JPWO2013133064A1 - Polyester film roll for optical phase difference plate and method for producing the same - Google Patents
Polyester film roll for optical phase difference plate and method for producing the same Download PDFInfo
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- JPWO2013133064A1 JPWO2013133064A1 JP2013544954A JP2013544954A JPWO2013133064A1 JP WO2013133064 A1 JPWO2013133064 A1 JP WO2013133064A1 JP 2013544954 A JP2013544954 A JP 2013544954A JP 2013544954 A JP2013544954 A JP 2013544954A JP WO2013133064 A1 JPWO2013133064 A1 JP WO2013133064A1
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 17
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 2
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- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- RTWNYYOXLSILQN-UHFFFAOYSA-N methanediamine Chemical compound NCN RTWNYYOXLSILQN-UHFFFAOYSA-N 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000005453 pelletization Methods 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
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- 229920001225 polyester resin Polymers 0.000 description 2
- 239000004645 polyester resin Substances 0.000 description 2
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- 229920000098 polyolefin Polymers 0.000 description 2
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 description 2
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- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
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- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 2
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 1
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 1
- NJWZAJNQKJUEKC-UHFFFAOYSA-N 4-[4-[2-[4-[(1,3-dioxo-2-benzofuran-4-yl)oxy]phenyl]propan-2-yl]phenoxy]-2-benzofuran-1,3-dione Chemical compound C=1C=C(OC=2C=3C(=O)OC(=O)C=3C=CC=2)C=CC=1C(C)(C)C(C=C1)=CC=C1OC1=CC=CC2=C1C(=O)OC2=O NJWZAJNQKJUEKC-UHFFFAOYSA-N 0.000 description 1
- LLLVZDVNHNWSDS-UHFFFAOYSA-N 4-methylidene-3,5-dioxabicyclo[5.2.2]undeca-1(9),7,10-triene-2,6-dione Chemical compound C1(C2=CC=C(C(=O)OC(=C)O1)C=C2)=O LLLVZDVNHNWSDS-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
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- 241000251468 Actinopterygii Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical group [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
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- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 1
- BWVAOONFBYYRHY-UHFFFAOYSA-N [4-(hydroxymethyl)phenyl]methanol Chemical compound OCC1=CC=C(CO)C=C1 BWVAOONFBYYRHY-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- 229910052783 alkali metal Inorganic materials 0.000 description 1
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- 150000008064 anhydrides Chemical class 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
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- 150000002148 esters Chemical class 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 1
- 229940018564 m-phenylenediamine Drugs 0.000 description 1
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
- 229940069446 magnesium acetate Drugs 0.000 description 1
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- 235000011285 magnesium acetate Nutrition 0.000 description 1
- 229940097364 magnesium acetate tetrahydrate Drugs 0.000 description 1
- XKPKPGCRSHFTKM-UHFFFAOYSA-L magnesium;diacetate;tetrahydrate Chemical compound O.O.O.O.[Mg+2].CC([O-])=O.CC([O-])=O XKPKPGCRSHFTKM-UHFFFAOYSA-L 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
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- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- JFNLZVQOOSMTJK-KNVOCYPGSA-N norbornene Chemical compound C1[C@@H]2CC[C@H]1C=C2 JFNLZVQOOSMTJK-KNVOCYPGSA-N 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 239000011146 organic particle Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000011242 organic-inorganic particle Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920001690 polydopamine Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000011045 prefiltration Methods 0.000 description 1
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- 230000002040 relaxant effect Effects 0.000 description 1
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- 229920002050 silicone resin Polymers 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 229920005792 styrene-acrylic resin Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000000000 tetracarboxylic acids Chemical class 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- GGUBFICZYGKNTD-UHFFFAOYSA-N triethyl phosphonoacetate Chemical compound CCOC(=O)CP(=O)(OCC)OCC GGUBFICZYGKNTD-UHFFFAOYSA-N 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3083—Birefringent or phase retarding elements
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/13363—Birefringent elements, e.g. for optical compensation
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Polarising Elements (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
Abstract
フィルム幅方向に対する配向主軸の傾きの角度（配向角）バラツキが６?以内であり、幅が１，２００ｍｍ以上２，０００ｍｍ未満であり、面内位相差値レターデーションが５０〜２００ｎｍであって、フィルム幅方向に対する面内位相差値レターデーションのバラツキが２０ｎｍ以下であり、局所的な位相差ムラが１０ｎｍ未満であり、厚みが２μｍ以上１０μｍ以下であるフィルムを巻き取った光学位相差板用ポリエステルフィルムロール。光学位相差板用として好適に適用できるポリエステルフィルムロールを提供する。The inclination angle (orientation angle) of the orientation main axis with respect to the film width direction is within 6 ?, the width is 1,200 mm or more and less than 2,000 mm, the in-plane retardation value retardation is 50 to 200 nm, Polyester for optical retardation plate obtained by winding a film having a variation of in-plane retardation value retardation in the film width direction of 20 nm or less, local retardation unevenness of less than 10 nm, and a thickness of 2 μm or more and 10 μm or less. Film roll. Provided is a polyester film roll that can be suitably used for an optical phase difference plate.
