and the prepared laminate was placed on the backlight. With the backlight turned on, the light transmitted through the laminate was observed in the front direction and in the tilting direction with a polar angle of about 60 °. At each observation position, “ ⁇ ” is visible if the tint is not visible, “ ⁇ ” if the tint is visible but very slight, and the tint and light leakage are visible at an unacceptable level. If it is, it is set as "x".
- crystalline polystyrene is used as the crystalline polymer having negative intrinsic birefringence to produce an optical film.
- the delayed phase axis was developed in the direction perpendicular to the stretching direction in all the examples, so that the obtained optical film was negatively birefringent. It can be confirmed that it has a refraction characteristic.
- all of the optical films obtained in the examples have an in-plane retardation satisfying the formula (1) and an NZ coefficient satisfying the formula (2).
- the optical film obtained in the examples has a reverse wavelength dispersibility, its optical function can be exhibited in a wide wavelength range. Therefore, the optical films of Examples 1 to 3 can function as a quarter wave plate in a wide wavelength range. Therefore, the circularly polarizing plate provided with the optical film can suppress the reflection of light in a wide wavelength range as a reflection suppressing film. Therefore, it is possible to suppress the coloring caused by the light of a part of the wavelength passing through the circularly polarizing plate. Further, the optical film of Example 4 can function as a 1/2 wave plate in a wide wavelength range. Therefore, the optical film can convert the vibration direction of linearly polarized light in a wide wavelength range transmitted through the optical film by 90 °. Therefore, it is possible to suppress coloring and light leakage due to the passage of light having a part of wavelengths through the laminate.
- the optical film obtained in the examples has an appropriate NZ coefficient, not only the light transmitted through the optical film in the thickness direction but also the polarization of the light transmitted in the inclined direction which is neither parallel nor perpendicular to the thickness direction.
- the state can also be changed appropriately. Therefore, since the optical films of Examples 1 to 3 can suppress the reflection of the light transmitted through the circularly polarizing plate in the tilting direction, the tinting can be suppressed not only in the front direction but also in the tilting direction. Further, since the optical film of Example 4 can suppress the passage of light of the laminated body in the inclined direction, it is possible to suppress coloring and light leakage not only in the front direction but also in the inclined direction.
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Abstract
Description
すなわち、本発明は、下記のものを含む。 The present inventor has diligently studied to solve the above-mentioned problems. As a result, the present inventor has used a method including a step of bringing a resin film containing a crystalline polymer into contact with a solvent to change birefringence in the thickness direction and a step of stretching the resin film in this order. For example, they have found that the above-mentioned problems can be solved, and have completed the present invention.
That is, the present invention includes the following.
前記光学フィルムが、負の複屈折特性を有し、
前記光学フィルムの測定波長450nm、550nm及び650nmにおける面内レターデーションRe(450)、Re(550)及びRe(650)が式(1)を満たし、
前記光学フィルムのNZ係数Nzが、式(2)を満たす、光学フィルム。
Re(450)<Re(550)<Re(650) (1)
0<Nz<1 (2)
〔2〕 前記光学フィルムが、単層構造を有する、〔1〕に記載の光学フィルム。
〔3〕 前記光学フィルムが、延伸フィルムである、〔1〕又は〔2〕に記載の光学フィルム。
〔4〕 前記光学フィルムが、一軸延伸フィルムである、〔1〕~〔3〕のいずれか一項に記載の光学フィルム。
〔5〕 前記光学フィルムが、長尺の形状を有する、〔1〕~〔4〕のいずれか一項に記載の光学フィルム。
〔6〕 負の固有複屈折を有する前記結晶性重合体と、正の固有複屈折を有する熱可塑性重合体と、を含む樹脂からなる、〔1〕~〔5〕のいずれか一項に記載の光学フィルム。
〔7〕 正の固有複屈折を有する前記熱可塑性重合体と負の固有複屈折を有する前記結晶性重合体との重量比(熱可塑性重合体/結晶性重合体)が、3/7以上である、〔6〕に記載の光学フィルム。
〔8〕 負の固有複屈折を有する前記結晶性重合体が、ポリスチレン系重合体であり、
正の固有複屈折を有する前記熱可塑性重合体が、ポリフェニレンエーテルである、〔6〕又は〔7〕に記載の光学フィルム。
〔9〕 〔1〕~〔8〕のいずれか一項に記載の光学フィルムと、偏光フィルムと、を備える偏光板。
〔10〕 前記光学フィルムの遅相軸と、前記偏光フィルムの吸収軸と、が80°~100°の角度をなす、〔9〕に記載の偏光板。
〔11〕 〔1〕~〔8〕のいずれか一項に記載の光学フィルムの製造方法であって、
負の固有複屈折を有する結晶性重合体と、正の固有複屈折を有する熱可塑性重合体と、を含む樹脂からなる樹脂フィルムを用意する工程と、
前記樹脂フィルムを、溶媒に接触させて、厚み方向の複屈折を変化させる工程と、
前記樹脂フィルムを延伸する工程と、をこの順に含む、光学フィルムの製造方法。 [1] An optical film containing a crystalline polymer.
The optical film has a negative birefringence characteristic and
The in-plane retardations Re (450), Re (550) and Re (650) of the optical film at the measurement wavelengths of 450 nm, 550 nm and 650 nm satisfy the formula (1).
An optical film in which the NZ coefficient Nz of the optical film satisfies the formula (2).
Re (450) <Re (550) <Re (650) (1)
0 <Nz <1 (2)
[2] The optical film according to [1], wherein the optical film has a single-layer structure.
[3] The optical film according to [1] or [2], wherein the optical film is a stretched film.
[4] The optical film according to any one of [1] to [3], wherein the optical film is a uniaxially stretched film.
