JP6723240B2 - Method of manufacturing polarizer - Google Patents
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- JP6723240B2 JP6723240B2 JP2017528613A JP2017528613A JP6723240B2 JP 6723240 B2 JP6723240 B2 JP 6723240B2 JP 2017528613 A JP2017528613 A JP 2017528613A JP 2017528613 A JP2017528613 A JP 2017528613A JP 6723240 B2 JP6723240 B2 JP 6723240B2
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- 238000004132 cross linking Methods 0.000 claims description 66
- 238000004043 dyeing Methods 0.000 claims description 56
- 238000000034 method Methods 0.000 claims description 38
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- 238000001035 drying Methods 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 239000012192 staining solution Substances 0.000 claims 1
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- 229910052740 iodine Inorganic materials 0.000 description 23
- 239000011630 iodine Substances 0.000 description 23
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 21
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 239000004372 Polyvinyl alcohol Substances 0.000 description 14
- 238000005520 cutting process Methods 0.000 description 14
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- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 8
- 150000001639 boron compounds Chemical class 0.000 description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 5
- 239000004327 boric acid Substances 0.000 description 5
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- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 3
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- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 description 3
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- 238000012986 modification Methods 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
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- CBECDWUDYQOTSW-UHFFFAOYSA-N 2-ethylbut-3-enal Chemical compound CCC(C=C)C=O CBECDWUDYQOTSW-UHFFFAOYSA-N 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- UNMYWSMUMWPJLR-UHFFFAOYSA-L Calcium iodide Chemical compound [Ca+2].[I-].[I-] UNMYWSMUMWPJLR-UHFFFAOYSA-L 0.000 description 1
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- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 description 1
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- 241000656145 Thyrsites atun Species 0.000 description 1
- 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 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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- SGUXGJPBTNFBAD-UHFFFAOYSA-L barium iodide Chemical compound [I-].[I-].[Ba+2] SGUXGJPBTNFBAD-UHFFFAOYSA-L 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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- 150000003949 imides Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002497 iodine compounds Chemical class 0.000 description 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-L isophthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC(C([O-])=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-L 0.000 description 1
- 239000012046 mixed solvent Substances 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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- 229920000098 polyolefin Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
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- 229920002223 polystyrene Polymers 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
- 238000005096 rolling process Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000009518 sodium iodide Nutrition 0.000 description 1
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- 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
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Polarising Elements (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Ophthalmology & Optometry (AREA)
Description
本発明は、偏光子の製造方法に関する。 The present invention relates to a method for manufacturing a polarizer.
液晶表示装置（ＬＣＤ）、電界発光（ＥＬ）表示装置、プラズマ表示装置（ＰＤＰ）、電界放出表示装置（ＦＥＤ）、有機発光ダイオード（ＯＬＥＤ）などのような各種の画像表示装置に用いられている偏光板は、一般的にポリビニルアルコール系（ｐｏｌｙｖｉｎｙｌ ａｌｃｏｈｏｌ、ＰＶＡ）フィルムにヨウ素系化合物または二色性偏光物質が吸着配向された偏光子を含み、偏光子の一面には偏光子保護フィルムが積層されており、偏光子の他の一面には偏光子保護フィルム、液晶セルと接合される粘着剤層と離型フィルムが順に積層された多層構造を有する。 It is used in various image display devices such as a liquid crystal display device (LCD), an electroluminescent (EL) display device, a plasma display device (PDP), a field emission display device (FED), and an organic light emitting diode (OLED). The polarizing plate generally includes a polarizer in which an iodine compound or a dichroic polarizing material is adsorbed and aligned on a polyvinyl alcohol (PVA) film, and a polarizer protective film is laminated on one surface of the polarizer. Therefore, the other side of the polarizer has a multilayer structure in which a polarizer protective film, a pressure-sensitive adhesive layer bonded to a liquid crystal cell, and a release film are sequentially laminated.
偏光板を構成する偏光子は画像表示装置に適用され、色再現性に優れた画像を提供するために高い透過率及び偏光度を兼備することが要求される。これを具現するために、ポリビニルアルコール系フィルム自体を改質するか、または昇華性があるヨウ素系偏光素子の代わりに非昇華性二色性染料を使用する方法を用いて偏光子を製造されている。 A polarizer that constitutes a polarizing plate is applied to an image display device and is required to have both high transmittance and polarization degree in order to provide an image with excellent color reproducibility. In order to realize this, a polarizer is manufactured by modifying a polyvinyl alcohol-based film itself or using a non-sublimable dichroic dye instead of a sublimable iodine-based polarizing element. There is.
このような側面で、薄膜のポリビニルアルコール系フィルムを用いて高い透過率を具現することができるが、薄膜のため製造工程中（特に、染色または、架橋ステップ）にフィルムが容易に切断され、偏光度などの光学特性が顕著に低下するという問題があった。 In this aspect, it is possible to realize a high transmittance by using a thin polyvinyl alcohol-based film, but the film is easily cut during the manufacturing process (particularly, the dyeing or cross-linking step) due to the thin film, so that the polarized light There is a problem that the optical characteristics such as the degree are significantly deteriorated.
韓国公開特許第１０−２００９−００７００８５号には偏光子の製造方法が開示されているが、上記の問題点に対する代案を提示できていない。 Korean Published Patent No. 10-2009-0070085 discloses a method for manufacturing a polarizer, but fails to present an alternative to the above problems.
本発明は、光学特性に優れた偏光子を製造することができ、製造工程中に偏光子形成用フィルムの切断が発生することを減少させ、生産性を向上させた偏光子の製造方法を提供することを目的とする。 The present invention provides a method for producing a polarizer capable of producing a polarizer having excellent optical properties, reducing the occurrence of cutting of a film for forming a polarizer during the production process, and improving productivity. The purpose is to do.
１．偏光子形成用フィルムを乾式延伸、応力緩和、染色及び架橋するステップを含み、
前記乾式延伸ステップは、前記フィルムの結晶化度が０．６乃至０．８を満足するように行われる、偏光子の製造方法。1. Dry stretching, stress relaxation, dyeing and cross-linking the film for forming a polarizer,
The method of manufacturing a polarizer, wherein the dry stretching step is performed so that the crystallinity of the film satisfies 0.6 to 0.8.
２．上記１において、前記フィルムの結晶化度は０．６１乃至０．７５である、偏光子の製造方法。 2. In the above 1, the method for producing a polarizer, wherein the film has a crystallinity of 0.61 to 0.75.
３．上記１において、前記偏光子形成用フィルムの厚みは１０乃至３０μｍである、偏光子の製造方法。 3. In the above 1, the method for manufacturing a polarizer, wherein the film for forming a polarizer has a thickness of 10 to 30 μm.
４．上記１において、前記乾式延伸ステップのフィルムの延伸比は４乃至５倍である、偏光子の製造方法。 4. In the above-mentioned 1, the method for producing a polarizer, wherein the stretch ratio of the film in the dry stretching step is 4 to 5 times.
５．上記１において、前記乾式延伸ステップは１２０乃至１４０℃で行われる、偏光子の製造方法。 5. In the above 1, the method for manufacturing a polarizer, wherein the dry stretching step is performed at 120 to 140°C.
６．上記１において、前記応力緩和ステップは２０乃至５０℃の応力緩和用水溶液に浸漬して行われる、偏光子の製造方法。 6. In the above-mentioned 1, the method for manufacturing a polarizer, wherein the stress relaxation step is performed by immersing in the stress relaxation aqueous solution at 20 to 50°C.
７．上記１において、前記応力緩和ステップは４０乃至１８０秒間行われる、偏光子の製造方法。 7. In the above-mentioned 1, the method for manufacturing a polarizer, wherein the stress relaxation step is performed for 40 to 180 seconds.
８．上記１において、前記応力緩和ステップのフィルムの延伸比は０．９乃至１倍である、偏光子の製造方法。 8. In the above 1, the method for producing a polarizer, wherein the stretch ratio of the film in the stress relaxation step is 0.9 to 1 times.
