CN113189692A - Method for manufacturing polarizing plate - Google Patents
Method for manufacturing polarizing plate Download PDFInfo
- Publication number
- CN113189692A CN113189692A CN202110494521.7A CN202110494521A CN113189692A CN 113189692 A CN113189692 A CN 113189692A CN 202110494521 A CN202110494521 A CN 202110494521A CN 113189692 A CN113189692 A CN 113189692A
- Authority
- CN
- China
- Prior art keywords
- polarizing plate
- crosslinking
- film
- polyvinyl alcohol
- dyeing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 56
- 238000000034 method Methods 0.000 title claims description 41
- 238000004132 cross linking Methods 0.000 claims description 57
- 238000004043 dyeing Methods 0.000 claims description 41
- 230000008961 swelling Effects 0.000 claims description 22
- 230000001186 cumulative effect Effects 0.000 claims description 16
- 239000012790 adhesive layer Substances 0.000 abstract description 37
- 230000001681 protective effect Effects 0.000 abstract description 33
- 239000004372 Polyvinyl alcohol Substances 0.000 description 64
- 229920002451 polyvinyl alcohol Polymers 0.000 description 64
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 53
- 229920005989 resin Polymers 0.000 description 52
- 239000011347 resin Substances 0.000 description 52
- 239000000853 adhesive Substances 0.000 description 35
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- 239000000203 mixture Substances 0.000 description 32
- 229910052740 iodine Inorganic materials 0.000 description 30
- 239000011630 iodine Substances 0.000 description 30
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 26
- 239000007864 aqueous solution Substances 0.000 description 26
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 24
- 230000003287 optical effect Effects 0.000 description 21
- -1 polyethylene terephthalate Polymers 0.000 description 21
- 238000001035 drying Methods 0.000 description 19
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- 239000003431 cross linking reagent Substances 0.000 description 16
- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical compound OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 description 16
- 125000002339 acetoacetyl group Chemical group O=C([*])C([H])([H])C(=O)C([H])([H])[H] 0.000 description 14
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 14
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 13
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- 238000006243 chemical reaction Methods 0.000 description 6
- WASQWSOJHCZDFK-UHFFFAOYSA-N diketene Chemical compound C=C1CC(=O)O1 WASQWSOJHCZDFK-UHFFFAOYSA-N 0.000 description 6
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
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- 229920002284 Cellulose triacetate Polymers 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 2
- MBHRHUJRKGNOKX-UHFFFAOYSA-N [(4,6-diamino-1,3,5-triazin-2-yl)amino]methanol Chemical compound NC1=NC(N)=NC(NCO)=N1 MBHRHUJRKGNOKX-UHFFFAOYSA-N 0.000 description 2
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- UAYWVJHJZHQCIE-UHFFFAOYSA-L zinc iodide Chemical compound I[Zn]I UAYWVJHJZHQCIE-UHFFFAOYSA-L 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
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- 238000012935 Averaging Methods 0.000 description 1
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- UNMYWSMUMWPJLR-UHFFFAOYSA-L Calcium iodide Chemical compound [Ca+2].[I-].[I-] UNMYWSMUMWPJLR-UHFFFAOYSA-L 0.000 description 1
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- 208000005156 Dehydration Diseases 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
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- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229920001893 acrylonitrile styrene Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
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- 239000003513 alkali Substances 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
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- CECABOMBVQNBEC-UHFFFAOYSA-K aluminium iodide Chemical compound I[Al](I)I CECABOMBVQNBEC-UHFFFAOYSA-K 0.000 description 1
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- 150000007860 aryl ester derivatives Chemical class 0.000 description 1
- SGUXGJPBTNFBAD-UHFFFAOYSA-L barium iodide Chemical compound [I-].[I-].[Ba+2] SGUXGJPBTNFBAD-UHFFFAOYSA-L 0.000 description 1
- 229910001638 barium iodide Inorganic materials 0.000 description 1
- 229940075444 barium iodide Drugs 0.000 description 1
- HAQRWNBBZAGEJU-UHFFFAOYSA-L barium(2+);oxaldehydate Chemical compound [Ba+2].[O-]C(=O)C=O.[O-]C(=O)C=O HAQRWNBBZAGEJU-UHFFFAOYSA-L 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 229910001640 calcium iodide Inorganic materials 0.000 description 1
- 229940046413 calcium iodide Drugs 0.000 description 1
- JIOBOQOAYFOKLJ-UHFFFAOYSA-L calcium;oxaldehydate Chemical compound [Ca+2].[O-]C(=O)C=O.[O-]C(=O)C=O JIOBOQOAYFOKLJ-UHFFFAOYSA-L 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
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- GBRBMTNGQBKBQE-UHFFFAOYSA-L copper;diiodide Chemical compound I[Cu]I GBRBMTNGQBKBQE-UHFFFAOYSA-L 0.000 description 1
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- AHPWAMGCMMEWNF-UHFFFAOYSA-L magnesium;oxaldehydate Chemical compound [Mg+2].[O-]C(=O)C=O.[O-]C(=O)C=O AHPWAMGCMMEWNF-UHFFFAOYSA-L 0.000 description 1
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- 238000007760 metering rod coating Methods 0.000 description 1
- JTHNLKXLWOXOQK-UHFFFAOYSA-N n-propyl vinyl ketone Natural products CCCC(=O)C=C JTHNLKXLWOXOQK-UHFFFAOYSA-N 0.000 description 1
- 125000003518 norbornenyl group Chemical group C12(C=CC(CC1)C2)* 0.000 description 1
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- 230000002093 peripheral effect Effects 0.000 description 1
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- 229920001643 poly(ether ketone) Polymers 0.000 description 1
- 229920001483 poly(ethyl methacrylate) polymer Polymers 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
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- 125000003367 polycyclic group Chemical group 0.000 description 1
- 229920001690 polydopamine Polymers 0.000 description 1
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- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- WOTCTOFEBNHWND-UHFFFAOYSA-M potassium;oxaldehydate Chemical compound [K+].[O-]C(=O)C=O WOTCTOFEBNHWND-UHFFFAOYSA-M 0.000 description 1
- SCUZVMOVTVSBLE-UHFFFAOYSA-N prop-2-enenitrile;styrene Chemical compound C=CC#N.C=CC1=CC=CC=C1 SCUZVMOVTVSBLE-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 235000009518 sodium iodide Nutrition 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- QPBYLOWPSRZOFX-UHFFFAOYSA-J tin(iv) iodide Chemical compound I[Sn](I)(I)I QPBYLOWPSRZOFX-UHFFFAOYSA-J 0.000 description 1
- NLLZTRMHNHVXJJ-UHFFFAOYSA-J titanium tetraiodide Chemical compound I[Ti](I)(I)I NLLZTRMHNHVXJJ-UHFFFAOYSA-J 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
- G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
- G02B5/3041—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks
- G02B5/305—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks including organic materials, e.g. polymeric layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2329/00—Polyvinylalcohols, polyvinylethers, polyvinylaldehydes, polyvinylketones or polyvinylketals
- B32B2329/04—Polyvinylalcohol
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Polarising Elements (AREA)
- Liquid Crystal (AREA)
- Laminated Bodies (AREA)
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention provides a polarizing plate comprising: a polarizing plate having a mean spacing between irregularities (RSm) of 500 to 5000 μm and a maximum height roughness (Rt) of 100 to 1000 nm; an adhesive layer having a thickness of 250 to 850nm formed on at least one surface of the polarizer; and a protective film laminated on the adhesive layer.