[5] The optical film according to any one of [1] to [4], wherein the optical film has a long shape.
[6] The item according to any one of [1] to [5], which comprises a resin containing the crystalline polymer having a negative intrinsic birefringence and a thermoplastic polymer having a positive intrinsic birefringence. Optical film.
[7] When the weight ratio (thermoplastic polymer / crystalline polymer) of the thermoplastic polymer having positive intrinsic birefringence and the crystalline polymer having negative intrinsic birefringence is 3/7 or more. The optical film according to [6].
[8] The crystalline polymer having a negative intrinsic birefringence is a polystyrene-based polymer.
The optical film according to [6] or [7], wherein the thermoplastic polymer having positive intrinsic birefringence is a polyphenylene ether.
[9] A polarizing plate comprising the optical film according to any one of [1] to [8] and a polarizing film.
[10] The polarizing plate according to [9], wherein the slow axis of the optical film and the absorption axis of the polarizing film form an angle of 80 ° to 100 °.
[11] The method for producing an optical film according to any one of [1] to [8].
A step of preparing a resin film made of a resin containing a crystalline polymer having a negative intrinsic birefringence and a thermoplastic polymer having a positive intrinsic birefringence.
The step of bringing the resin film into contact with a solvent to change the birefringence in the thickness direction,
A method for producing an optical film, comprising the steps of stretching the resin film in this order.
本発明の一実施形態に係る光学フィルムは、結晶性重合体を含む。この光学フィルムは、下記の要件(A)~(C)を組み合わせて満たす。 [1. Overview of optical film]
The optical film according to an embodiment of the present invention contains a crystalline polymer. This optical film meets the following requirements (A) to (C) in combination.
要件(B):光学フィルムの測定波長450nm、550nm及び650nmにおける面内レターデーションRe(450)、Re(550)及びRe(650)が式(1)を満たす。
要件(C):光学フィルムのNZ係数Nzが、式(2)を満たす。
Re(450)<Re(550)<Re(650) (1)
0<Nz<1 (2) Requirement (A): The optical film has negative birefringence characteristics.
Requirement (B): In-plane retardations Re (450), Re (550) and Re (650) of the optical film at the measurement wavelengths of 450 nm, 550 nm and 650 nm satisfy the formula (1).
Requirement (C): The NZ coefficient Nz of the optical film satisfies the equation (2).
Re (450) <Re (550) <Re (650) (1)
0 <Nz <1 (2)
本実施形態に係る光学フィルムは、負の複屈折特性を有する。
フィルムが「負の複屈折特性を有する」とは、フィルムを一の延伸方向に延伸した場合に、延伸方向における屈折率の増加量よりも、延伸方向に垂直な方向における屈折率の増加量が、大きいことをいう。また、フィルムが「正の複屈折特性を有する」とは、フィルムを一の延伸方向に延伸した場合に、延伸方向における屈折率の増加量が、延伸方向に垂直な方向における屈折率の増加量よりも、大きいことをいう。増加量であるから、延伸によって屈折率が大きくなった場合には、当該屈折率の増加量はプラスの値となり、延伸によって屈折率が小さくなった場合には、当該屈折率の増加量はマイナスの値となる。ここで、前記の延伸方向は、通常、厚み方向に対して垂直であり、よって、面内方向でありうる。 [2. Birefringence characteristics of optical film]
The optical film according to this embodiment has a negative birefringence characteristic.
"The film has negative birefringence characteristics" means that when the film is stretched in one stretching direction, the amount of increase in the refractive index in the direction perpendicular to the stretching direction is larger than the amount of increase in the refractive index in the stretching direction. , Say big. Further, the film "has a positive birefringence characteristic" means that when the film is stretched in one stretching direction, the amount of increase in the refractive index in the stretching direction is the amount of increase in the refractive index in the direction perpendicular to the stretching direction. It means that it is bigger than. Since it is an increase amount, when the refractive index increases due to stretching, the increase amount of the refractive index becomes a positive value, and when the refractive index decreases due to stretching, the increase amount of the refractive index becomes negative. Is the value of. Here, the stretching direction is usually perpendicular to the thickness direction, and thus may be in-plane.
本実施形態に係る光学フィルムの測定波長450nmにおける面内レターデーションRe(450)、測定波長550nmにおける面内レターデーションRe(550)、及び、測定波長650nmにおける面内レターデーションRe(650)は、式(1)を満たす。
Re(450)<Re(550)<Re(650) (1) [3. Wavelength dispersibility of optical film]
The in-plane retardation Re (450) at a measurement wavelength of 450 nm, the in-plane retardation Re (550) at a measurement wavelength of 550 nm, and the in-plane retardation Re (650) at a measurement wavelength of 650 nm according to the present embodiment are Equation (1) is satisfied.
Re (450) <Re (550) <Re (650) (1)
本実施形態に係る光学フィルムのNZ係数Nzは、式(2)を満たす。この式(2)を満たすNZ係数Nzを有する光学フィルムの三次元複屈折nx、ny及びnzは、nx>nz>nyを満たすことができる。
0<Nz<1 (2)
詳細には、光学フィルムのNZ係数Nzは、通常0.0より大きく、好ましくは0.1より大きく、更に好ましくは0.2より大きく、また、通常1.0未満、好ましくは0.9未満、更に好ましくは0.8未満である。 [4. NZ coefficient of optical film]
The NZ coefficient Nz of the optical film according to the present embodiment satisfies the formula (2). The three-dimensional birefringence nx, ny and nz of the optical film having the NZ coefficient Nz satisfying this equation (2) can satisfy nx>nz> ny.