９．上記１において、前記染色ステップは５乃至４２℃の染色用水溶液に浸漬して行われる、偏光子の製造方法。 9. In the above-mentioned 1, the method of manufacturing a polarizer, wherein the dyeing step is performed by immersing the dyeing solution in an aqueous solution for dyeing at 5 to 42°C.
１０．上記１において、前記染色ステップは６０秒乃至２００秒間行われる、偏光子の製造方法。 10. 1. In the above-mentioned 1, the method of manufacturing a polarizer, wherein the dyeing step is performed for 60 seconds to 200 seconds.
１１．上記１において、前記染色ステップのフィルムの延伸比は１乃至１．１倍である、偏光子の製造方法。 11. 1. In the above-mentioned 1, the method for producing a polarizer, wherein the stretching ratio of the film in the dyeing step is 1 to 1.1 times.
１２．上記１において、前記架橋ステップは２０乃至９０℃の架橋用水溶液に浸漬して行われる、偏光子の製造方法。 12. In the above-mentioned 1, the method for producing a polarizer, wherein the crosslinking step is performed by immersing in a crosslinking aqueous solution at 20 to 90°C.
１３．上記１において、前記架橋ステップは１秒乃至１５分間行われる、偏光子の製造方法。 13. In the above 1, the method for producing a polarizer, wherein the crosslinking step is performed for 1 second to 15 minutes.
１４．上記１において、前記架橋ステップのフィルムの延伸比は０．９９乃至１．６５倍である、偏光子の製造方法。 14. In the above-mentioned 1, the method for producing a polarizer, wherein the stretching ratio of the film in the crosslinking step is 0.99 to 1.65 times.
１５．上記１において、前記架橋ステップの後、水洗及び乾燥ステップをさらに含む、偏光子の製造方法。 15. In the above 1, the method for producing a polarizer, further comprising washing and drying steps after the crosslinking step.
本発明の偏光子の製造方法は、湿式工程に入る前に乾式延伸工程を行い、前記乾式工程中にフィルムの結晶化度を特定の範囲にすることにより、製造工程中にフィルムの切断が生じず、生産性に優れる。 The method for producing a polarizer of the present invention comprises performing a dry stretching step before entering a wet step, and setting the crystallinity of the film in a specific range during the dry step, whereby cutting of the film occurs during the production step. And excellent in productivity.
本発明の偏光子の製造方法は、光学特性に優れた偏光子を製造することができる。 The polarizer manufacturing method of the present invention can manufacture a polarizer having excellent optical characteristics.
本発明は偏光子の製造方法に関し、より詳細には、偏光子形成用フィルムを乾式延伸、応力緩和、染色及び架橋するステップで行われる製造工程中、乾式延伸ステップをフィルムの結晶化度が０．６乃至０．８を満足するように行うことにより、薄膜のフィルムを用いても染色または架橋工程でフィルムの切断が発生しないため偏光子の生産性を向上させることができ、光学特性に優れた偏光子を製造することができる方法に関する。 The present invention relates to a method for manufacturing a polarizer, and more specifically, in the manufacturing process performed in the steps of dry stretching, stress relaxation, dyeing and cross-linking a film for forming a polarizer, the dry stretching step is performed so that the crystallinity of the film is 0. By performing so as to satisfy 6 to 0.8, it is possible to improve the productivity of the polarizer because the film is not cut in the dyeing or crosslinking process even if a thin film is used, and the optical properties are excellent. And a method by which a polarizer can be manufactured.
偏光子は、適用されるディスプレイが要求する光学特性を具現するために、偏光子形成用フィルムの材料、工程条件などを適切に調節して製造されるが、ＯＬＥＤに用いられる偏光子の場合、高い透過率を有する偏光子が要求されることもある。このような、高い透過率を有する偏光子を製造するために、薄膜の偏光子形成用フィルムを用いたが、この場合、製造工程中（特に、染色または、架橋ステップ）にフィルムが容易に切断され、偏光度などの光学特性が顕著に低下するという問題があった。 The polarizer is manufactured by appropriately adjusting the material of the film for forming the polarizer, the process conditions, etc. in order to realize the optical characteristics required by the applied display. In the case of the polarizer used for the OLED, A polarizer having a high transmittance may be required. In order to manufacture such a polarizer having a high transmittance, a thin film for forming a polarizer was used. In this case, the film was easily cut during the manufacturing process (particularly, the dyeing or crosslinking step). However, there is a problem in that the optical characteristics such as the degree of polarization are significantly reduced.
そこで、本発明は湿式工程に入る前に乾式延伸工程を行い、乾式延伸ステップを通じて適正な結晶化度を有するフィルムを製造することにより、薄膜のフィルムを用いても前述した問題が発生しない偏光子の製造方法を導き出した。 Therefore, according to the present invention, a dry stretching process is performed before a wet process is performed, and a film having an appropriate crystallinity is manufactured through the dry stretching process, so that the above-mentioned problems do not occur even when a thin film is used. The manufacturing method was derived.
本発明の偏光子の製造方法は、偏光子形成用フィルムを乾式延伸、応力緩和、染色及び架橋するステップで行われる。 The method for producing a polarizer of the present invention is performed in the steps of dry stretching, stress relaxation, dyeing and crosslinking of a film for forming a polarizer.
以下、本発明の一実施例を挙げてより詳細に説明することとする。 Hereinafter, one embodiment of the present invention will be described in more detail.
＜乾式延伸ステップ＞
本発明による偏光子の製造方法は、湿式工程に入る前に偏光子形成用フィルムを乾式延伸する工程を行う。<Dry stretching step>
In the method for manufacturing a polarizer according to the present invention, a step of dry-stretching a film for forming a polarizer is performed before starting a wet step.
前記乾式延伸ステップにより、フィルムの結晶化度が０．６乃至０．８を満足するように延伸されることにより、フィルムの強度が改善して、薄膜に製造しても後述する湿式工程（特に、染色及び架橋ステップ）でフィルムの切断発生率を減少させることができ、これによって偏光子の生産性が向上する。また、乾式延伸ステップの終了時にフィルムの結晶化度が前記結晶化度の範囲を満足する場合、偏光度が低下しにくい。 In the dry stretching step, the strength of the film is improved by stretching the film so that the crystallinity of the film satisfies 0.6 to 0.8. The dyeing and cross-linking step) can reduce the incidence of film scission, thereby improving the productivity of the polarizer. When the crystallinity of the film at the end of the dry stretching step satisfies the crystallinity range, the degree of polarization is less likely to decrease.
本発明で「結晶化度」とは、乾式延伸工程を経た偏光子形成用フィルムに対して、前記フィルムを成す高分子の結晶部分と非結晶部分の全体のうちの結晶部分に対する割合を意味し、前記結晶化度は当分野に通常知られた方法を通じて測定することができる。 In the present invention, the "crystallinity" means a ratio of the polymer portion of the polymer forming the film to the crystal portion of the entire crystal portion with respect to the polarizer-forming film that has undergone the dry stretching step. The crystallinity can be measured by a method commonly known in the art.
本発明による乾式延伸ステップで、乾式延伸終了時のフィルムの結晶化度が０．６未満である場合、後述する染色及び架橋工程で切断が容易に発生し、乾式延伸終了時のフィルムの結晶化度が０．８を超える場合、光学特性、特に、偏光度が低下し得る。また、前記フィルムの結晶化度は好ましくは０．６１乃至０．７５であってもよく、この場合、前述した問題点なしにより優れた光学特性を具現することができる。 In the dry stretching step according to the present invention, when the crystallinity of the film at the end of the dry stretching is less than 0.6, cutting easily occurs in the dyeing and cross-linking process described below, and the film is crystallized at the end of the dry stretching. If the degree exceeds 0.8, the optical properties, especially the degree of polarization, may be reduced. Also, the crystallinity of the film may be preferably 0.61 to 0.75, in which case excellent optical properties can be realized without the above-mentioned problems.