Description
The present application is a divisional application of an invention patent application having an application date of 2016, 8/17, an application number of 201680045107.5, and an invention name of "polarizing plate and method for manufacturing the same".
Technical Field
The present invention relates to a polarizing plate excellent in both optical characteristics and appearance characteristics, a method for manufacturing the same, and an image display device including the polarizing plate.
Background
Image display devices are electronic products that are commonly used, such as watches, mobile phones, PDAs, notebook computers, PC monitors, DVD players, TVs, and the like. A polarizing plate is used as a basic component of an image display device.
In the production of a polarizing plate, if the stretching ratio is increased in order to improve the orientation of the iodine complex of the polarizer for the purpose of improving the performance of the polarizing plate, the width of the polarizer is reduced, and appearance defects such as unevenness of a stripe pattern are generated in the polarizing plate.
Here, patent document 1 (korean laid-open patent No. 2014-0114923) discloses a technique of improving a contact angle and appearance defects by using an adhesive composition produced by adding a leveling agent having an acetylene skeleton.
However, even with this method, it is not possible to improve the appearance defects of the polarizing plate and maintain the required excellent optical characteristics.
Documents of the prior art
Patent document
Patent document 1: korean laid-open patent No. 2014-0114923
Disclosure of Invention
Problems to be solved by the invention
The present invention aims to provide a polarizing plate capable of preventing appearance defects without reducing optical characteristics such as transmittance and polarization degree, and an image display device including the polarizing plate.
Another object of the present invention is to provide a polarizing plate having excellent physical properties such as adhesiveness, water resistance, moisture resistance, and heat resistance (hereinafter, moisture resistance and heat resistance are collectively referred to as "moist heat resistance"), and an image display device including the polarizing plate.
Means for solving the problems
1. A polarizing plate, comprising: a polarizing plate having a mean spacing between irregularities (RSm) of 500 to 5000 μm and a maximum height roughness (Rt) of 100 to 1000 nm; an adhesive layer having a thickness of 250 to 850nm formed on at least one surface of the polarizer; and a protective film laminated on the adhesive layer.
2. The polarizing plate of claim 1, wherein the adhesive layer has a thickness of 300 to 800 nm.
3. The polarizing plate according to claim 1, wherein the adhesive layer is formed of an adhesive composition containing a polyvinyl alcohol resin containing an acetoacetyl group and a glyoxylate crosslinking agent.
4. A method of manufacturing a polarizing plate, the method comprising: (i) a step of manufacturing a polarizing plate having a concave-convex average spacing (RSm) of 500 to 5000 μm and a maximum height roughness (Rt) of 100 to 1000 nm; (ii) a step of applying an adhesive composition to at least one of the polarizing plate and the protective film to form an adhesive layer of 250 to 850 nm; and (iii) a step of bonding the polarizing plate and the protective film with the adhesive layer interposed therebetween.
5. The method for manufacturing a polarizing plate according to the above 4, wherein the adhesive composition comprises a polyvinyl alcohol resin containing an acetoacetyl group, and a glyoxylate crosslinking agent.
6. The method for manufacturing a polarizing plate according to 5, wherein the acetoacetyl group-containing polyvinyl alcohol resin and the glyoxylate crosslinking agent are contained in a total amount of 2.5 to 6 wt% based on the total weight of the adhesive composition on a solid content basis.
7. The method of manufacturing a polarizing plate according to item 4 above, wherein a bonding speed of bonding the polarizer and the protective film is 10 to 35 m/min.
8. An image display device comprising the polarizing plate of any one of 1 to 3 above.
Effects of the invention
The polarizing plate of the present invention has no deterioration in optical characteristics such as transmittance and polarization degree, and has significantly less appearance defects such as unevenness of fringe patterns.
The polarizing plate of the present invention can have excellent adhesiveness, water resistance, and moist heat resistance.
According to the method for manufacturing a polarizing plate of the present invention, the range in which a polarizer can be used can be widened, the fraction defective can be reduced, an additional process for removing the defect is not required, and convenience, high efficiency, and economy can be secured in the manufacturing process.
Drawings
Fig. 1 is a photograph for analyzing the surface of a polarizing plate manufactured in a manufacturing example of the present invention.
Fig. 2 is a diagram schematically showing a method for testing the water resistance of the polarizing plate of the present invention.
Detailed Description
< polarizing plate >
One embodiment of the present invention relates to a polarizing plate comprising a polarizer having a concave-convex average spacing (RSm) of 500 to 5000 μm and a maximum height roughness (Rt) of 100 to 1000 nm; an adhesive layer having a thickness of 250 to 850nm formed on at least one surface of the polarizer; and a protective film laminated on the adhesive layer, whereby the optical characteristics and appearance characteristics are excellent.
< polarizing plate >
The polarizing plate of the present invention comprises a polarizer having a concave-convex average spacing (RSm) of 500 to 5000 μm and a maximum height roughness (Rt) of 100 to 1000 nm.
The average spacing between irregularities (RSm) is a value defined in ISO 4287-1997, and is a value obtained by extracting a reference length from the roughness curve in the direction of the average line, obtaining the sum of the lengths of the average lines corresponding to 1 mountain and 1 valley adjacent thereto, and averaging the sum over the reference length. The average concave-convex interval (RSm) corresponds to a distance defined by JIS B0601: 2013, the average length (RSm) of the elements of the roughness curve.
The maximum height roughness (Rt) is a value specified by ISO 4287-1997 and refers to the sum of the maximum value of the mountain height and the maximum value of the valley depth of the roughness curve in the reference length. The maximum height roughness (Rt) corresponds to a roughness measured in accordance with JIS B0601: 2013, the maximum cross-sectional height (Rt) of the roughness curve.
By providing the polarizing plate of the present invention with RSm and Rt in the above-mentioned specific ranges, a polarizing plate having excellent optical characteristics and appearance characteristics can be produced. If RSm is less than 500. mu.m, the optical characteristics are deteriorated, and if RSm is more than 5000. mu.m, the appearance is not improved. Further, if Rt is less than 100nm, there is a problem that optical characteristics are deteriorated, and if it exceeds 1000nm, there is a problem that appearance defects cannot be improved. From the viewpoint of further improving the optical properties and further improving the appearance defects, it is preferable that RSm is 750 to 5000 μm and Rt is 120 to 970 nm.
< adhesive layer >
The polarizing plate of the present invention includes an adhesive layer having a thickness of 250 to 850nm on at least one side of the polarizer.
When the polarizing plate having the above-described RSm and Rt ranges of the present invention is used in the production of a polarizing plate by a general method, the polarizing plate may have uneven fringe patterns. Therefore, in the present invention, by introducing the adhesive layer having the thickness in the above-described specific range, the unevenness of the stripe pattern of the polarizing plate is remarkably reduced without lowering the optical characteristics such as the degree of polarization or the transmittance. If the thickness of the adhesive layer is less than 250nm, the appearance defects cannot be improved, and if it exceeds 850nm, the optical characteristics are deteriorated. The thickness of the adhesive layer is more preferably 300 to 800nm from the viewpoint of further reducing the unevenness of the fringe pattern of the polarizing plate without lowering the optical characteristics.
The method for increasing the thickness of the adhesive layer is not particularly limited, and for example, a method of increasing the concentration of solid components in the adhesive composition or a method of increasing the bonding speed of bonding the polarizing plate and the protective film via the adhesive layer may be used.