0 <Nz <1 (2)
Specifically, the NZ coefficient Nz of the optical film is usually greater than 0.0, preferably greater than 0.1, more preferably greater than 0.2, and usually less than 1.0, preferably less than 0.9. , More preferably less than 0.8.
本発明の一実施形態に係る光学フィルムは、結晶性重合体を含む。結晶性重合体とは、結晶性を有する重合体を表す。結晶性を有する重合体とは、融点Tmを有する重合体を表す。すなわち、結晶性を有する重合体とは、示差走査熱量計(DSC)で融点Tmを観測することができる重合体を表す。以下の説明において、結晶性重合体を含む樹脂を「結晶性樹脂」ということがある。この結晶性樹脂は、好ましくは熱可塑性樹脂である。光学フィルムは、結晶性樹脂を含むこと好ましく、結晶性樹脂のみからなることがより好ましい。 [5. Optical film composition]
The optical film according to an embodiment of the present invention contains a crystalline polymer. The crystalline polymer represents a polymer having crystallinity. The crystalline polymer represents a polymer having a melting point Tm. That is, the crystalline polymer represents a polymer whose melting point Tm can be observed with a differential scanning calorimeter (DSC). In the following description, a resin containing a crystalline polymer may be referred to as a "crystalline resin". This crystalline resin is preferably a thermoplastic resin. The optical film preferably contains a crystalline resin, and more preferably consists only of the crystalline resin.
光学フィルムは、複数の層を含む複層構造を有していてもよいが、単層構造を有することが好ましい。単層構造とは、同じ組成を有する単一の層のみを有し、前記の組成とは異なる組成を有する層を備えない構造を表す。よって、光学フィルムは、前記の結晶性樹脂で形成された層を単独で有することが好ましい。 [6. Layer structure of optical film]
The optical film may have a multi-layer structure including a plurality of layers, but preferably has a single-layer structure. The single-layer structure represents a structure having only a single layer having the same composition and not having a layer having a composition different from the above-mentioned composition. Therefore, it is preferable that the optical film has a single layer formed of the crystalline resin.
光学フィルムは、その用途に応じた適切な範囲の面内レターデーションを有することが好ましい。 [7. Characteristics of optical film]
The optical film preferably has an in-plane retardation in an appropriate range according to the application.
上述した光学フィルムは、
負の固有複屈折を有する結晶性重合体と、正の固有複屈折を有する熱可塑性重合体と、を含む結晶性樹脂からなる樹脂フィルムを用意する工程(i)と;
樹脂フィルムを、溶媒に接触させて、厚み方向の複屈折を変化させる工程(ii)と;
樹脂フィルムを延伸する工程(iii)と、
をこの順に含む製造方法によって、製造できる。
以下の説明では、樹脂フィルムのうち、工程(ii)において溶媒と接触させられる前の樹脂フィルムを「原反フィルム」、工程(ii)において溶媒接触させられた後の樹脂フィルムを「延伸前フィルム」ということがある。 [8. Outline of manufacturing method of optical film]
The above-mentioned optical film is
The step (i) of preparing a resin film made of a crystalline resin containing a crystalline polymer having a negative intrinsic birefringence and a thermoplastic polymer having a positive intrinsic birefringence;
The step (ii) of bringing the resin film into contact with a solvent to change the birefringence in the thickness direction;
The step of stretching the resin film (iii) and
Can be manufactured by a manufacturing method containing the above in this order.
In the following description, among the resin films, the resin film before being brought into contact with the solvent in step (ii) is referred to as "raw film", and the resin film after being brought into contact with the solvent in step (ii) is referred to as "pre-stretched film". ".
光学フィルムの製造方法は、溶媒に接触させる前の樹脂フィルムとしての原反フィルムを用意する工程を含む。 [9. Step of preparing a resin film (i)]
The method for producing an optical film includes a step of preparing a raw film as a resin film before contacting with a solvent.
光学フィルムの製造方法は、工程(i)の後に、原反フィルムとしての樹脂フィルムを溶媒に接触させる工程(ii)を含む。この工程(ii)により、原反フィルムの厚み方向の複屈折が変化して、原反フィルムとは異なる厚み方向の複屈折を有する延伸前フィルムが得られる。 [10. Step of bringing the resin film into contact with the solvent (ii)]
The method for producing an optical film includes a step (ii) in which a resin film as a raw film is brought into contact with a solvent after the step (i). By this step (ii), the birefringence in the thickness direction of the raw film is changed, and a pre-stretched film having a birefringence in the thickness direction different from that of the raw film is obtained.
光学フィルムの製造方法は、工程(ii)の後に、延伸前フィルムとしての樹脂フィルムを延伸する工程(iii)を含む。延伸により、樹脂フィルムに含まれる重合体の分子を延伸方向に応じた方向に配向させることができる。よって、工程(iii)での延伸によれば、樹脂フィルムの面内方向の複屈折Re/d、面内レターデーションRe、厚み方向の複屈折Rth/d、厚み方向のレターデーションRth、NZ係数等の光学特性を調整して、上述した光学フィルムを得ることができる。 [11. Step of stretching the resin film (iii)]
The method for producing an optical film includes a step (iii) of stretching a resin film as a pre-stretching film after the step (iii). By stretching, the molecules of the polymer contained in the resin film can be oriented in a direction corresponding to the stretching direction. Therefore, according to the stretching in the step (iii), the in-plane birefringence Re / d, the in-plane retardation Re, the thickness direction birefringence Rth / d, the thickness direction birefringence Rth, and the NZ coefficient The above-mentioned optical film can be obtained by adjusting the optical characteristics such as.