前記結晶化度は当分野で公知の方法によって具現することができ、例えば、ＭＤ方向への延伸倍率を高くすると延伸後の結晶化度が高くなる傾向があるので延伸倍率の調整により結晶化度を制御でき、さらに、フィルムの温度、偏光子形成用フィルムの材料、添加剤（可塑剤など）の種類及び含量、フィルムの水分率などを適正範囲に調節することによっても具現することができ、これに限定されるものではない。 The crystallinity can be embodied by a method known in the art. For example, if the stretching ratio in the MD direction is increased, the crystallinity after stretching tends to increase. Therefore, the crystallinity can be adjusted by adjusting the stretching ratio. The temperature of the film, the material of the film for forming a polarizer, the type and content of additives (plasticizer, etc.), the moisture content of the film, etc. can be controlled within an appropriate range. It is not limited to this.
本発明による偏光子形成用フィルムは、前述した本発明の乾式延伸工程を容易に行うことができるものであって、二色性物質、すなわちヨウ素などによって染色可能なフィルムであればその種類が特に限定されず、例えばポリビニルアルコールフィルム、部分的に鹸化されたポリビニルアルコールフィルム；ポリエチレンテレフタレートフィルム、エチレン−酢酸ビニル共重合体フィルム、エチレン−ビニルアルコール共重合体フィルム、セルロースフィルム、これらの部分的に鹸化されたフィルムなどのような親水性高分子フィルム；または脱水処理されたポリビニルアルコール系フィルム、脱塩酸処理されたポリビニルアルコール系フィルムなどのようなポリエン配向フィルムなどが挙げられる。これらの中で、面内で偏光度の均一性を強化する効果に優れているだけでなく、ヨウ素に対する染色親和性に優れているという点で、ポリビニルアルコール系フィルムが好ましい。 The film for forming a polarizer according to the present invention can be easily subjected to the dry stretching step of the present invention described above, and if the film can be dyed with a dichroic substance, i.e. iodine, its kind is particularly Without limitation, for example, polyvinyl alcohol film, partially saponified polyvinyl alcohol film; polyethylene terephthalate film, ethylene-vinyl acetate copolymer film, ethylene-vinyl alcohol copolymer film, cellulose film, partially saponified thereof. A hydrophilic polymer film such as a treated film; or a polyene oriented film such as a dehydrated polyvinyl alcohol-based film and a dehydrochlorination-treated polyvinyl alcohol-based film. Among them, the polyvinyl alcohol film is preferable because it is excellent in the effect of enhancing the uniformity of the degree of polarization in the plane and is excellent in the dyeing affinity for iodine.
前記偏光子形成用フィルムの厚みは特に限定されないが、例えば、１０乃至３０μｍであってもよく、上記の範囲を満足する場合、優れた透過率を具現することができ、本発明の製造工程を通じて十分な強度を確保し、後述する湿式工程でフィルムの切断が生じないため適合する。 The thickness of the film for forming a polarizer is not particularly limited, and may be, for example, 10 to 30 μm, and when the above range is satisfied, excellent transmittance can be realized, and the manufacturing process of the present invention can be performed. It is suitable because it secures sufficient strength and the film is not cut in the wet process described below.
本発明の乾式延伸ステップで、フィルムの延伸比は特に限定されないが、約４乃至５倍であってもよく、好ましくは４．０乃至４．８倍であってもよい。上記の範囲を満足する場合、前述した適正な結晶化度を具現することに適合し、約５倍を超える場合、染色工程でヨウ素の染色性が低下して要求される光学特性を具現し難い。 In the dry stretching step of the present invention, the stretching ratio of the film is not particularly limited, but may be about 4 to 5 times, preferably 4.0 to 4.8 times. When the above range is satisfied, it is suitable for realizing the above-mentioned appropriate crystallinity, and when it exceeds about 5 times, the dyeability of iodine is lowered in the dyeing process, and it is difficult to realize the required optical characteristics. ..
本発明の乾式延伸ステップの遂行温度は特に限定されないが、例えば、１２０乃至１４０℃であってもよく、好ましくは１２５乃至１３５℃であってもよい。上記の範囲を満足する場合、前述した適正な結晶化度を具現することに適合し、１４０℃を超える場合、結晶化度が過度に高くなり、染色工程でヨウ素の染色性が低下して要求される光学特性を具現し難い。 The temperature at which the dry stretching step of the present invention is performed is not particularly limited, but may be, for example, 120 to 140°C, preferably 125 to 135°C. If the above range is satisfied, it is suitable for realizing the above-mentioned appropriate crystallinity, and if it exceeds 140°C, the crystallinity becomes excessively high, and the dyeing property of iodine decreases in the dyeing step, which is required. It is difficult to realize the optical characteristics that are used.
本発明の乾式延伸ステップの遂行時間は特に限定されないが、前述した適正な結晶化度に到逹する範囲内で適切に行うことができ、例えば、１秒乃至１分間行うことができ、好ましくは５乃至３０秒間行うことができる。 The execution time of the dry stretching step of the present invention is not particularly limited, but it can be appropriately performed within a range that reaches the above-mentioned appropriate crystallinity, for example, 1 second to 1 minute, preferably It can be done for 5 to 30 seconds.
本発明の乾式延伸ステップの遂行方法は特に限定されないが、例えば、フィルムに張力を付与して加圧ロールによって圧延する方法、フィルムに張力を付与して加熱ロールに接触させる方法、加熱オーブンの内部または外部に設置されたロール間でフィルムを加熱しつつ引張力を加えながら延伸する方法、２つの加熱ロールの間を通過させて圧縮延伸させる方法などが挙げられ、このとき、前述した乾式延伸ステップの遂行温度は、延伸用のロールやオーブンの温度を調節することにより具現することができる。 The method of performing the dry stretching step of the present invention is not particularly limited, for example, a method of applying tension to the film and rolling with a pressure roll, a method of applying tension to the film to contact the heating roll, the inside of a heating oven. Or a method of stretching while applying a tensile force while heating the film between the rolls installed outside, a method of passing through between two heating rolls and compression stretching, and the like, at this time, the dry stretching step described above. The execution temperature can be realized by adjusting the temperature of a drawing roll or an oven.
本発明による偏光子の製造方法において、偏光子形成用フィルムの延伸は、乾式延伸ステップの他に、後述する湿式工程（応力緩和、染色、架橋工程など）で同時に行うことができる。 In the method for producing a polarizer according to the present invention, the film for forming a polarizer can be simultaneously stretched by a wet process (stress relaxation, dyeing, crosslinking process, etc.) described later in addition to the dry stretching step.
＜応力緩和ステップ＞
本発明による偏光子の製造工程は、乾式延伸の後、応力緩和ステップを行う。<Stress relaxation step>
In the manufacturing process of the polarizer according to the present invention, a stress relaxation step is performed after dry stretching.
応力緩和ステップは、乾式延伸後の偏光子形成用フィルムを染色工程の前に応力緩和用水溶液で満たされた応力緩和槽に浸漬し、フィルム表面上に堆積したほこりまたはブロッキング防止剤のような不純物を取り除き、偏光子形成用フィルムの応力を緩和させ、染色性を向上させて染色不均一性も防止し、偏光子の物性を向上させるためのステップである。 The stress relaxation step involves immersing the polarizer-formed film after dry stretching in a stress relaxation tank filled with a stress relaxation aqueous solution before the dyeing step, to collect dust or impurities such as an antiblocking agent deposited on the film surface. Is a step for alleviating the stress of the film for forming a polarizer, improving the dyeing property to prevent uneven dyeing, and improving the physical properties of the polarizer.
応力緩和用水溶液としては、通常、水（純水、脱イオン水）を単独で用いてもよく、高分子フィルムの加工性を向上させるために、少量のグリセリンまたはヨウ化カリウムを添加してもよい。 As the stress-releasing aqueous solution, water (pure water, deionized water) may be generally used alone, or a small amount of glycerin or potassium iodide may be added to improve the processability of the polymer film. Good.