< protective film >
The protective film of the present invention is not particularly limited as long as it is a film excellent in transparency, mechanical strength, thermal stability, water resistance, isotropy, and the like, and specific examples thereof include films made of polyester resins such as polyethylene terephthalate, polyethylene isophthalate, and polybutylene terephthalate; cellulose resins such as diacetylcellulose, triacetylcellulose, and cellulose acetate propionate; a polycarbonate-based resin; polyacrylic resins such as polymethyl (meth) acrylate and polyethyl (meth) acrylate; styrene resins such as polystyrene and acrylonitrile-styrene copolymer; polyolefin resins such as polyethylene, polypropylene, polyolefins having a cyclic or norbornene structure, and ethylene-propylene copolymers; polyamide resins such as nylon and aromatic polyamide; an imide-based resin; a polyether sulfone-based resin; a sulfone-based resin; a polyether ketone resin; polyphenylene sulfide-based resin; a vinyl alcohol resin; a vinylidene chloride resin; a vinyl butyral resin; an aryl ester-based resin; a polyoxymethylene resin; a film made of a thermoplastic resin such as an epoxy resin may be used as well as a film made of a blend of the above thermoplastic resins. Further, a film containing a thermosetting resin or an ultraviolet-curable resin such as (meth) acrylic, urethane, epoxy, or silicon may be used.
When a cycloolefin resin is used for the protective film, a cycloolefin resin known in the art can be used without particular limitation. For example, the cycloolefin resin may be a thermoplastic resin having a monomer unit of a cycloolefin such as a norbornene or polycyclic norbornene monomer, a hydrogenated product of a ring-opened polymer of the above cycloolefin or a ring-opened copolymer using 2 or more kinds of the above cycloolefins, or an addition copolymer of a cycloolefin and a chain olefin or an aromatic compound having a vinyl group. Further, a polar group may be introduced into the cycloolefin resin.
Among the above resins, a film made of a cellulose-based resin, a polyolefin-based resin, or a polyacrylic resin is preferable in view of polarization characteristics and durability.
< method for producing polarizing plate >
Another embodiment of the present invention relates to a method for manufacturing a polarizing plate, including: a step of manufacturing a polarizing plate having a concave-convex average spacing (RSm) of 500 to 5000 μm and a maximum height roughness (Rt) of 100 to 1000 nm; a step of applying an adhesive composition to at least one surface of the polarizing plate or the protective film to form an adhesive layer of 250 to 850 nm; and a step of bonding the polarizing plate and the protective film with the adhesive layer interposed therebetween.
Hereinafter, the method for producing the polarizing plate of the present invention will be described in more detail.
First, a polarizing plate (i) having an average space between irregularities (RSm) of 500 to 5000 μm and a maximum height roughness (Rt) of 100 to 1000nm was produced.
In order to make the polarizing plate have the above-mentioned specific RSm and Rt ranges, the conditions of the manufacturing process of the polarizing plate may be adjusted. For example, the draw ratio, drying time, etc. may be adjusted. An example of the method for producing a polarizing plate of the present invention will be specifically described below.
The polymer film used for producing the polarizer is not particularly limited as long as it is a polymer film used for producing a polarizing plate, and a film dyeable with a dichroic substance (e.g., iodine) known in the art may be used, and for example, a polyvinyl alcohol film or a partially saponified polyvinyl alcohol film; hydrophilic polymer films such as polyethylene terephthalate films, ethylene-vinyl acetate copolymer films, ethylene-vinyl alcohol copolymer films, cellulose films, and partially saponified films thereof; or a polyene-oriented film such as a polyvinyl alcohol film subjected to dehydration treatment, a polyvinyl chloride film subjected to desalting treatment, or the like; and the like. Among them, a polyvinyl alcohol film is preferable in that it is excellent not only in the effect of enhancing uniformity of the degree of polarization in the plane but also in the dyeing affinity for iodine.
The method for manufacturing the polarizing plate may include a swelling step, a dyeing step, a crosslinking step, a color complementing step, a stretching step, a water washing step, and a drying step, and may be classified by a stretching method. Examples thereof include a dry stretching method, a wet stretching method, and a hybrid stretching method in which the above 2 stretching methods are mixed. The method for producing the polarizing plate of the present invention will be described below by taking a wet stretching method as an example, but the method is not limited thereto.
The remaining steps except the drying step among the above steps may be performed in a state in which the polyvinyl alcohol film is immersed in a constant-temperature water bath (bath) filled with 1 or more kinds of solutions selected from various solutions.
< swelling step >
The swelling step is a step of immersing an unstretched polyvinyl alcohol film in a swelling tank filled with an aqueous swelling solution before dyeing, and removing impurities such as dust and an anti-blocking agent deposited on the surface of the polyvinyl alcohol film to swell the polyvinyl alcohol film, thereby improving the stretching efficiency, preventing dyeing unevenness, and improving the physical properties of the polarizing plate.
The aqueous solution for swelling may be any one known in the art, and for example, water (pure water or deionized water) may be used alone, and when a small amount of glycerin or potassium iodide is added thereto, the polymer film can be swollen and the processability can be improved. The content of glycerin may be 5 wt% or less and the content of potassium iodide may be 10 wt% or less with respect to 100 wt% of the aqueous swelling solution, but is not limited thereto.
The temperature of the swelling bath is not particularly limited, and may be 20 to 45 ℃, for example, 25 to 40 ℃.
The execution time of the swelling step (swelling bath immersion time) may be any one known in the art without particular limitation, and may be, for example, 180 seconds or less, preferably 90 seconds or less. When the immersion time is within the above range, swelling is suppressed from becoming excessively saturated, and breakage due to softening of the polyvinyl alcohol film is prevented, so that iodine adsorption in the dyeing step becomes uniform, and the degree of polarization is improved.
The stretching step may be carried out simultaneously with the swelling step, and in this case, the stretching ratio may be about 1.1 to 3.5 times, without limitation, and may preferably be 1.5 to 3.0 times. If the stretching ratio is less than 1.1 times, wrinkles may be generated, and in the case of more than 3.5 times, the initial optical characteristics may become weak.
< dyeing step >
The dyeing step is a step of immersing the polyvinyl alcohol film in a dyeing bath filled with an aqueous solution for dyeing containing a dichroic substance such as iodine, and adsorbing iodine to the polyvinyl alcohol film.
The aqueous solution for dyeing may be any aqueous solution for dyeing known in the art without particular limitation, and may contain water, a water-soluble organic solvent or a mixed solvent thereof, and iodine. The content of iodine may be 0.4 to 400mmol/L relative to the aqueous solution for dyeing, however, is not limited thereto, and may be preferably 0.8 to 275mmol/L, and most preferably 1 to 200 mmol/L. In order to improve the dyeing efficiency, an iodide may be further contained as a dissolution assistant. As the iodide, an iodide known in the art may be used without limitation, and for example, at least 1 selected from potassium iodide, lithium iodide, sodium iodide, zinc iodide, aluminum iodide, lead iodide, copper iodide, barium iodide, calcium iodide, tin iodide, and titanium iodide may be contained, and among them, potassium iodide is preferable in view of its high solubility in water. The content of the iodide may be 0.01 to 10% by weight, but is not limited thereto, and may preferably be 0.1 to 5% by weight, relative to 100% by weight of the aqueous solution for dyeing.