光学フィルムの製造方法は、上述した工程(i)~工程(iii)に組み合わせて、更に任意の工程を含んでいてもよい。任意の工程としては、例えば、工程(iii)の前に延伸前フィルムを予熱する工程、工程(iii)で得られた光学フィルムに熱処理を施して結晶性重合体の結晶化を促進する工程、光学フィルムを乾燥してフィルム中の溶媒量を減らす工程、光学フィルムを熱収縮させてフィルム中の残留応力を除去する工程、などが挙げられる。 [12. Arbitrary process]
The method for producing an optical film may be combined with the above-mentioned steps (i) to (iii) and further include any step. As an arbitrary step, for example, a step of preheating the pre-stretched film before the step (iii), a step of heat-treating the optical film obtained in the step (iii) to promote the crystallization of the crystalline polymer, and the like. Examples thereof include a step of drying the optical film to reduce the amount of the solvent in the film, a step of heat-shrinking the optical film to remove residual stress in the film, and the like.
本発明の一実施形態に係る偏光板は、上述した光学フィルムと、偏光フィルムとを備える。偏光フィルムは、通常、直線偏光子として機能できる。よって、偏光板は、一部の偏光を透過し、他の偏光を遮ることができる。 [13. Polarizer]
The polarizing plate according to the embodiment of the present invention includes the above-mentioned optical film and a polarizing film. The polarizing film can usually function as a linear splitter. Therefore, the polarizing plate can transmit a part of the polarized light and block the other polarized light.
以下の説明において、量を表す「%」及び「部」は、別に断らない限り、重量基準である。また、以下に説明する操作は、別に断らない限り、常温常圧(23℃1気圧)大気中の条件において行った。 Hereinafter, the present invention will be specifically described with reference to examples. However, the present invention is not limited to the examples shown below, and may be arbitrarily modified and carried out without departing from the scope of claims of the present invention and the equivalent scope thereof.
In the following description, "%" and "part" representing quantities are based on weight unless otherwise specified. Further, the operations described below were performed under normal temperature and pressure (23 ° C., 1 atm) in the atmosphere unless otherwise specified.
重合体のガラス転移温度Tg及び融点Tmの測定は、以下のようにして行った。まず、重合体を、加熱によって融解させ、融解した重合体をドライアイスで急冷した。続いて、この重合体を試験体として用いて、示差走査熱量計(DSC)を用いて、10℃/分の昇温速度(昇温モード)で、重合体のガラス転移温度Tg及び融点Tmを測定した。 [Measurement method of glass transition temperature Tg and melting point Tm]
The glass transition temperature Tg and the melting point Tm of the polymer were measured as follows. First, the polymer was melted by heating, and the melted polymer was rapidly cooled with dry ice. Subsequently, using this polymer as a test piece, the glass transition temperature Tg and melting point Tm of the polymer were measured at a heating rate of 10 ° C./min (heating mode) using a differential scanning calorimeter (DSC). It was measured.
光学フィルムの面内レターデーションRe、厚み方向のレターデーションRth、NZ係数及び遅相軸方向は、位相差計(AXOMETRICS社製「AxoScan OPMF-1」)により測定した。 [Measurement method of optical film retardation, NZ coefficient and slow phase axial direction]
The in-plane retardation Re of the optical film, the retardation Rth in the thickness direction, the NZ coefficient, and the slow phase axial direction were measured by a phase difference meter (“AXoScan OPMF-1” manufactured by AXOMETRICS).
アルゴン置換した内容積500mlのガラス製容器に、硫酸銅5水塩(CuSO4・5H2O)17.8g(71ミリモル)、トルエン200ml、及び、トリメチルアルミニウム24ml(250ミリモル)を入れ、40℃で8時間反応させた。その後、固体部分を除去して溶液を得た。得られた溶液から、更に、トルエンを室温下で減圧留去して、接触生成物6.7gを得た。この接触生成物の分子量を、凝固点下降法によって測定したところ、610であった。 [Manufacturing example 1. Manufacture of crystalline polystyrene]
17.8 g (71 mmol) of copper sulfate pentahydrate (CuSO 4.5H 2 O), 200 ml of toluene, and 24 ml (250 mmol) of trimethylaluminum were placed in a glass container having an internal volume of 500 ml and substituted with argon, and the temperature was 40 ° C. Was reacted for 8 hours. Then, the solid part was removed to obtain a solution. Toluene was further distilled off from the obtained solution under reduced pressure at room temperature to obtain 6.7 g of a contact product. The molecular weight of this contact product was measured by the freezing point lowering method and found to be 610.
この操作を繰り返して、評価に必要なシンジオタクチック構造を有する結晶性ポリスチレンを準備した。 The weight average molecular weight of this polymer was measured by gel permeation chromatography at 135 ° C. using 1,2,4-trichlorobenzene as a solvent. As a result, the weight average molecular weight Mw of this polymer was 350,000. Further, it was confirmed by measuring the melting point Tm and 13 C-NMR that the obtained polymer was crystalline polystyrene having a syndiotactic structure. The melting point Tm of crystalline polystyrene was 270 ° C., and the glass transition temperature was 100 ° C.
By repeating this operation, crystalline polystyrene having the syndiotactic structure required for evaluation was prepared.
金属製の耐圧反応器を、充分に乾燥した後、窒素置換した。この金属製耐圧反応器に、シクロヘキサン154.5部、ジシクロペンタジエン(エンド体含有率99%以上)の濃度70%シクロヘキサン溶液42.8部(ジシクロペンタジエンの量として30部)、及び1-ヘキセン1.9部を加え、53℃に加温した。 [Manufacturing example 2. Production of crystalline polymer with positive intrinsic birefringence]
The pressure resistant reactor made of metal was sufficiently dried and then replaced with nitrogen. In this metal pressure resistant reactor, 154.5 parts of cyclohexane, 42.8 parts of a 70% cyclohexane solution of dicyclopentadiene (endo content of 99% or more) (30 parts as the amount of dicyclopentadiene), and 1- 1.9 parts of hexene was added and heated to 53 ° C.