グリセリン及びヨウ化カリウムを含む場合、その含量は特に限定されず、例えば応力緩和用水溶液の総重量中それぞれ５重量％以下、１０重量％以下であってもよい。 When glycerin and potassium iodide are contained, their contents are not particularly limited, and may be 5 wt% or less and 10 wt% or less, respectively, in the total weight of the stress relaxation aqueous solution.
応力緩和ステップの遂行温度（応力緩和用水溶液の温度）は特に限定されず、例えば２０乃至５０℃であってもよく、好ましくは２５乃至４０℃であるのがよい。応力緩和ステップの温度が上記の範囲内である場合、応力緩和が適切に行われ、フィルムの切断発生を顕著に減少させることができる。 The temperature at which the stress relaxation step is performed (the temperature of the stress relaxation aqueous solution) is not particularly limited, and may be, for example, 20 to 50° C., preferably 25 to 40° C. When the temperature of the stress relaxation step is within the above range, the stress relaxation is appropriately performed, and the occurrence of film breakage can be significantly reduced.
応力緩和ステップの遂行時間（応力緩和槽浸漬時間）は特に限定されず、例えば４０秒乃至１８０秒以下であってもよく、好ましくは９０秒以下であるのがよい。応力緩和ステップの遂行時間が上記の範囲内である場合、応力緩和ステップの温度が上記の範囲内である場合、応力緩和が適切に行われ、フィルムの切断発生を顕著に減少させることができる。 The execution time of the stress relaxation step (stress relaxation tank immersion time) is not particularly limited and may be, for example, 40 seconds to 180 seconds or less, preferably 90 seconds or less. When the execution time of the stress relaxation step is within the above range, and when the temperature of the stress relaxation step is within the above range, the stress relaxation is appropriately performed, and the occurrence of cutting of the film can be significantly reduced.
応力緩和ステップとともに湿式延伸ステップを同時に行うことができ、この場合、前記応力緩和ステップの延伸比は約０．９乃至１倍であってもよく、上記の範囲内で、光学特性の低下なしに適正範囲で応力緩和を行うことができる。 The wet stretching step may be performed simultaneously with the stress relaxation step, and in this case, the stretching ratio of the stress relaxation step may be about 0.9 to 1 times, and within the above range, without deteriorating the optical characteristics. Stress relaxation can be performed within an appropriate range.
＜染色ステップ＞
本発明による偏光子の製造方法は、前記応力緩和ステップの後、染色ステップを行う。<Dyeing step>
In the method for manufacturing a polarizer according to the present invention, a dyeing step is performed after the stress relaxation step.
染色ステップは、偏光子形成用フィルムを二色性物質、例えばヨウ素を含む染色用水溶液で満たされた染色槽に浸漬させ、偏光子形成用フィルムにヨウ素を吸着させるステップである。 The dyeing step is a step of immersing the polarizer-forming film in a dyeing tank filled with a dichroic substance, for example, an aqueous dyeing solution containing iodine, and adsorbing iodine to the polarizer-forming film.
染色用水溶液は、水、水溶性有機溶媒またはこれらの混合溶媒とヨウ素を含むものであってもよい。 The dyeing aqueous solution may contain water, a water-soluble organic solvent or a mixed solvent thereof, and iodine.
前記染色用水溶液内のヨウ素の濃度は、染色液中０．４乃至４００ｍｍｏｌ／Ｌであってもよく、好ましくは０．８乃至２７５ｍｍｏｌ／Ｌ、より好ましくは１乃至２００ｍｍｏｌ／Ｌであってもよい。 The concentration of iodine in the dyeing aqueous solution may be 0.4 to 400 mmol/L in the dyeing solution, preferably 0.8 to 275 mmol/L, and more preferably 1 to 200 mmol/L. ..
また、前記染色用水溶液は、染色効率の改善のために溶解補助剤としてヨウ化物をさらに含んでいてもよい。 Further, the dyeing aqueous solution may further contain iodide as a solubilizing agent in order to improve dyeing efficiency.
ヨウ化物の種類は特に限定されず、例えばヨウ化カリウム、ヨウ化リチウム、ヨウ化ナトリウム、ヨウ化亜鉛、ヨウ化アルミニウム、ヨウ化鉛、ヨウ化銅、ヨウ化バリウム、ヨウ化カルシウム、ヨウ化錫、ヨウ化チタンなどが挙げられ、水に対する溶解度が大きいという点でヨウ化カリウムが好ましい。これらは単独または２種以上混合して用いてもよい。 The type of iodide is not particularly limited, and examples thereof include potassium iodide, lithium iodide, sodium iodide, zinc iodide, aluminum iodide, lead iodide, copper iodide, barium iodide, calcium iodide, tin iodide. , Titanium iodide, and the like, and potassium iodide is preferable because it has high solubility in water. You may use these individually or in mixture of 2 or more types.
前記ヨウ化物の含量は特に限定されず、例えば染色用水溶液の総重量中０．０１乃至１０重量％であってもよく、好ましくは０．１乃至５重量％であるのがよい。 The content of the iodide is not particularly limited, and may be 0.01 to 10% by weight, preferably 0.1 to 5% by weight, based on the total weight of the dyeing aqueous solution.
また、前記染色用水溶液は偏光子形成用フィルムのヨウ素錯体含量を増加させるためにホウ酸をさらに含んでいてもよい。 The dyeing aqueous solution may further contain boric acid to increase the iodine complex content of the polarizer-forming film.
前記ホウ酸の含量は特に限定されず、例えば染色用水溶液の総重量中０．３乃至５重量％であってもよい。上記の範囲を満足する場合、ＰＶＡ−Ｉ３ −錯体及びＰＶＡ−Ｉ５ −錯体の含量が増加するため好ましく、但し、５重量％を超える場合、フィルムの切断の危険性が増加するようになる。The content of boric acid is not particularly limited, and may be, for example, 0.3 to 5% by weight based on the total weight of the dyeing aqueous solution. If within the ranges described above, PVA-I 3 - complex and PVA-I 5 - preferably for the content of the complex is increased, however, if it exceeds 5 wt%, so that the risk of cutting of the film is increased ..
染色ステップの遂行温度（染色用水溶液の温度）は特に限定されないが、例えば５乃至４２℃であってもよく、好ましくは１０乃至３５℃であるのがよい。染色ステップの温度が上記の範囲内である場合、フィルムの切断なしにヨウ素がフィルムに効果的に吸着して優れた光学特性を具現することができる。 The temperature at which the dyeing step is performed (the temperature of the dyeing aqueous solution) is not particularly limited, but may be, for example, 5 to 42° C., and preferably 10 to 35° C. When the temperature of the dyeing step is within the above range, iodine can be effectively adsorbed to the film without cutting the film to realize excellent optical characteristics.
染色ステップの遂行時間（染色槽浸漬時間）は特に限定されず、例えば６０乃至２００秒であってもよく、好ましくは８０乃至１５０秒であってもよい。染色ステップの時間が上記の範囲内である場合、フィルムの切断なしにヨウ素がフィルムに効果的に吸着して優れた光学特性を具現することができる。 The execution time of the dyeing step (dyeing bath immersion time) is not particularly limited and may be, for example, 60 to 200 seconds, preferably 80 to 150 seconds. When the time of the dyeing step is within the above range, iodine can be effectively adsorbed to the film without cutting the film to realize excellent optical characteristics.
染色ステップとともに湿式延伸ステップを同時に行うことができ、この場合、前記染色ステップの延伸比は約１乃至１．１倍であってもよく、上記の範囲内で、フィルムの切断なしに優れた光学特性を具現することができる。 The wet drawing step may be performed simultaneously with the dyeing step, and in this case, the draw ratio of the dyeing step may be about 1 to 1.1 times, and within the above range, excellent optical performance without cutting the film may be achieved. The characteristics can be realized.