In addition, in order to increase the content of the iodine complex in the polyvinyl alcohol film, boric acid may be added to the dyeing bath in an amount of 0.3 to 5% by weight with respect to 100% by weight of the aqueous solution for dyeing, but the present invention is not limited thereto. In the case where the boric acid content of the dyeing bath is less than 0.3% by weight, it is possible for PVA-I3 －Complex and PVA-I5 －The increase in the complex content is not effective, and in the case where the boric acid in the dyeing bath is at a concentration higher than 5% by weight, the risk of film breakage may become high.
The temperature of the dyeing bath may be 5 to 42 ℃, however, is not limited thereto, and may preferably be 10 to 35 ℃. The time for immersing the polyvinyl alcohol film in the dyeing bath is not particularly limited, and may be 1 to 20 minutes, and preferably 2 to 10 minutes.
In the present invention, the stretching step may be carried out simultaneously with the dyeing step, and in this case, the stretching ratio may be 1.01 to 2.0 times, but is not limited thereto, and may preferably be 1.1 to 1.8 times.
In addition, the cumulative stretching ratio up to the dyeing step including the swelling and the dyeing step may be 1.2 to 4.0 times. If the cumulative stretching ratio is less than 1.2 times, wrinkles of the film may occur to cause appearance defects, and if it is more than 4.0 times, the initial optical characteristics may become weak.
< crosslinking step >
The crosslinking step is a step of immersing the dyed polyvinyl alcohol film in an aqueous crosslinking solution so that the dyeing properties of the physically adsorbed iodine molecules are not lowered by the external environment, and immobilizing the adsorbed iodine molecules.
When the crosslinking reaction of iodine as a dichroic dye is insufficient, iodine molecules are separated by a moist heat environment, and thus a sufficient crosslinking reaction is required. In addition, in order to orient the iodine molecules located between the molecules of the polyvinyl alcohol and improve the optical properties, stretching may be performed at the maximum stretching ratio in the crosslinking step, but is not limited thereto.
In the present invention, the method for producing the polarizing plate may be any method known in the art, and for example, a method comprising a first and second crosslinking step may be performed, and an aqueous crosslinking solution containing a boron compound may be used for 1 or more of the first and second crosslinking steps. This can improve the optical characteristics and color durability of the polarizing plate.
The aqueous crosslinking solution may be any aqueous crosslinking solution known in the art, and may include, for example, water as a solvent, and a boron compound such as boric acid or sodium borate, or may further include an organic solvent and an iodide that are mutually soluble together with water.
The boron compound imparts a short crosslinking bond and rigidity to the polarizing plate, and suppresses the formation of wrinkles in the film during the process, thereby improving the handling properties of the film and forming an iodine orientation effect of the polarizing plate.
The content of the boron compound may be applied in a content known in the art, for example, may be 1 to 10% by weight, and may preferably be 2 to 6% by weight, relative to 100% by weight of the crosslinking aqueous solution. When the content is less than 1% by weight, the crosslinking effect of the boron compound is reduced and it becomes difficult to impart rigidity to the polarizing plate, and when the content is more than 10% by weight, the crosslinking reaction of the inorganic crosslinking agent is excessively activated and it becomes difficult to efficiently perform the crosslinking reaction of the organic crosslinking agent.
In the present invention, an iodide may be used in order to maintain uniformity of the in-plane polarization degree of the polarizing plate and to prevent desorption of the stained iodine. The iodide may be the same as the iodide used in the dyeing step, and the content thereof may be 0.05 to 15% by weight with respect to 100% by weight of the crosslinking aqueous solution, but is not limited thereto, and may preferably be 0.5 to 14% by weight. If the content is less than 0.05 wt%, iodine ions in the film may be released to increase the transmittance of the polarizing plate, and if the content is more than 15 wt%, iodine ions in the aqueous solution may penetrate into the film to decrease the transmittance of the polarizing plate.
In the present invention, the temperature of the crosslinking bath may be 20 to 70 ℃, but is not limited thereto. The immersion time of the polyvinyl alcohol film in the crosslinking bath may be 1 second to 15 minutes, but is not limited thereto, and may preferably be 5 seconds to 10 minutes.
The stretching step may be performed simultaneously with the crosslinking step, and in this case, the stretching ratio of the first crosslinking step may be 1.4 to 3.0 times, but is not limited thereto, and may be preferably 1.5 to 2.5 times.
In addition, the stretching ratio of the second crosslinking step may be 1.01 to 2.0 times, but is not limited thereto, and may be preferably 1.2 to 1.8 times.
The cumulative stretching ratio in the first and second crosslinking steps may be 1.5 to 5.0 times, but is not limited thereto, and may preferably be 1.7 to 4.5 times. If the cumulative stretching ratio is less than 1.5 times, the iodine orientation effect may become insufficient, and if it is more than 5.0 times, the film may be broken by excessive stretching, and the productivity may be lowered.
< step of complementing color >
The color complementing step may be a step of aligning the iodine complex located between molecules in the polyvinyl alcohol film physically adsorbed with the iodine complex in proximity to boric acid crosslinking to stabilize the iodine complex.
Further, the color of the polyvinyl alcohol film may be corrected by the step of insufficiently dyeing the iodine complex in the crosslinking step.
The aqueous solution used in the color-compensating step may be any aqueous solution known in the art without particular limitation, and may contain, for example, water as a solvent and a boron compound such as boric acid, or may further contain an organic solvent and an iodide that are mutually soluble together with water.
In the present invention, the boron compound imparts a short crosslinking bond and rigidity to the polarizing plate, and suppresses the formation of wrinkles in the film during the process, thereby improving the handling properties of the film and forming an iodine orientation effect of the polarizing plate.
The content of the boron compound may be 1 to 10% by weight with respect to 100% by weight of the aqueous solution of the complementary color step, but is not limited thereto, and may preferably be 2 to 6% by weight. When the content is less than 1% by weight, the crosslinking effect of the boron compound is reduced and it becomes difficult to impart rigidity to the polarizing plate, and when the content is more than 10% by weight, the crosslinking reaction of the inorganic crosslinking agent is excessively activated and it becomes difficult to efficiently perform the crosslinking reaction of the organic crosslinking agent.
In the present invention, an iodide may be used in order to maintain uniformity of the in-plane polarization degree of the polarizing plate and to prevent desorption of the stained iodine. The iodide may be the same as the iodide used in the dyeing step, and the content thereof may be 0.05 to 15% by weight with respect to 100% by weight of the aqueous solution in the color-compensating step, but is not limited thereto, and may preferably be 0.5 to 11% by weight. If the content is less than 0.05 wt%, iodine ions in the film may be released to increase the transmittance of the polarizing plate, and if the content is more than 15 wt%, iodine ions in the aqueous solution may penetrate into the film to decrease the transmittance of the polarizing plate.
In the present invention, the temperature of the color compensation tank may be 20 to 70 ℃. The immersion time of the polyvinyl alcohol film in the color correction bath may be 1 second to 15 minutes, but is not limited thereto, and may preferably be 5 seconds to 10 minutes.
The stretching step may be performed simultaneously with the complementary color step, and in this case, the stretching ratio of the complementary color step may be 1.01 to 1.1 times, but is not limited thereto, and may be preferably 1.01 to 1.08 times.
If the stretching ratio is less than 1.01 times, the effect of stabilizing the iodine complex may be insufficient, and if it is more than 1.1 times, the film may be broken by excessive stretching, and the productivity may be lowered.
< stretching step >
In the present invention, the stretching step may be performed simultaneously with other steps as described above, or may be performed separately.