(1-1.結晶性樹脂の用意)
製造例1で得たシンジオタクチック構造を有する結晶性ポリスチレン60部と、ポリフェニレンエーテル(サビックイノベーティブプラスチックスジャパン社製「ノリルPPO640」、重量平均分子量Mw=43,000、ガラス転移温度Tg=130℃)40部とを、295℃において2軸押出機で混練し、透明な結晶性樹脂のペレットを製造した。 [Example 1]
(1-1. Preparation of crystalline resin)
60 parts of crystalline polystyrene having a syndiotactic structure obtained in Production Example 1, polyphenylene ether (“Noryl PPO640” manufactured by SABIC Innovative Plastics Japan Co., Ltd., weight average molecular weight Mw = 43,000, glass transition temperature Tg = 130 40 parts (° C.) was kneaded at 295 ° C. with a twin-screw extruder to produce transparent crystalline resin pellets.
結晶性樹脂のペレットを、Tダイを備える熱溶融押出しフィルム成形機(Optical Control Systems社製「Measuring Extruder Type Me-20/2800V3」)を用いて溶融押し出しし、1.5m/分の速度でロールに巻き取って、およそ幅120mmの溶媒接触前の樹脂フィルムとして長尺の原反フィルムを得た。フィルム成形機の運転条件を、以下に箇条書きで記す。
・バレル温度設定=280℃~300℃
・ダイ温度=300℃
・スクリュー回転数=30rpm
・キャストロール温度=80℃ (1-2. Extrusion film formation)
Crystalline resin pellets are melt-extruded using a thermal melt extrusion film forming machine equipped with a T-die (“Measuring Extruder Type Me-20 / 2800V3” manufactured by Optical Control Systems) and rolled at a speed of 1.5 m / min. A long raw film was obtained as a resin film having a width of about 120 mm before contacting with a solvent. The operating conditions of the film forming machine are itemized below.
・ Barrel temperature setting = 280 ° C to 300 ° C
・ Die temperature = 300 ℃
・ Screw rotation speed = 30 rpm
・ Cast roll temperature = 80 ℃
前記の原反フィルムを120mm×120mmの矩形にカットした。この矩形の原反フィルムを、バットに貯められた溶媒としてのシクロヘキサン中に、面内レターデーションRe=2nm、厚み方向のレターデーションRth=41nmになるまで浸漬して、溶媒接触後の樹脂フィルムとして延伸前フィルムを得た。延伸前フィルムをシクロヘキサンから取り出し、フィルム表面に付着したシクロヘキサンを拭き取った後、大気中で自然乾燥させた。得られた延伸前フィルムの厚みは、160μmであった。 (1-3. Solvent contact)
The raw film was cut into a rectangle of 120 mm × 120 mm. This rectangular raw film is immersed in cyclohexane as a solvent stored in a bat until the in-plane retardation Re = 2 nm and the thickness direction retardation Rth = 41 nm, and used as a resin film after contact with the solvent. A pre-stretched film was obtained. The pre-stretched film was taken out from cyclohexane, the cyclohexane adhering to the film surface was wiped off, and then the film was naturally dried in the air. The thickness of the obtained pre-stretched film was 160 μm.
バッチ式二軸延伸装置(エトー社製)を用意した。この延伸装置は、オーブンユニットと、フィルムを固定可能な延伸用のクリップとを備えていた。この延伸装置を用いれば、オーブン内でクリップによってフィルムを引っ張って、前記のフィルムを延伸することが可能である。 (1-4. Stretching)
A batch type biaxial stretching device (manufactured by Eto'o) was prepared. The stretching device was equipped with an oven unit and a stretching clip capable of fixing the film. Using this stretching device, it is possible to stretch the film by pulling the film with a clip in the oven.
工程(1-2)におけるライン速度を変更して、長尺の原反フィルムの厚みを107μmに変更した。
また、工程(1-3)において原反フィルムの溶媒中への浸漬を、面内レターデーションRe=2nm、厚み方向のレターデーションRth=28nmの延伸前フィルムが得られるように浸漬時間を調整して行った。
さらに、工程(1-4)における延伸倍率を1.3倍に変更した。
以上の事項以外は実施例1と同じ方法によって、光学フィルムの製造を行った。 [Example 2]
The line speed in step (1-2) was changed to change the thickness of the long raw film to 107 μm.
Further, in step (1-3), the immersion time of the raw film in the solvent was adjusted so that a pre-stretched film having an in-plane retardation Re = 2 nm and a thickness direction retardation Rth = 28 nm could be obtained. I went there.
Further, the draw ratio in the step (1-4) was changed to 1.3 times.
The optical film was manufactured by the same method as in Example 1 except for the above items.
工程(1-2)におけるライン速度を変更して、長尺の原反フィルムの厚みを276μmに変更した。
また、工程(1-3)において原反フィルムの溶媒中への浸漬を、面内レターデーションRe=4nm、厚み方向のレターデーションRth=71nmの延伸前フィルムが得られるように浸漬時間を調整して行った。
さらに、工程(1-4)における延伸倍率を1.1倍に変更した。
以上の事項以外は実施例1と同じ方法によって、光学フィルムの製造を行った。 [Example 3]
The line speed in step (1-2) was changed to change the thickness of the long raw film to 276 μm.
Further, in step (1-3), the immersion time of the raw film in the solvent was adjusted so that a pre-stretched film having an in-plane retardation Re = 4 nm and a thickness direction retardation Rth = 71 nm could be obtained. I went there.