また、応力緩和ステップ及び染色ステップでの累積延伸比は０．９乃至１．１倍であることが好ましく、前記累積延伸比が０．９倍未満である場合、フィルムにしわが発生して外観不良が発生する場合があり、１．１倍を超える場合、延伸ムラが発生する場合がある。 In addition, the cumulative stretching ratio in the stress relaxation step and the dyeing step is preferably 0.9 to 1.1 times, and when the cumulative stretching ratio is less than 0.9 times, the film has wrinkles and a poor appearance. May occur, and when it exceeds 1.1 times, stretching unevenness may occur.
＜架橋ステップ＞
本発明による偏光子の製造方法は、前記染色ステップの後、架橋ステップを行う。<Crosslinking step>
In the method for manufacturing a polarizer according to the present invention, a crosslinking step is performed after the dyeing step.
架橋ステップは、物理的に吸着されているヨウ素分子による染色性が外部環境によって低下しないように、染色された偏光子形成用フィルムを架橋用水溶液に浸漬させて架橋し、吸着されたヨウ素分子を固定させるステップである。二色性染料であるヨウ素は架橋反応が不十分な場合、湿熱環境によりヨウ素分子が脱離することがあり、十分な架橋反応が要求される。また、偏光子形成用フィルムは、分子と分子との間に位置するヨウ素分子を配向させ、光学特性を向上させるためには、架橋ステップで大きい延伸比で延伸されることが好ましい。 In the crosslinking step, the dyed film for forming a polarizer is immersed in an aqueous solution for crosslinking so that the dyeing property due to physically adsorbed iodine molecules is not deteriorated by the external environment, and the adsorbed iodine molecules are removed. This is the step of fixing. When the crosslinking reaction of iodine, which is a dichroic dye, is insufficient, iodine molecules may be desorbed due to a wet heat environment, and a sufficient crosslinking reaction is required. The polarizer-forming film is preferably stretched at a high stretching ratio in the crosslinking step in order to orient the iodine molecules located between the molecules and improve the optical properties.
よって、前記架橋ステップは第１架橋ステップ及び第２架橋ステップによって行うことができ、前記ステップの少なくとも１つのステップで、ホウ素化合物を含む架橋用水溶液を用いてもよく、この場合、前記ホウ素化合物によって偏光子の光学特性の向上と同時に色耐久性が向上することができるため好ましい。 Therefore, the cross-linking step may be performed by the first cross-linking step and the second cross-linking step, and an aqueous solution for cross-linking containing a boron compound may be used in at least one of the steps, and in this case, depending on the boron compound. This is preferable because it is possible to improve the color durability as well as the optical characteristics of the polarizer.
架橋用水溶液は水とホウ素化合物を含んでいてもよく、水と共に相互作用可能な有機溶媒及びヨウ化物をさらに含んでいてもよい。 The aqueous solution for crosslinking may contain water and a boron compound, and may further contain an organic solvent capable of interacting with water and iodide.
ホウ素化合物は、短い架橋結合とフィルムの剛直性を付与し、工程中のフィルムのしわ発生を抑制することにより、取扱性を向上させ、ヨウ素配向を形成する役割をする。 The boron compound serves to impart short cross-linking and rigidity of the film, suppress wrinkling of the film during the process, improve handleability, and form iodine orientation.
前記架橋用水溶液内のホウ素化合物の濃度は特に限定されず、例えば架橋用水溶液の総重量中１乃至１０重量％であってもよく、上記の範囲を満足する場合、適正範囲に架橋され、優れた光学特性を具現することができる。また、１重量％未満である場合、架橋効果が減少してフィルムにおける剛直性が低下する場合があり、１０重量％を超える場合、過度な架橋結合によってフィルムの切断が発生する場合がある。 The concentration of the boron compound in the crosslinking aqueous solution is not particularly limited, and may be, for example, 1 to 10% by weight based on the total weight of the crosslinking aqueous solution. When the above range is satisfied, the boron compound is crosslinked in an appropriate range and excellent. It is possible to realize excellent optical characteristics. If it is less than 1% by weight, the cross-linking effect may be reduced and the rigidity of the film may be lowered, and if it exceeds 10% by weight, the film may be cut due to excessive cross-linking.
また、架橋用水溶液は、偏光子の面内での偏光度の均一性と染着されたヨウ素の脱着を防止するため、ヨウ化物をさらに含んでいてもよい。 The crosslinking aqueous solution may further contain iodide in order to prevent the uniformity of the degree of polarization in the plane of the polarizer and the desorption of dyed iodine.
前記架橋用水溶液内のヨウ化物の含量は特に限定されないが、例えば架橋用水溶液の総重量中０．０５乃至１５重量％であってもよく、好ましくは０．５乃至１１重量％であってもよい。上記の範囲を満足する場合、染色ステップで吸着されたヨウ素イオンがフィルムから抜け出たり架橋液に含まれたヨウ素イオンがフィルムに浸透したりすることを防ぎ、透過率の変化を抑制することができる。 The content of iodide in the crosslinking aqueous solution is not particularly limited, but may be, for example, 0.05 to 15% by weight, preferably 0.5 to 11% by weight, based on the total weight of the crosslinking aqueous solution. Good. When the above range is satisfied, it is possible to prevent the iodine ions adsorbed in the dyeing step from escaping from the film or the iodine ions contained in the cross-linking liquid from penetrating into the film, and suppressing the change in transmittance. ..
架橋ステップの遂行温度（架橋用水溶液の温度）は特に限定されないが、例えば２０乃至９０℃であってもよく、好ましくは５０乃至７５℃であってもよく、架橋ステップの温度が上記の範囲内である場合、フィルムの切断なしにヨウ素が適正範囲に配向され、優れた光学特性を具現することができる。 The temperature at which the crosslinking step is performed (the temperature of the aqueous solution for crosslinking) is not particularly limited, but may be, for example, 20 to 90°C, preferably 50 to 75°C, and the temperature of the crosslinking step is within the above range. In this case, iodine can be oriented in an appropriate range without cutting the film, and excellent optical characteristics can be realized.
架橋ステップの遂行時間（架橋槽浸漬時間）は特に限定されず、例えば１秒乃至１５分であってもよく、好ましくは５秒乃至１０分であるのがよい。架橋ステップの時間が上記の範囲内である場合、フィルムの切断なしにヨウ素が適正範囲に配向され、優れた光学特性を具現することができる。 The time of performing the crosslinking step (immersion time in the crosslinking tank) is not particularly limited, and may be, for example, 1 second to 15 minutes, preferably 5 seconds to 10 minutes. When the time of the cross-linking step is within the above range, iodine can be oriented in an appropriate range without cutting the film, and excellent optical properties can be realized.
架橋ステップとともに湿式延伸ステップを同時に行うことができ、この場合、前記架橋ステップの延伸比は約０．９９乃至１．６５倍であってもよく、上記の範囲内で、フィルムの切断なしにヨウ素が適正範囲に配向され、優れた光学特性を具現することができ、これによって偏光子の生産性を向上させることができる。 The wet stretching step may be performed simultaneously with the crosslinking step, and in this case, the stretching ratio of the crosslinking step may be about 0.99 to 1.65 times, and within the above range, iodine may be obtained without cutting the film. Can be oriented in an appropriate range, and excellent optical characteristics can be realized, thereby improving the productivity of the polarizer.
また、前記架橋ステップが第１架橋ステップ及び第２架橋ステップによって行われる場合、第１架橋ステップの延伸比は約１．１乃至１．５倍であってもよく、第２架橋ステップの延伸比は約１乃至１．３倍であってもよく、第１架橋ステップ及び第２架橋ステップの累積延伸比は約１．１乃至２．５倍であってもよい。 In addition, when the cross-linking step is performed by the first cross-linking step and the second cross-linking step, the stretch ratio of the first cross-linking step may be about 1.1 to 1.5 times, and the stretch ratio of the second cross-linking step may be about 1. May be about 1 to 1.3 times, and the cumulative draw ratio of the first crosslinking step and the second crosslinking step may be about 1.1 to 2.5 times.