The stretching step may be performed at least 1 time, or may be performed a plurality of times. When the polarizing plate is produced a plurality of times, the polarizing plate may be produced separately in an arbitrary step in the production process of the polarizing plate.
In the present invention, the adjustment may be made by increasing the stretching ratio to increase Rt and decreasing the stretching ratio to decrease Rt. The adjustment may be made by increasing the stretch ratio to increase RSm and decreasing the stretch ratio to decrease RSm.
In the production method of the present invention, the total cumulative stretching ratio of the polarizing plate is preferably 4.0 to 7.0 times, more preferably 5.3 to 6.5 times.
In the present specification, the "cumulative stretch ratio" may include a value of a product of the stretch ratios in the respective steps.
< Water washing step >
The polyvinyl alcohol film after the crosslinking and stretching may be immersed in a washing tank filled with a washing aqueous solution to remove unnecessary residues such as boric acid adhering to the polyvinyl alcohol film in the step before the washing step.
In the present invention, the aqueous washing solution may be any aqueous washing solution known in the art, and may be, for example, water, or an iodide may be further added thereto, but is not limited thereto.
In the present invention, the temperature of the rinsing bath may be 10 to 60 ℃, but is not limited thereto, and may be preferably 15 to 40 ℃.
The water washing step may be omitted or may be carried out at the end of each step before the water washing step such as the dyeing step or the crosslinking step. The repetition may be performed 1 or more times, and the number of repetitions is not particularly limited.
< drying step >
In the present invention, the drying step of the method for producing a polarizing plate is a step of drying the polyvinyl alcohol-based film washed with water, and further improving the orientation of the dyed iodine molecules by utilizing the neck-in caused by the drying, thereby obtaining a polarizing plate having excellent optical characteristics. The neck-in refers to a narrowing of the width of the film.
As the drying method, a drying method known in the art may be used without limitation, and for example, a method such as natural drying, air drying, heat drying, far-infrared drying, microwave drying, hot air drying, and the like may be used, and for example, hot air drying may be performed at 20 to 100 ℃ for 1 to 10 minutes. The drying temperature may be lowered to prevent deterioration of the polarizing plate, but is not limited thereto, and may be preferably 100 ℃.
In the present invention, the drying time can be adjusted by increasing Rt to increase it and by decreasing Rt to decrease it. Further, the drying time may be adjusted to be longer to increase RSm and shorter to decrease RSm.
After the polarizing plate is manufactured by the above-described method, the adhesive composition is applied to at least one of the polarizing plate and the protective film to form the adhesive layer (ii) having a thickness of 250 to 850 nm.
The adhesive layer may be formed using an adhesive composition known in the art without particular limitation, and for example, an aqueous adhesive composition may be used, and an adhesive composition containing a polyvinyl alcohol resin containing an acetoacetyl group and a crosslinking agent of glyoxylate may be used as the aqueous adhesive composition in order to improve water resistance.
< acetoacetyl-modified polyvinyl alcohol resin >
The acetoacetyl (acetoacetyl) based modified polyvinyl alcohol (PVA) based resin can improve the adhesion between a polyvinyl alcohol (PVA) based polarizing plate and a protective film such as a cellulose based film or an olefin based film.
In the present invention, the acetoacetyl-modified polyvinyl alcohol (PVA) -based resin contains a functional group having higher reactivity than a modified polyvinyl alcohol resin such as a carboxyl-modified polyvinyl alcohol resin, a hydroxymethyl-modified polyvinyl alcohol resin, or an amino-modified polyvinyl alcohol resin, and is excellent in terms of improvement in durability.
The acetoacetyl group-modified polyvinyl alcohol resin may be used and produced by any method known in the art without particular limitation, and for example, an acetoacetyl group-modified polyvinyl alcohol resin may be obtained by reacting a polyvinyl alcohol resin with diketene (diketene) by a known method. For example, a method of dispersing a polyvinyl alcohol resin in a solvent such as acetic acid and then adding diketene thereto; a method in which a polyvinyl alcohol resin is dissolved in a solvent such as dimethylformamide or dioxane in advance, and then diketene is added thereto; or a method in which a diketene gas or a diketene liquid is directly contacted with a polyvinyl alcohol resin, to produce an acetoacetyl-modified polyvinyl alcohol resin. The acetoacetyl group-modified polyvinyl alcohol resin is not particularly limited as long as the acetoacetyl group modification degree is 0.1 mol% or more, and may be, for example, 0.1 to 40 mol%, preferably 1 to 20 mol%, and most preferably 2 to 7 mol%. If the modification degree of the acetoacetyl group is less than 0.1 mol%, the water resistance of the adhesive layer may be insufficient and unsuitable, and if the modification degree of the acetoacetyl group is more than 40 mol%, the effect of improving the water resistance may be insufficient.
In the present invention, the saponification degree of the acetoacetyl-modified polyvinyl alcohol resin is not particularly limited, and may be 80 mol% or more, and preferably 85 mol% or more. If the polyvinyl alcohol resin contained in the adhesive composition has a low saponification degree, the adhesive composition is difficult to exhibit sufficient water solubility, and thus the adhesiveness is insufficient.
The polyvinyl alcohol used in the production of the acetoacetyl-modified polyvinyl alcohol resin is not particularly limited, but in order to exhibit high adhesiveness between the polarizer and the protective film in the polarizing plate, the average polymerization degree may be in the range of 100 to 3000, and the average saponification degree may preferably be in the range of 80 to 100 mol%.
Examples of the acetoacetyl-modified polyvinyl alcohol resin product include Z-100, Z-200H, Z-210, Z-220, and Z-320 (Gohsefimer, Japan synthetic chemical Co., Ltd.).
< glyoxylate crosslinking agent >
In the present invention, the glyoxylate crosslinking agent contained in the adhesive composition of the method for producing a polarizing plate can improve the adhesion between the acetoacetyl (acetoacetyl) modified polyvinyl alcohol (PVA) resin and a protective film such as a polyvinyl alcohol (PVA) polarizing plate, a cellulose-based film, an olefin-based film, or the like.
The glyoxylate may be an alkali metal salt or an alkaline earth metal salt of glyoxylic acid. In the present invention, the same effect can be obtained when either one of the alkali metal salt of glyoxylic acid and the alkaline earth metal salt is used. The reason is not bound by any theory, however, because the alkali metal and the alkaline earth metal are both elements with small electronegativity, the chemical properties of the carboxylate are similar, and the aldehyde part of the glyoxylate functions as a crosslinking agent of the acetoacetyl-modified polyvinyl alcohol.
The glyoxylate may be any one known in the art, and examples thereof include alkali metal salts such as lithium glyoxylate, sodium glyoxylate, and potassium glyoxylate, and alkaline earth metal salts such as magnesium glyoxylate, calcium glyoxylate, strontium glyoxylate, and barium glyoxylate. Among them, alkali metal salts are preferable because they are easily dissolved in water, and sodium glyoxylate is particularly preferable.
The glyoxylate may be in a range of 3 to 25 parts by weight with respect to 100 parts by weight of the acetoacetyl group-containing polyvinyl alcohol-based resin. When the weight ratio of the glyoxylate to 100 parts by weight of the polyvinyl alcohol resin is 3 parts by weight or less, it is difficult to sufficiently exhibit the water resistance of the adhesive layer when the polarizing plate is produced, and when the weight ratio of the glyoxylate to 100 parts by weight of the polyvinyl alcohol resin is more than 25 parts by weight, the optical properties of the polarizing plate may be deteriorated.