Further, the draw ratio in the step (1-4) was changed to 1.1 times.
The optical film was manufactured by the same method as in Example 1 except for the above items.
工程(1-1)において、シンジオタクチック構造を有する結晶性ポリスチレンの量を50部に変更し、ポリフェニレンエーテルの量を50部に変更した。
また、工程(1-2)におけるライン速度を変更して、長尺の原反フィルムの厚みを201μmに変更した。
さらに、工程(1-3)において原反フィルムの溶媒中への浸漬を、面内レターデーションRe=42nm、厚み方向のレターデーションRth=540nmの延伸前フィルムが得られるように浸漬時間を調整して行った。
また、工程(1-4)における延伸温度を160℃に、延伸倍率を1.6倍に変更した。
以上の事項以外は実施例1と同じ方法によって、光学フィルムの製造を行った。 [Example 4]
In step (1-1), the amount of crystalline polystyrene having a syndiotactic structure was changed to 50 parts, and the amount of polyphenylene ether was changed to 50 parts.
Further, the line speed in the step (1-2) was changed to change the thickness of the long raw film to 201 μm.
Further, in step (1-3), the immersion time of the raw film in the solvent was adjusted so that a pre-stretched film having an in-plane retardation Re = 42 nm and a thickness direction retardation Rth = 540 nm could be obtained. I went there.
Further, the stretching temperature in the step (1-4) was changed to 160 ° C., and the stretching ratio was changed to 1.6 times.
The optical film was manufactured by the same method as in Example 1 except for the above items.
工程(1-2)におけるライン速度を変更して、長尺の原反フィルムの厚みを115μmに変更した。
また、工程(1-3)における原反フィルムの溶媒中への浸漬を行わなかった。
さらに、工程(1-4)において延伸前フィルムの代わりに原反フィルムを延伸し、延伸温度を132℃に変更し、延伸倍率を2.2倍に変更した。
以上の事項以外は実施例1と同じ方法によって、光学フィルムの製造を行った。 [Comparative Example 1]
The line speed in step (1-2) was changed to change the thickness of the long raw film to 115 μm.
In addition, the raw film was not immersed in the solvent in step (1-3).
Further, in step (1-4), the raw film was stretched instead of the pre-stretched film, the stretching temperature was changed to 132 ° C., and the stretching ratio was changed to 2.2 times.
The optical film was manufactured by the same method as in Example 1 except for the above items.
製造例2で得られたジシクロペンタジエンの開環重合体の水素化物100部に、酸化防止剤(テトラキス〔メチレン-3-(3’,5’-ジ-t-ブチル-4’-ヒドロキシフェニル)プロピオネート〕メタン;BASFジャパン社製「イルガノックス(登録商標)1010」)1.1部を混合後、内径3mmΦのダイ穴を4つ備えた二軸押出し機(東芝機械社製「TEM-37B」)に投入した。ジシクロペンタジエンの開環重合体の水素化物及び酸化防止剤の混合物を、熱溶融押出し成形によりストランド状の成形した後、ストランドカッターにて細断して、結晶性樹脂のペレットを得た。 [Comparative Example 2]
An antioxidant (tetrakis [methylene-3- (3', 5'-di-t-butyl-4'-hydroxyphenyl)] was added to 100 parts of the hydride of the ring-opening polymer of dicyclopentadiene obtained in Production Example 2. ) Propionate] Methane; BASF Japan's "Irganox (registered trademark) 1010") After mixing 1.1 parts, a twin-screw extruder equipped with four die holes with an inner diameter of 3 mmΦ (Toshiba Machine Co., Ltd. "TEM-37B" ”). A mixture of a hydride of a ring-opening polymer of dicyclopentadiene and an antioxidant was formed into a strand by hot melt extrusion molding, and then shredded with a strand cutter to obtain pellets of a crystalline resin.
また、工程(1-3)において、溶媒の種類をトルエンに変更した。更に、原反フィルムの溶媒中への浸漬を、面内レターデーションRe=8nm、厚み方向のレターデーションRth=-73nmの延伸前フィルムが得られるように浸漬時間を調整して行った。
さらに、工程(1-4)における延伸温度を130℃に変更し、延伸倍率を1.5倍に変更した。
以上の事項以外は実施例1と同じ方法によって、光学フィルムの製造を行った。 This pellet was used in step (1-2). Further, the line speed in the step (1-2) was changed to change the thickness of the long raw film to 13 μm.
Further, in step (1-3), the type of solvent was changed to toluene. Further, the raw film was immersed in the solvent by adjusting the immersion time so that a pre-stretched film having an in-plane retardation Re = 8 nm and a thickness direction retardation Rth = −73 nm could be obtained.
Further, the stretching temperature in the step (1-4) was changed to 130 ° C., and the stretching ratio was changed to 1.5 times.
The optical film was manufactured by the same method as in Example 1 except for the above items.
偏光フィルム(サンリッツ社製「HLC2-5618S」、厚さ180μm、幅方向に偏光透過軸を有する偏光子)を用意した。この偏光フィルムの一方の面と、実施例1~3および比較例1~2で得た光学フィルムとを、偏光フィルムの偏光透過軸と光学フィルムの遅相軸とが45°の角度をなすように、粘着剤層(日東電工製「CS9621」)を介して貼り合わせて、円偏光板を得た。 [Evaluation of Optical Films Obtained in Examples 1 to 3 and Comparative Examples 1 and 2]
A polarizing film (“HLC2-5618S” manufactured by Sanritz Co., Ltd., a polarizing element having a thickness of 180 μm and a polarization transmission axis in the width direction) was prepared. With respect to one surface of the polarizing film and the optical films obtained in Examples 1 to 3 and Comparative Examples 1 and 2, the polarization transmission axis of the polarizing film and the slow axis of the optical film form an angle of 45 °. A circular polarizing plate was obtained by laminating with a pressure-sensitive adhesive layer (“CS9621” manufactured by Nitto Denko).