＜水洗ステップ＞
必要に応じて、本発明の偏光子の製造方法は、架橋ステップが完了した後に水洗ステップをさらに含んでいてもよい。<Washing step>
If necessary, the method for producing a polarizer of the present invention may further include a water washing step after the crosslinking step is completed.
水洗ステップは、延伸及び架橋が完了した偏光子形成用フィルムを水洗用水溶液で満たされた水洗槽に浸漬させ、前のステップで偏光子形成用フィルムに付着した不要な残留物を取り除くステップである。 The water-washing step is a step of immersing the polarizer-forming film that has been stretched and cross-linked in a water-washing tank filled with a water-washing aqueous solution, and removing unnecessary residues attached to the polarizer-forming film in the previous step. ..
水洗用水溶液は水（脱イオン水）であってもよく、これにヨウ化物がさらに添加されてもよい。 The water solution for washing may be water (deionized water), and iodide may be further added thereto.
水洗ステップの遂行温度（水洗用水溶液の温度）は特に限定されず、例えば０乃至６０℃であってもよく、好ましくは５乃至３０℃であってもよい。 The temperature at which the washing step is performed (the temperature of the aqueous solution for washing) is not particularly limited, and may be, for example, 0 to 60°C, preferably 5 to 30°C.
水洗ステップは省略可能であり、応力緩和ステップ、染色ステップ及び架橋ステップのような前のステップが完了するたびに行うこともできる。また、１回以上繰り返してもよく、その繰り返し回数は特に制限されない。 The water washing step is optional and can be performed every time previous steps such as stress relaxation, dyeing and crosslinking steps are completed. Further, it may be repeated one or more times, and the number of repetitions is not particularly limited.
＜乾燥ステップ＞
乾燥ステップは、水洗された偏光子形成用フィルムを乾燥させ、乾燥によるネックインで染着されたヨウ素分子の配向をより向上させ、光学特性に優れた偏光子を得るステップである。<Drying step>
The drying step is a step in which the water-washed film for forming a polarizer is dried to further improve the orientation of iodine molecules dyed by the neck-in due to drying, thereby obtaining a polarizer having excellent optical properties.
乾燥方法は特に限定されないが、自然乾燥、エア乾燥、加熱乾燥、遠赤外線乾燥、マイクロ波乾燥、熱風乾燥などの方法を用いることができ、最近ではフィルム内にある水のみを活性化させて乾燥させるマイクロ波処理が新たに用いられており、通常、熱風処理と遠赤外線処理が主に用いられている。 The drying method is not particularly limited, and methods such as natural drying, air drying, heat drying, far infrared ray drying, microwave drying, and hot air drying can be used, and recently, only the water in the film is activated to dry. Microwave treatment is newly used, and usually hot air treatment and far infrared treatment are mainly used.
熱風乾燥時の遂行温度は特に限定されないが、偏光子の劣化を防止するために比較的低い温度で行われることが好ましく、例えば２０乃至１０５℃であってもよく、好ましくは１００℃以下であるのがよい。 The temperature for performing hot air drying is not particularly limited, but it is preferably performed at a relatively low temperature in order to prevent deterioration of the polarizer, and may be, for example, 20 to 105° C., preferably 100° C. or less. It's good.
前記熱風乾燥の遂行時間は特に限定されず、例えば１乃至１０分間行うことができる。 The hot air drying time is not particularly limited and may be, for example, 1 to 10 minutes.
本発明による偏光子の製造方法は、前述のステップのうちの乾式延伸ステップ及び乾燥ステップを除いた残りのステップは全て恒温水槽内で偏光子形成用フィルムを浸漬して行われるものであってもよい。 In the method for producing a polarizer according to the present invention, the remaining steps other than the dry stretching step and the drying step among the above steps may be performed by immersing the film for forming a polarizer in a constant temperature water bath. Good.
前記偏光子の製造方法による偏光子に関し、前記偏光子は少なくとも一面に保護フィルムが積層された偏光板を製造するのに用いることができる。 Regarding the polarizer according to the method for manufacturing a polarizer, the polarizer can be used for manufacturing a polarizing plate having a protective film laminated on at least one surface thereof.
前記保護フィルムの種類は、透明性、機械的強度、熱安定性、水分遮蔽性、等方性などに優れたフィルムであれば特に限定されず、具体的な例を挙げると、ポリエチレンテレフタレート、ポリエチレンイソフタレート、ポリブチレンテレフタレートなどのポリエステル系樹脂；ジアセチルセルロース、トリアセチルセルロースなどのセルロース系樹脂；ポリカーボネート系樹脂；ポリメチル（メタ）アクリレート、ポリエチル（メタ）アクリレートなどのポリアクリル系樹脂；ポリスチレン、アクリロニトリル−スチレン共重合体などのスチレン系樹脂；ポリエチレン、ポリプロピレン、シクロ系またはノルボルネン構造を有するポリオレフィン、エチレンプロピレン共重合体などのポリオレフィン系樹脂；ナイロン、芳香族ポリアミドなどのポリアミド系樹脂；イミド系樹脂；ポリエーテルスルホン系樹脂；スルホン系樹脂；ポリエーテルケトン系樹脂；硫化ポリフェニレン系樹脂；ビニルアルコール系樹脂；塩化ビニリデン系樹脂；ビニルブチラール系樹脂；アリレート系樹脂；ポリオキシメチレン系樹脂；エポキシ系樹脂などのような熱可塑性樹脂で構成されたフィルムが挙げられ、前記熱可塑性樹脂のブレンド物で構成されたフィルムも用いることができる。また、（メタ）アクリル系、ウレタン系、エポキシ系、シリコン系などの熱硬化性樹脂または紫外線硬化型樹脂からなるフィルムを用いることもできる。これらの中でも特にアルカリなどによって鹸化された表面を有するセルロース系フィルムが偏光特性または耐久性を考慮すると好ましい。また、保護フィルムは下記の光学層の機能を兼備したものであってもよい。 The type of the protective film is not particularly limited as long as it is a film excellent in transparency, mechanical strength, thermal stability, moisture shielding property, isotropic property, and specific examples thereof include polyethylene terephthalate and polyethylene. Polyester resin such as isophthalate and polybutylene terephthalate; Cellulose resin such as diacetyl cellulose and triacetyl cellulose; Polycarbonate resin; Polyacrylic resin such as polymethyl (meth)acrylate and polyethyl (meth)acrylate; Polystyrene and acrylonitrile- Styrene-based resins such as styrene copolymers; polyolefin-based resins such as polyethylene, polypropylene, polyolefins having a cyclo-based or norbornene structure, ethylene-propylene copolymers; polyamide-based resins such as nylon and aromatic polyamide; imide-based resins; poly Ether sulfone resin; sulfone resin; polyetherketone resin; polyphenylene sulfide resin; vinyl alcohol resin; vinylidene chloride resin; vinyl butyral resin; arylate resin; polyoxymethylene resin; epoxy resin, etc. A film made of such a thermoplastic resin can be used, and a film made of a blend of the above thermoplastic resins can also be used. Further, a film made of a thermosetting resin such as a (meth)acrylic resin, a urethane resin, an epoxy resin, a silicon resin or an ultraviolet curable resin can be used. Among these, a cellulosic film having a surface saponified with an alkali or the like is particularly preferable in view of polarization characteristics or durability. Further, the protective film may also have the following function of the optical layer.