The thickness of the adhesive layer of the present invention can be adjusted by adjusting the concentration of the solid component in the adhesive composition, for example. For example, the total amount of the acetoacetyl group-containing polyvinyl alcohol resin and the glyoxylate crosslinking agent may be contained in an amount of 2.5 to 6% by weight, preferably 3 to 5% by weight, based on the total weight of the adhesive composition, based on the solid content. If the thickness is within the above range, the thickness of the adhesive layer can be adjusted to the range of the thickness of the adhesive layer in the polarizing plate of the present invention.
In the present invention, the adhesive composition can be used with a pH in the range of 4 to 10. When the pH of the aqueous solution is less than 4, the water resistance of the polarizing plate cannot be sufficiently exhibited when the polarizing plate is manufactured using the aqueous solution, and when the pH of the aqueous solution is more than 10, the adhesive composition may be gelled.
The adhesive composition may have a viscosity at 20 ℃ in the range of 3 to 25mPa · sec. When the viscosity of the adhesive composition is less than 3mPa · sec, the water resistance thereof cannot be sufficiently exhibited when the adhesive composition is used to manufacture a polarizing plate, and when the viscosity is more than 25mPa · sec, the optical characteristics of the polarizing plate may be lowered.
In the present invention, the adhesive composition may be formed by adding at least 1 kind of suitable additives known in the art, such as a plasticizer, a silane coupling agent, an antistatic agent, fine particles, an alcohol having good diffusibility, and a metal salt, in a range not to impair the effects thereof.
The form of the adhesive composition may be any form known in the art, and may be a liquid form, for example, in order to form a uniform adhesive layer on the surface of a polarizing plate or a protective film as an adherend. Such liquid adhesives may be of the solution type or dispersion type using various solvents, and the solution type is preferable in view of the coatability of the substrate, and the solution type or dispersion type using water as a solvent is applicable in view of the stability.
In addition, for the purpose of shortening the drying step, a water/alcohol mixed solvent in which an alcohol solvent that is miscible with water and has a lower boiling point than water is mixed may be used in the adhesive solution. The boiling point of the alcohol solvent is not particularly limited, and may be 100 ℃ or lower, may be 80 ℃ or lower, and may preferably be 70 ℃ or lower.
And (iii) bonding the polarizing plate and the protective film with the adhesive layer interposed therebetween.
The method for joining the protective film of the present invention may be any method known in the art, and for example, the adhesive composition may be applied to the adhesive surface of the polarizing plate and/or the protective film by a casting method, a meyer bar coating method, a gravure coating method, a die coating method, a dip coating method, a spraying method, or the like, and the both may be superposed. Here, the term "joined" means that the polarizing plate and the protective film are bonded to each other by being in contact with each other in a grounded manner via the adhesive layer.
After the adhesive composition is applied, the polarizing plate and the protective film may be sandwiched and bonded by a nip roll.
In the present invention, the bonding speed is not limited as long as the bonding speed can make the thickness of the adhesive layer thick, and for example, the bonding speed for bonding the protective film on the adhesive layer may be 10 to 35m/min, and preferably 20 to 30 m/min. If the thickness is within the above range, the thickness of the adhesive layer can be adjusted to the range of the thickness of the adhesive layer in the polarizing plate of the present invention. Here, the bonding speed is a length per unit time at which the polarizing plate and the protective film are bonded with the adhesive layer interposed therebetween.
In addition, in order to improve the adhesiveness, treatments known in the art may be applied without particular limitation, and for example, the surface of the polarizing plate and/or the protective film may be subjected to a surface treatment such as a plasma treatment, a corona treatment, an ultraviolet irradiation treatment, a flame treatment, or a saponification treatment. The saponification treatment may be carried out by immersing the resin in an aqueous solution of an alkali such as sodium hydroxide or potassium hydroxide.
In the present invention, the polarizing plate, the adhesive layer, and the protective film may be laminated and then subjected to a drying treatment. The drying treatment may be carried out by spraying hot air, and the temperature may be in the range of 50 to 100 ℃, but is not limited thereto, and the drying time may be 30 to 1000 seconds, but is not limited thereto.
< image display device >
In addition, the present invention provides an image display device including the polarizing plate.
The polarizing plate of the present invention can be applied to an image display device including a structure known in the art in addition to a polarizing plate. The image display device to which the polarizing plate of the present invention can be applied is not particularly limited as long as it is an image display device to which a polarizing plate can be applied, and may be, for example, various image display devices such as a general liquid crystal display device, a field emission display device, a plasma display device, and a field emission display device.
[ examples ]
Hereinafter, production examples and embodiments that are preferable for the understanding of the present invention are given, and these production examples and embodiments are merely examples illustrating the present invention and are not examples limiting the scope of the technical solution of the present application, and it is obvious to those skilled in the art that various changes and modifications can be made to the production examples and embodiments within the scope of the scope and technical idea of the present invention, and these changes and modifications naturally fall within the scope of the technical solution of the present application.
Production example 1: production of polarizing plate
A transparent unstretched polyvinyl alcohol film (PE60, KURARAY) having a saponification degree of 99.9% or more was immersed in water (deionized water) at 25 ℃ for 1 minute and 20 seconds to swell (swelling step), and then immersed in a 30 ℃ aqueous dyeing solution containing 1.25mM/L iodine, 1.25 wt% potassium iodide, and 0.3 wt% boric acid for 2 minutes and 30 seconds to dye (dyeing step). At this time, in the swelling and dyeing steps, stretching was performed at a stretching ratio of 1.56 times and 1.64 times, respectively, so that the cumulative stretching ratio up to the dyeing bath was 2.56 times. Then, the resultant was immersed in a crosslinking aqueous solution containing 13.9 wt% of potassium iodide and 3 wt% of boric acid at 56 ℃ for 26 seconds (first crosslinking step) to crosslink the film, and simultaneously, the film was stretched at a stretch ratio of 1.7 times. Thereafter, the resultant was immersed in a crosslinking aqueous solution containing 13.9 wt% of potassium iodide and 3 wt% of boric acid at 56 ℃ for 20 seconds (second crosslinking step) to crosslink the film, and simultaneously, the film was stretched at a stretch ratio of 1.34 times. Then, the resultant was immersed in an aqueous solution containing 5 wt% of potassium iodide and 2 wt% of boric acid at 40 ℃ for 10 seconds (color correction step), and stretched 1.01-fold. At this time, the total cumulative draw ratio in the swelling, dyeing and crosslinking, complementary color steps was made 6 times. After completion of the crosslinking, the polyvinyl alcohol film was dried in an oven at 90 ℃ for 4 minutes to produce a polarizing plate having a stripe pattern unevenness of Lv3 at a level described later (RSm 3000 μm, Rt 700 nm).
The measurement methods of RSm and Rt are shown below.
The polarizing plates fabricated in the production examples were prepared so as to have a width of 10mm × a length of 10mm, and then fixed with tape on the X/Y stage of a Bruker interferometer microscope (model Contour GT-I) in order to maintain the surface of the sample without causing warpage.
The measurement was carried out under conditions set by AcuityXR PSI Mode, Object 10X, Multiplier 1.0.0X, measurement area 10 mm. times.10 mm, Illumination Green, and then the surface of the polarizing plate was measured, and RSm and Rt were calculated based on ISO 4287-1997.
For reference, a surface photograph of the manufactured polarizing plate is shown in fig. 1.