偏光フィルム(サンリッツ社製「HLC2-5618S」、厚さ180μm、幅方向に偏光透過軸を有する偏光子)を2枚用意し、クロスニコルに配置した。クロスニコルとは、厚み方向から見て偏光透過軸が垂直になることをいう。これら偏光フィルムの間に実施例4で得た光学フィルムを、視認側の偏光フィルム(即ち、後述するバックライトに設置した時に視認側になる偏光フィルム)の偏光透過軸と光学フィルムの遅相軸とが一致するように設置した。粘着剤層(日東電工製「CS9621」)を介して偏光フィルムと光学フィルムとを貼り合わせて、積層体を得た。 [Evaluation of Optical Film Obtained in Example 4]
Two polarizing films (“HLC2-5618S” manufactured by Sanritz, 180 μm in thickness, and a polarizing element having a polarizing transmission axis in the width direction) were prepared and placed on a cross Nicol. Cross Nicol means that the polarization transmission axis is vertical when viewed from the thickness direction. Between these polarizing films, the optical film obtained in Example 4 is placed on the polarizing transmission axis of the polarizing film on the viewing side (that is, the polarizing film on the viewing side when installed in a backlight described later) and the slow axis of the optical film. It was installed so that it matches. A polarizing film and an optical film were bonded to each other via an adhesive layer (“CS9621” manufactured by Nitto Denko) to obtain a laminated body.
前記の実施例及び比較例の結果を、下記の表に示す。下記の表において、略称の意味は、下記の通りである。
SPS:結晶性ポリスチレン。
PPE:ポリフェニレンエーテル。
Cy:シクロヘキサン。
Tl:トルエン。 [result]
The results of the above-mentioned Examples and Comparative Examples are shown in the table below. In the table below, the meanings of the abbreviations are as follows.
SPS: Crystalline polystyrene.
PPE: Polyphenylene ether.
Cy: Cyclohexane.
Tl: Toluene.
実施例においては、負の固有複屈折を有する結晶性重合体として結晶性ポリスチレンを用いて、光学フィルムを製造している。当該光学フィルムを製造するために延伸前フィルムを自由一軸延伸したとき、いずれの実施例でも延伸方向に垂直な方向に遅相軸が発現していることから、得られた光学フィルムが負の複屈折特性を有していることが確認できる。また、実施例で得られた光学フィルムは、いずれも、式(1)を満たす面内レターデーションを有し、且つ、式(2)を満たすNZ係数を有する。 [examination]
In the examples, crystalline polystyrene is used as the crystalline polymer having negative intrinsic birefringence to produce an optical film. When the pre-stretched film was freely uniaxially stretched to produce the optical film, the delayed phase axis was developed in the direction perpendicular to the stretching direction in all the examples, so that the obtained optical film was negatively birefringent. It can be confirmed that it has a refraction characteristic. Further, all of the optical films obtained in the examples have an in-plane retardation satisfying the formula (1) and an NZ coefficient satisfying the formula (2).
よって、実施例1~3の光学フィルムは、広い波長範囲において1/4波長板として機能できる。したがって、その光学フィルムを備える円偏光板は、反射抑制フィルムとして広い波長範囲の光の反射を抑制できる。そのため、一部の波長の光が円偏光板を通過することによる色味付きを抑制できる。
また、実施例4の光学フィルムは、広い波長範囲において1/2波長板として機能できる。したがって、その光学フィルムは、当該光学フィルムを透過する広い波長範囲の直線偏光の振動方向を90°変換することができる。そのため、一部の波長の光が積層体を通過することによる色味付き及び光漏れを抑制できる。 Since the optical film obtained in the examples has a reverse wavelength dispersibility, its optical function can be exhibited in a wide wavelength range.
Therefore, the optical films of Examples 1 to 3 can function as a quarter wave plate in a wide wavelength range. Therefore, the circularly polarizing plate provided with the optical film can suppress the reflection of light in a wide wavelength range as a reflection suppressing film. Therefore, it is possible to suppress the coloring caused by the light of a part of the wavelength passing through the circularly polarizing plate.
Further, the optical film of Example 4 can function as a 1/2 wave plate in a wide wavelength range. Therefore, the optical film can convert the vibration direction of linearly polarized light in a wide wavelength range transmitted through the optical film by 90 °. Therefore, it is possible to suppress coloring and light leakage due to the passage of light having a part of wavelengths through the laminate.
よって、実施例1~3の光学フィルムは、傾斜方向に円偏光板を透過する光の反射を抑制できるので、正面方向だけでなく傾斜方向においても色味付きを抑制できる。
また、実施例4の光学フィルムは、傾斜方向における積層体の光の通過を抑制できるので、正面方向だけでなく傾斜方向においても色味付き及び光漏れを抑制できる。 Further, since the optical film obtained in the examples has an appropriate NZ coefficient, not only the light transmitted through the optical film in the thickness direction but also the polarization of the light transmitted in the inclined direction which is neither parallel nor perpendicular to the thickness direction. The state can also be changed appropriately.
Therefore, since the optical films of Examples 1 to 3 can suppress the reflection of the light transmitted through the circularly polarizing plate in the tilting direction, the tinting can be suppressed not only in the front direction but also in the tilting direction.
Further, since the optical film of Example 4 can suppress the passage of light of the laminated body in the inclined direction, it is possible to suppress coloring and light leakage not only in the front direction but also in the inclined direction.