前記偏光板の構造は特に制限されず、必要な光学特性を満足させることができる様々な種類の光学層が偏光子上に積層されたものであってもよい。例えば、偏光子の少なくとも一面に偏光子を保護する保護フィルムが積層された構造；偏光子の少なくとも一面または保護フィルム上に、ハードコーティング層、反射防止層、粘着防止層、拡散防止層、防眩層などの表面処理層が積層された構造；偏光子の少なくとも一面または保護フィルム上に、視野角を補償する配向液晶層、または他の機能性膜が積層された構造を有するものであってもよい。また、各種の画像表示装置を形成することに用いられる偏光変換装置のような光学膜、リフレクタ、半透過板、１／２波長板または１／４波長板などの波長板（λ板を含む）を含む位相差板、視野角補償膜、輝度向上膜のうちの１つ以上が光学層として積層された構造であってもよい。より詳細には、偏光子の一面に保護フィルムが積層された構造の偏光板であって、積層された保護フィルム上にリフレクタまたは半透過リフレクタが積層された反射型偏光板または半透過型偏光板；位相差板が積層された楕円形または円形偏光板；視野角補償層または視野角補償膜が積層された広視野角偏光板；或いは輝度向上膜が積層された偏光板などが好ましい。 The structure of the polarizing plate is not particularly limited, and various kinds of optical layers capable of satisfying necessary optical characteristics may be laminated on the polarizer. For example, a structure in which a protective film for protecting the polarizer is laminated on at least one surface of the polarizer; a hard coating layer, an antireflection layer, an antisticking layer, a diffusion preventing layer, an antiglare layer on at least one surface of the polarizer or on the protective film. A structure in which a surface-treated layer such as a layer is laminated; an alignment liquid crystal layer for compensating a viewing angle or another functional film is laminated on at least one surface of a polarizer or a protective film Good. Further, a wavelength plate (including a λ plate) such as an optical film such as a polarization conversion device used for forming various image display devices, a reflector, a semi-transmissive plate, a ½ wavelength plate or a ¼ wavelength plate. It may have a structure in which one or more of a retardation film including, a viewing angle compensation film, and a brightness enhancement film are laminated as an optical layer. More specifically, a polarizing plate having a structure in which a protective film is laminated on one surface of a polarizer, and a reflective polarizing plate or a semitransparent polarizing plate in which a reflector or a semi-transmissive reflector is laminated on the laminated protective film. An elliptical or circular polarizing plate having a retardation plate laminated thereon; a wide viewing angle polarizing plate having a viewing angle compensating layer or a viewing angle compensating film laminated thereon; or a polarizing plate having a brightness improving film laminated thereon is preferable.
このような偏光板は、通常の液晶表示装置だけはなく、有機電界発光表示装置（ＯＬＥＤ）、プラズマ表示装置、電界放出表示装置などの各種の画像表示装置に適用可能である。 Such a polarizing plate can be applied not only to a normal liquid crystal display device, but also to various image display devices such as an organic light emitting display device (OLED), a plasma display device, and a field emission display device.
以下、本発明の理解を助けるために好ましい実施例を提示するが、これらの実施例は本発明を例示するものに過ぎず、クレーム範囲を制限するものではなく、本発明の範疇及び技術思想の範囲内で実施例に対する様々な変更及び修正が可能であることは当業者にとって明らかであり、これらの変形及び修正が添付のクレーム範囲に属することも当然のことである。 Hereinafter, preferred examples will be presented in order to facilitate understanding of the present invention. However, these examples merely illustrate the present invention and do not limit the scope of the claims, and the scope and technical idea of the present invention are not limited thereto. It will be apparent to those skilled in the art that various changes and modifications to the embodiments can be made within the scope, and it is to be understood that these variations and modifications fall within the scope of the appended claims.
実施例及び比較例
（実施例１）
３０μｍの厚さを有し鹸化度が９９．９％以上である透明な未延伸ポリビニルアルコールフィルム（ＰＥ３０、ＫＵＲＡＲＡＹ社）を１２０℃の熱ロールで４倍乾式延伸した。延伸後にフィルムの結晶化度を測定した。Examples and Comparative Examples (Example 1)
A transparent unstretched polyvinyl alcohol film (PE30, KURARAY) having a thickness of 30 μm and a saponification degree of 99.9% or more was dry-stretched 4 times by a hot roll at 120° C. The crystallinity of the film was measured after stretching.
その後、乾式延伸済のフィルムを２５℃の水（脱イオン水）に１分２０秒間浸漬して応力緩和させた後、ヨウ素１．２５ｍＭ／Ｌとヨウ化カリウム１．２５重量％、ホウ酸０．３重量％が含有された３０℃の染色用水溶液に２分浸漬して染色した。このとき、応力緩和及び染色ステップでそれぞれ０．９２倍、１．００２倍の延伸比で延伸して、応力緩和槽から染色槽までの累積延伸比が０．９２２になるように延伸した。次いで、ヨウ化カリウム１０重量％、ホウ酸８重量％が含有された６５℃の架橋液に３０秒間浸漬（第１架橋ステップ）して架橋させながら、１．３倍の延伸比で延伸した。その後に、ヨウ化カリウム１０重量％、ホウ酸８重量％が含有された６５℃の架橋液に２０秒間浸漬（第２架橋ステップ）して架橋させながら、１．０３倍の延伸比で延伸した。 Then, the dry-stretched film was immersed in water (deionized water) at 25° C. for 1 minute and 20 seconds to relax the stress, and then iodine 1.25 mM/L, potassium iodide 1.25% by weight, boric acid 0 Dyeing was carried out by immersing in a dyeing aqueous solution containing 30% of 0.3% by weight for 2 minutes. At this time, stretching was performed at a stretching ratio of 0.92 times and 1.002 times in the stress relaxation and dyeing steps, respectively, so that the cumulative stretching ratio from the stress relaxation tank to the dyeing tank was 0.922. Then, while being immersed in a crosslinking liquid containing 65% by weight of potassium iodide and 8% by weight of boric acid at 65° C. for 30 seconds (first crosslinking step) to perform crosslinking, the film was stretched at a stretch ratio of 1.3 times. Then, while being immersed in a crosslinking liquid containing 65% by weight of potassium iodide and 8% by weight of boric acid at 65° C. for 20 seconds (second crosslinking step) to perform crosslinking, the film was stretched at a stretching ratio of 1.03 times. ..
このとき、応力緩和、染色及び架橋ステップの総累積延伸比が１．２３４倍になるようにした。架橋が完了した後、ポリビニルアルコールフィルムを１００℃のオーブンで１分間乾燥させて偏光子を製造し、製造された偏光子の透過率は４３．５％であった。 At this time, the total cumulative stretch ratio of the stress relaxation, dyeing and crosslinking steps was set to 1.234 times. After the crosslinking was completed, the polyvinyl alcohol film was dried in an oven at 100° C. for 1 minute to manufacture a polarizer, and the transmittance of the manufactured polarizer was 43.5%.
以下、実施例１乃至１０及び比較例１乃至７の全ての透過率が４３．５％（偏差０．２％）の範囲内となるようにサンプルを製作した。 Hereinafter, samples were manufactured such that all the transmittances of Examples 1 to 10 and Comparative Examples 1 to 7 were within the range of 43.5% (deviation 0.2%).
（実施例２乃至７及び比較例１乃至４）
下記の表１に記載された乾式延伸倍率及び乾式延伸温度を調節したことを除いては、実施例１と同様の方法で偏光子を製造した。(Examples 2 to 7 and Comparative Examples 1 to 4)
A polarizer was manufactured in the same manner as in Example 1, except that the dry stretching ratio and the dry stretching temperature shown in Table 1 below were adjusted.
（比較例５）
乾式延伸を行わないことを除いては、実施例１と同様の方法で偏光子を製造した。(Comparative example 5)
A polarizer was produced in the same manner as in Example 1, except that dry stretching was not performed.
（実施例８）
ポリビニルアルコールフィルムの厚みが２０μｍで異なることを除いては、実施例１と同様の方法で偏光子を製造した。(Example 8)
A polarizer was produced in the same manner as in Example 1, except that the thickness of the polyvinyl alcohol film was 20 μm.