In describing the examples of the present invention, unevenness of the stripe pattern was visually confirmed by the fluorescent lamp reflection method according to the following criteria. The fluorescent lamp reflection method is an evaluation method in which light incident on a fluorescent lamp from an oblique direction of about 45 ° is reflected, and unevenness of a polarizing plate is visually observed by the reflected light.
Lv 1.: unevenness of stripe pattern was not confirmed
Lv 2.: the unevenness of the stripe pattern can be recognized by the reflection method of the fluorescent lamp, but cannot be confirmed by visual observation
Lv 3.: unevenness of stripe pattern can be visually recognized by fluorescent lamp reflection method
Production example 2: production of polarizing plate
A polarizing plate was produced in the same manner as in production example 1, except that the temperatures in the first and second crosslinking steps were changed from 56 ℃ to 59 ℃ and the total cumulative stretching ratio in the swelling, dyeing, crosslinking, and color-complementing steps was changed to 6.1 times. (unevenness of stripe pattern: Lv3, RSm 3700 μm, Rt 790 nm).
Production example 3: production of polarizing plate
A polarizing plate was produced in the same manner as in production example 1, except that the temperature in the first and second crosslinking steps was changed from 56 ℃ to 59 ℃, the boric acid in the aqueous crosslinking solution in the first and second crosslinking steps was changed from 3% by weight to 3.6% by weight, and the total cumulative stretching ratio in the swelling, dyeing, crosslinking, and color-complementing steps was changed to 6.3 times. (unevenness of stripe pattern: Lv3, RSm 4900 μm, Rt 950 nm).
Production example 4: production of polarizing plate
A polarizing plate was produced in the same manner as in production example 1, except that the temperature in the first and second crosslinking steps was changed from 56 ℃ to 59 ℃, the boric acid in the aqueous crosslinking solution in the first and second crosslinking steps was changed from 3% by weight to 3.6% by weight, and the total cumulative stretching ratio in the swelling, dyeing, crosslinking, and color-complementing steps was changed to 6.5 times. (unevenness of stripe pattern: Lv3, RSm 6000 μm, Rt 1100 nm).
Production example 5: production of polarizing plate
A polarizing plate was produced in the same manner as in production example 1, except that the immersion time in the swelling step was changed from 1 minute to 20 seconds to 50 seconds, the immersion time in the dyeing step was changed from 2 minutes to 30 seconds to 2 minutes, the cumulative draw ratio up to the dyeing step was changed from 2.56 times to 3 times, and the total cumulative draw ratio in the swelling, dyeing, crosslinking, and color-complementing steps was changed from 6 times to 5.4 times. (unevenness of stripe pattern: Lv1, RSm 1000 μm, Rt 140 nm).
< example 1 >
(a) Production of adhesive composition
An acetoacetyl-modified polyvinyl alcohol resin (GOSEINOL Z-200, japan synthetic chemical industry ltd.) having a saponification degree of 99.2 mol% was dissolved in water (distilled water) to prepare an aqueous solution having a solid content of 3 wt%.
This acetoacetyl group-modified polyvinyl alcohol resin aqueous solution and sodium glyoxylate (10% aqueous solution) as a crosslinking agent were mixed so that the solid content of sodium glyoxylate was 10 parts by weight based on 100 parts by weight of the solid content of the acetoacetyl group-modified polyvinyl alcohol resin to produce an adhesive composition having a total solid content of 3.3% by weight. At this time, the adhesive composition had a pH of 6.1 and a viscosity of 7.5 mPasec.
(b) Manufacture of polarizing plates
After coating both sides of the polarizing plate of the above production example 1 with the adhesive composition produced in (a), triacetyl cellulose film KC8UX (saponified TAC of Konica) as a protective film was bonded to both sides. The joining speed was 20 m/min.
After the bonding, the resulting film was dried at 80 ℃ for 5 minutes to prepare a polarizing plate (thickness of adhesive layer: 300 nm).
< examples 2 to 9 and comparative examples 1 to 4 >
Polarizing plates were produced in the same manner as in example 1, except that the concentration of the adhesive solid component and the bonding speed were changed to adjust the thickness of the adhesive layer as shown in table 1. However, methylolmelamine available from Aldrich was used as the crosslinking agent in the adhesive composition of example 7.
< examples 10 and 11 >
Polarizing plates were produced in the same manner as in example 1 (example 10) and example 2 (example 11), respectively, except that the polarizing plate of production example 2 was used.
< examples 12 and 13 >
Polarizing plates were produced in the same manner as in example 1 (example 12) and example 2 (example 13), respectively, except that the polarizing plate of production example 3 was used.
< comparative example 5 >
A polarizing plate was produced in the same manner as in example 1, except that the polarizing plate of production example 4 was used.
< example 14 >
A polarizing plate was produced in the same manner as in example 1, except that the polarizing plate of production example 5 was used.
[ Table 1]
[ Table 1]
[ evaluation test ]
The polarizing plates obtained in examples 1 to 14 and comparative examples 1 to 5 were subjected to the following evaluation tests.
1. Adhesiveness (cutter evaluation)
After each polarizing plate was left to stand at room temperature for 1 hour, the blade edge of the cutter was pulled between the films of the polarizing plate (between the polarizer and one protective film and between the polarizer and the other protective film), and the manner of blade edge entry when pushing the blade edge was evaluated in accordance with the following criteria.
Very good: the blade of the cutter does not enter between the films of either side.
O: the edge of the cutter blade stops when the blade enters the space between the films by 2mm or less.
And (delta): when the blade is pushed forward, the blade stops when entering at least one film space by more than 2mm and 5mm or less.
X: when the blade is pushed, the blade enters at least one of the films without difficulty (if the blade enters one of the films without difficulty, the blade cannot enter the other film, or the blade stops when entering at 5mm or less).
2. Water resistance
The following water resistance test (warm water immersion test) was carried out on each polarizing plate left to stand at 23 ℃ and 55% relative humidity for 24 hours to evaluate the water resistance. First, a polarizing plate was cut in a 5cm × 2cm rectangular shape with the absorption axis (stretching direction) of the polarizing plate as the long side to prepare a sample, and the dimension in the long side direction was accurately measured. Here, the sample uniformly exhibits a specific color over the entire surface due to iodine adsorbed to the polarizing plate. Here, fig. 2 is a view schematically showing the method of the evaluation test of water resistance, fig. 2(a) shows the sample (1) before immersion in warm water, and fig. 2(B) shows the sample (1) after immersion in warm water. As shown in FIG. 2A, 1 short side of the sample was held by a holding part (5), and the sample was immersed in a water bath at 60 ℃ for 4 hours at about 8 degrees in the longitudinal direction. Thereafter, the sample (1) was taken out from the water tank to wipe off water.
The polarizer (4) of the polarizing plate shrinks due to the immersion in warm water. The degree of shrinkage of the polarizing plate (4) was evaluated as the shrinkage length by measuring the distance from the end (1a) (end of the protective film) of the sample (1) to the end of the shrunk polarizing plate (4) at the center of the short side of the sample (1). As shown in fig. 2B, the polarizing plate (4) located at the center of the polarizing plate shrinks due to immersion in warm water, and a region (2) where the polarizing plate (4) is not present is formed between the protective films.