Claims (11)
- 結晶性重合体を含む光学フィルムであって、
前記光学フィルムが、負の複屈折特性を有し、
前記光学フィルムの測定波長450nm、550nm及び650nmにおける面内レターデーションRe(450)、Re(550)及びRe(650)が式(1)を満たし、
前記光学フィルムのNZ係数Nzが、式(2)を満たす、光学フィルム。
Re(450)<Re(550)<Re(650) (1)
0<Nz<1 (2) An optical film containing a crystalline polymer,
The optical film has a negative birefringence characteristic and
The in-plane retardations Re (450), Re (550) and Re (650) of the optical film at the measurement wavelengths of 450 nm, 550 nm and 650 nm satisfy the formula (1).
An optical film in which the NZ coefficient Nz of the optical film satisfies the formula (2).
Re (450) <Re (550) <Re (650) (1)
0 <Nz <1 (2) - 前記光学フィルムが、単層構造を有する、請求項1に記載の光学フィルム。 The optical film according to claim 1, wherein the optical film has a single-layer structure.
- 前記光学フィルムが、延伸フィルムである、請求項1又は2に記載の光学フィルム。 The optical film according to claim 1 or 2, wherein the optical film is a stretched film.
- 前記光学フィルムが、一軸延伸フィルムである、請求項1~3のいずれか一項に記載の光学フィルム。 The optical film according to any one of claims 1 to 3, wherein the optical film is a uniaxially stretched film.
- 前記光学フィルムが、長尺の形状を有する、請求項1~4のいずれか一項に記載の光学フィルム。 The optical film according to any one of claims 1 to 4, wherein the optical film has a long shape.
- 負の固有複屈折を有する前記結晶性重合体と、正の固有複屈折を有する熱可塑性重合体と、を含む樹脂からなる、請求項1~5のいずれか一項に記載の光学フィルム。 The optical film according to any one of claims 1 to 5, comprising a resin containing the crystalline polymer having a negative intrinsic birefringence and a thermoplastic polymer having a positive intrinsic birefringence.
- 正の固有複屈折を有する前記熱可塑性重合体と負の固有複屈折を有する前記結晶性重合体との重量比(熱可塑性重合体/結晶性重合体)が、3/7以上である、請求項6に記載の光学フィルム。 Claimed that the weight ratio (thermoplastic polymer / crystalline polymer) of the thermoplastic polymer having a positive intrinsic compound refraction to the crystalline polymer having a negative intrinsic compound refraction is 3/7 or more. Item 6. The optical film according to Item 6.
- 負の固有複屈折を有する前記結晶性重合体が、ポリスチレン系重合体であり、
正の固有複屈折を有する前記熱可塑性重合体が、ポリフェニレンエーテルである、請求項6又は7に記載の光学フィルム。 The crystalline polymer having a negative intrinsic birefringence is a polystyrene-based polymer.
The optical film according to claim 6 or 7, wherein the thermoplastic polymer having positive intrinsic birefringence is a polyphenylene ether. - 請求項1~8のいずれか一項に記載の光学フィルムと、偏光フィルムと、を備える偏光板。 A polarizing plate comprising the optical film according to any one of claims 1 to 8 and a polarizing film.
- 前記光学フィルムの遅相軸と、前記偏光フィルムの吸収軸と、が80°~100°の角度をなす、請求項9に記載の偏光板。 The polarizing plate according to claim 9, wherein the slow axis of the optical film and the absorption axis of the polarizing film form an angle of 80 ° to 100 °.
- 請求項1~8のいずれか一項に記載の光学フィルムの製造方法であって、
負の固有複屈折を有する結晶性重合体と、正の固有複屈折を有する熱可塑性重合体と、を含む樹脂からなる樹脂フィルムを用意する工程と、
前記樹脂フィルムを、溶媒に接触させて、厚み方向の複屈折を変化させる工程と、
前記樹脂フィルムを延伸する工程と、をこの順に含む、光学フィルムの製造方法。 The method for manufacturing an optical film according to any one of claims 1 to 8.
A step of preparing a resin film made of a resin containing a crystalline polymer having a negative intrinsic birefringence and a thermoplastic polymer having a positive intrinsic birefringence.
The step of bringing the resin film into contact with a solvent to change the birefringence in the thickness direction,
A method for producing an optical film, comprising the steps of stretching the resin film in this order.
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JP2003161832A (en) * | 2001-11-22 | 2003-06-06 | Fuji Photo Film Co Ltd | Retardation plate |
JP2007191505A (en) * | 2006-01-17 | 2007-08-02 | Fujifilm Corp | Cellulose acylate film, polarizing plate and liquid crystal display device |
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JP2015157928A (en) * | 2013-06-07 | 2015-09-03 | 東ソー株式会社 | Resin composition and optical compensation film employing the same |
JP2016079377A (en) * | 2014-10-15 | 2016-05-16 | 東ソー株式会社 | Resin composition and optical compensation film |
WO2019188205A1 (en) * | 2018-03-30 | 2019-10-03 | 日本ゼオン株式会社 | Optical anisotropic layered body, polarizing plate, and image display device |
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JP2003161832A (en) * | 2001-11-22 | 2003-06-06 | Fuji Photo Film Co Ltd | Retardation plate |
JP2007191505A (en) * | 2006-01-17 | 2007-08-02 | Fujifilm Corp | Cellulose acylate film, polarizing plate and liquid crystal display device |
JP2015157928A (en) * | 2013-06-07 | 2015-09-03 | 東ソー株式会社 | Resin composition and optical compensation film employing the same |
US20150042928A1 (en) * | 2013-08-09 | 2015-02-12 | Samsung Display Co., Ltd. | Display device |
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