（実施例９）
水に１分３０秒浸漬して応力緩和する以外は実施例１と同様の方法で偏光子を製造した。(Example 9)
A polarizer was manufactured in the same manner as in Example 1 except that the stress was relaxed by immersing in water for 1 minute and 30 seconds.
（実施例１０）
４０℃の水に浸漬して応力緩和する以外は実施例１と同様の方法で偏光子を製造した。(Example 10)
A polarizer was produced in the same manner as in Example 1 except that the stress was relaxed by immersing it in water at 40°C.
（実施例１１）
４０℃の水に１分３０秒浸漬して応力緩和する以外は実施例１と同様の方法で偏光子を製造した。(Example 11)
A polarizer was manufactured in the same manner as in Example 1, except that the stress was relaxed by immersing in water at 40°C for 1 minute and 30 seconds.
（比較例６）
ポリビニルアルコールフィルムの厚みが６０μｍで異なることを除いては、比較例１と同様の方法で偏光子を製造した。(Comparative example 6)
A polarizer was manufactured in the same manner as in Comparative Example 1, except that the thickness of the polyvinyl alcohol film was 60 μm and was different.
＜乾式延伸後のフィルムの結晶化度＞
吸光度の測定:ポリビニルアルコール系フィルムを乾式延伸後、幅及び長さを１０＊１０ｍｍ以上にカッティングした後、ATR-IR法(Attenuated total Reflection Infrared Spectroscopy;全反射減衰赤外分光法)による赤外分光スペクトルをフーリエ変換赤外分光光度計(Thermo fisher scientific社製赤外分光光度計:NICOLET 5700, Pike Technology社製ATRユニット:VeeMAXIII)を用いて、以下の条件で吸光度の測定を行った。
スキャン回数：１６回、
Ｆｉｎａｌ ｆｏｒｍａｔ：吸光モード、
測定角度：４５度
波数分解能：４ｃｍ−１
測定波数範囲：４００〜４０００ｃｍ−１
スキャンスピード：９．６ｋHz、
ローパスフィルタ：Auto
光源：IR（ceramic）
ビームスプリッタ：KBr
検出器：DTGS KBr
結晶はZnSe
測定方向：光の入射方向と偏光子吸収軸方向が平行となるように測定<Crystallinity of film after dry stretching>
Measurement of absorbance: After dry stretching of a polyvinyl alcohol film, after cutting the width and length to 10*10 mm or more, infrared spectroscopy by ATR-IR method (Attenuated total Reflection Infrared Spectroscopy) The spectra were measured using a Fourier transform infrared spectrophotometer (Infrared spectrophotometer manufactured by Thermo fisher scientific: NICOLET 5700, ATR unit manufactured by Pike Technology: VeeMAX III) under the following conditions.
Number of scans: 16 times
Final format: absorption mode,
Measurement angle: 45 degrees Wave number resolution: 4 cm -1
Measurement wave number range: 400 to 4000 cm -1
Scan speed: 9.6kHz,
Low-pass filter: Auto
Light source: IR (ceramic)
Beam splitter: KBr
Detector: DTGS KBr
The crystal is ZnSe
Measurement direction: Measure so that the incident direction of light and the absorption axis of the polarizer are parallel
結晶化度は下記の式を用いて求める。（Ｃ＝結晶化度）
＜偏光子の特性評価＞
上記の実施例及び比較例において製造された偏光子の物性を下記の方法で測定し、その結果を下記の表２に示した。<Characteristic evaluation of polarizer>
The physical properties of the polarizers manufactured in the above Examples and Comparative Examples were measured by the following methods, and the results are shown in Table 2 below.
１．光学特性（偏光度、透過率） 1. Optical characteristics (polarization degree, transmittance)
製造された偏光子を４ｃｍ×４ｃｍのサイズに切断した後、紫外可視光線分光計（Ｖ−７１００、ＪＡＳＣＯ社製）を用いて透過率を測定した。このとき、偏光度は下記の式（１）で定義される。 After cutting the produced polarizer into a size of 4 cm×4 cm, the transmittance was measured using an ultraviolet-visible light spectrometer (V-7100, manufactured by JASCO). At this time, the degree of polarization is defined by the following equation (1).
偏光度（Ｐ）＝［（Ｔ１−Ｔ２）／（Ｔ１＋Ｔ２）］１／２ （１）Polarization degree (P)=[(T 1 −T 2 )/(T 1 +T 2 )] 1/2 (1)
（式中、Ｔ１は一対の偏光子を吸収軸が平行な状態で配置した場合に得られる平行透過率であり、Ｔ２は一対の偏光子を吸収軸が直交する状態で配置した場合に得られる直交透過率である）。(In the formula, T 1 is a parallel transmittance obtained when a pair of polarizers are arranged in a state where the absorption axes are parallel, and T 2 is a case where a pair of polarizers are arranged in a state where the absorption axes are orthogonal to each other. The resulting orthogonal transmittance).
２．切断評価 2. Disconnection evaluation
実施例及び比較例の条件で偏光子製造時に切断の有／無の発生について下記の評価基準に基づいて目視で確認した。 Under the conditions of the examples and comparative examples, the presence/absence of breakage during the production of the polarizer was visually confirmed based on the following evaluation criteria.
＜評価基準＞
〇：フィルムの切断やクラックが全く発生しない
△：フィルムの切断又はクラックが２回以下発生
Х：フィルムの切断又はクラックが３回以上発生<Evaluation criteria>
◯: The film is not cut or cracked at all. Δ: The film is cut or cracked twice or less. Х: The film is cut or cracked three times or more.
前記表２から分かるように、本発明による製造方法によって製造された偏光子は、優れた光学特性を示すとともに、製造工程中に切断がいずれも発生しなかった。 As can be seen from Table 2, the polarizer manufactured by the manufacturing method according to the present invention showed excellent optical characteristics and did not cause any breakage during the manufacturing process.
乾式延伸ステップの後、結晶化度が本発明の範囲を逸脱する比較例１乃至４及び６の場合、工程中にフィルムの切断が発生するかまたは微細クラックが多量発生したことが確認でき、結晶化度が本発明の上限範囲を逸脱する比較例２、３及び６の場合、光学特性が顕著に低下することが確認できた。 After the dry stretching step, in the case of Comparative Examples 1 to 4 and 6 in which the crystallinity is out of the range of the present invention, it can be confirmed that the film is cut or a large number of fine cracks are generated during the process. It was confirmed that in Comparative Examples 2, 3 and 6 in which the degree of chemical conversion deviates from the upper limit of the present invention, the optical characteristics are remarkably reduced.
特に、乾式延伸ステップを全く行わない比較例５の場合、製造工程中に切断が多発発生したことが確認できた。 In particular, in Comparative Example 5 in which the dry stretching step was not performed at all, it was confirmed that the cutting occurred frequently during the manufacturing process.
また、実施例８と比較例６を比べる場合、実施例８の場合は２０μｍの薄膜のフィルムを用いる場合にも切断が生じなかったが、結晶化度が本発明の範囲を逸脱する比較例８は、６０μｍにもかかわらず、フィルムに切断が２回以下で発生したことが確認できた。 When comparing Example 8 with Comparative Example 6, no breakage occurred even when a thin film of 20 μm was used in Example 8, but the crystallinity was out of the range of the present invention. It was confirmed that the film was cut twice or less even though it was 60 μm.
Claims (14)
前記乾式延伸ステップは、前記フィルムの結晶化度が０．６乃至０．８を満足するように行われ、
前記応力緩和ステップのフィルムの延伸比は０．９０４〜０．９２倍である、偏光子の製造方法。 Dry stretching, stress relaxation, dyeing and cross-linking the film for forming a polarizer,
The dry stretching step is performed so that the crystallinity of the film satisfies 0.6 to 0.8 ,
The method for producing a polarizer , wherein the stretch ratio of the film in the stress relaxation step is 0.904 to 0.92 times .
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