Further, iodine eluted from the periphery of the polarizing plate (4) which was in contact with the warm water by the immersion in the warm water, and a discolored portion (3) was generated in the periphery of the sample (1). The degree of discoloration was evaluated as the deiodination length by measuring the distance from the edge of the shrunk polarizer (4) to the region (6) where the color peculiar to the polarizing plate remained in the center of the short side of the sample (1). The total of the shrinkage length and the deiodination length is defined as a total etching length (X). That is, the total etching length (X) is the distance from the end (1a) (end of the protective film) of the sample (1) to the region (6) where the color specific to the polarizing plate remains in the center of the short side of the sample (1). The smaller the shrinkage length, deiodination length and total etched length (X), the higher the adhesiveness (water resistance) in the presence of water can be judged.
Very good: the total etching length X is less than 2mm
O: the total etching length X is more than 2mm and less than 3mm
And (delta): the total etching length X is more than 3mm and less than 5mm
X: the total etching length X is more than 5mm
3. Determination of the level of unevenness of a striped pattern
After the polarizing plate was manufactured, the presence or absence of the unevenness of the stripe pattern was confirmed by the fluorescent lamp reflection method in accordance with the above-described criteria.
4. Optical Properties (transmissivity, degree of polarization)
The polarizing plate thus produced was cut into a size of 4cm × 4cm, and the transmittance was measured using an ultraviolet-visible spectrometer (V-7100, JASCO corporation). In this case, the degree of polarization is defined by the following equation 1.
[ mathematical formula 1]
Degree of polarization (P) [ (T1-T2)/(T1+ T2)]1/2
(in the formula, T1 represents parallel transmittance obtained when the pair of polarizing plates are arranged so that their absorption axes are parallel, and T2 represents orthogonal transmittance obtained when the pair of polarizing plates are arranged so that their absorption axes are orthogonal).
[ Table 2]
[ Table 2]
Referring to table 2, it was confirmed that the polarizing plates of the examples were superior to those of the comparative examples in both optical characteristics (degree of polarization) and appearance characteristics (level of unevenness of fringe pattern).
In addition, it was confirmed that example 1 in which sodium glyoxylate was used as a crosslinking agent was superior in water resistance to example 7 in which methylolmelamine was used as a crosslinking agent.
Description of the symbols
Claims (2)
1. A method for manufacturing a polarizing plate, comprising:
swelling step, dyeing step, crosslinking step, color complementing step and stretching step,
the crosslinking step includes a first crosslinking step and a second crosslinking step,
the temperature of the first crosslinking step and the second crosslinking step is 56 ℃ or higher,
until the cumulative stretch ratio in the dyeing step is 1.2 to 4.0 times,
the cumulative stretching ratio of the first crosslinking step and the second crosslinking step is 1.5 times to 5.0 times,
the total cumulative stretch ratio is 5.3 to 6.5 times.
2. The polarizing plate production method according to claim 1, wherein,
the temperature of the color complementing step is 20-40 ℃.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020150115866A KR20170021476A (en) | 2015-08-18 | 2015-08-18 | Polarizing plate and method of preparing the same |
| KR10-2015-0115866 | 2015-08-18 | ||
| CN201680045107.5A CN107850723B (en) | 2015-08-18 | 2016-08-17 | Polarizing plate and method for manufacturing same |
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| CN201680045107.5A Division CN107850723B (en) | 2015-08-18 | 2016-08-17 | Polarizing plate and method for manufacturing same |
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| CN113189692A true CN113189692A (en) | 2021-07-30 |
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| CN202110494521.7A Pending CN113189692A (en) | 2015-08-18 | 2016-08-17 | Method for manufacturing polarizing plate |
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| JP (2) | JP6878281B2 (en) |
| KR (2) | KR20170021476A (en) |
| CN (2) | CN107850723B (en) |
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| JP2020024240A (en) * | 2018-08-06 | 2020-02-13 | 日東電工株式会社 | Method for manufacturing polarizer |
| CN115083319B (en) * | 2021-09-10 | 2023-06-20 | 荣耀终端有限公司 | Display assembly, terminal equipment and processing method of display assembly |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000249832A (en) * | 1999-03-01 | 2000-09-14 | Nitto Denko Corp | Polarizing film, polarizing plate and optical member |
| JP2007268898A (en) * | 2006-03-31 | 2007-10-18 | Fujifilm Corp | Manufacturing method for optical film, optical film, polarizing plate, and liquid crystal display unit |
| WO2014115897A1 (en) * | 2013-01-28 | 2014-07-31 | 住友化学株式会社 | Process for manufacturing polarizing film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009008329A1 (en) * | 2007-07-06 | 2009-01-15 | Nitto Denko Corporation | Polarization plate |
| JP5789936B2 (en) * | 2009-10-22 | 2015-10-07 | 住友化学株式会社 | Optical laminate and method for producing the same |
| JP2012068593A (en) * | 2010-09-27 | 2012-04-05 | Nitto Denko Corp | Polarizer, method for manufacturing polarizer, optical film, and image display device |
| JP6103335B2 (en) * | 2012-01-18 | 2017-03-29 | 日本電気硝子株式会社 | GLASS SUBSTRATE, ITS MANUFACTURING METHOD, AND ORGANIC EL DEVICE USING GLASS SUBSTRATE |
| KR20140114923A (en) | 2013-03-18 | 2014-09-30 | 동우 화인켐 주식회사 | Adhesive composition and polarizing plate using the same |
| JP2014206702A (en) * | 2013-04-16 | 2014-10-30 | 富士フイルム株式会社 | Polarizing plate and image display device |
| KR101400132B1 (en) * | 2013-10-07 | 2014-05-30 | 동우 화인켐 주식회사 | Preparing method for polarizer |
| JP2015114456A (en) * | 2013-12-11 | 2015-06-22 | 住友化学株式会社 | Method for manufacturing surface-modified cycloolefin resin film and polarizing plate |
| JP6349082B2 (en) * | 2013-12-12 | 2018-06-27 | 住友化学株式会社 | Polarizing plate and display device |
| KR101938411B1 (en) * | 2014-01-13 | 2019-01-15 | 동우 화인켐 주식회사 | Polarizing plate |
| KR101663698B1 (en) * | 2015-03-16 | 2016-10-07 | 동우 화인켐 주식회사 | Preparing method for polarizer |
-
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- 2015-08-18 KR KR1020150115866A patent/KR20170021476A/en unknown
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- 2016-08-17 JP JP2017535549A patent/JP6878281B2/en active Active
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- 2016-08-17 WO PCT/JP2016/074000 patent/WO2017030144A1/en active Application Filing
- 2016-08-17 CN CN202110494521.7A patent/CN113189692A/en active Pending
- 2016-08-17 KR KR1020187007371A patent/KR20180031801A/en not_active Application Discontinuation
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000249832A (en) * | 1999-03-01 | 2000-09-14 | Nitto Denko Corp | Polarizing film, polarizing plate and optical member |
| JP2007268898A (en) * | 2006-03-31 | 2007-10-18 | Fujifilm Corp | Manufacturing method for optical film, optical film, polarizing plate, and liquid crystal display unit |
| WO2014115897A1 (en) * | 2013-01-28 | 2014-07-31 | 住友化学株式会社 | Process for manufacturing polarizing film |
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| JP2021140164A (en) | 2021-09-16 |
| TW201711839A (en) | 2017-04-01 |
| JP6878281B2 (en) | 2021-05-26 |
| WO2017030144A1 (en) | 2017-02-23 |
| CN107850723A (en) | 2018-03-27 |
| JPWO2017030144A1 (en) | 2018-06-07 |
| KR20180031801A (en) | 2018-03-28 |
| TWI726902B (en) | 2021-05-11 |
| CN107850723B (en) | 2021-08-17 |
| KR20170021476A (en) | 2017-02-28 |
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