Description
本発明は、液晶表示用途等の部材において、偏光板と組み合わせて好適に用いられる光学位相差板用ポリエステルフィルムロールに関するものである。 The present invention relates to a polyester film roll for an optical phase difference plate that is suitably used in combination with a polarizing plate in a member such as a liquid crystal display.
近年、偏光板を利用した表示デバイスの普及が進んでいるが、これらのデバイスにおいては、偏光眼鏡をかけると見る角度によって画面が暗くなるという問題が着目されている。 In recent years, display devices using polarizing plates have been widely used. However, in these devices, attention has been paid to the problem that the screen becomes dark depending on the viewing angle when wearing polarized glasses.
これは、偏光眼鏡にある偏光膜の偏光軸と表示デバイスの視認者側に配置されている偏光板の偏光軸の方向とのズレによる透過率の差が原因となっている。 This is caused by a difference in transmittance due to deviation between the polarization axis of the polarizing film in the polarizing glasses and the direction of the polarization axis of the polarizing plate arranged on the viewer side of the display device.
この問題は偏光眼鏡をかけて観察する機会が多いカーナビゲーション、ＰＮＤ、航空機コックピット、ＰＤＡ、携帯電話、魚群探知機等において発生しうるが、近年は画面の角度を回転させて操作させるスマートフォンやタブレットなどのデバイスにおいて特に発生しうる問題である。さらにまた、これらのデバイスでは、従来の厚いフィルムを適用すると、軽量化のニーズに応えきれないという問題もあった。 This problem can occur in car navigation systems, PNDs, aircraft cockpits, PDAs, cell phones, fish finders, etc., where there are many opportunities to observe with polarized glasses. This is a problem that can occur particularly in devices such as. Furthermore, in these devices, there is a problem that when the conventional thick film is applied, the need for weight reduction cannot be met.
これらの問題に対し、表示デバイスの視認者側偏光板の外側（視認者側）に、複屈折性を有する光学位相差板（λ／４位相板、λ／２位相差板）を設けることで表示デバイスからの光を直線偏光から円偏光にする方法が提案されている（例えば特許文献１参照）。 For these problems, by providing an optical phase difference plate (λ / 4 phase plate, λ / 2 phase difference plate) having birefringence outside the viewer side polarizing plate of the display device (viewer side). A method has been proposed in which light from a display device is changed from linearly polarized light to circularly polarized light (see, for example, Patent Document 1).
特許文献２，３にはλ／４位相差板に使用されるフィルムの例が示されているが、用いられている樹脂は、ポリカーボネート系、ポリビニルアルコール系、ポリスチレン系、ポリメチルメタクリレート系、ポリプロピレンの如きポリオレフィン系、ポリアリレート系、ポリアミド系、ノルボルネンの如き環状オレフィンをモノマーとする環状ポリオレフィン系等が挙げられている。 Patent Documents 2 and 3 show examples of films used for λ / 4 retardation plates, but the resins used are polycarbonate, polyvinyl alcohol, polystyrene, polymethyl methacrylate, polypropylene. And polyolefins such as polyarylates, polyamides, and cyclic polyolefins using cyclic olefins such as norbornene as monomers.
一方、ポリエチレンテレフタレートなどのポリエステル樹脂からなるフィルム、特に二軸配向ポリエステルフィルムは優れた寸法安定性、剛性を有しているものの、配向による複屈折への寄与が他の樹脂に比較して大きいため、λ／４位相差板、λ／２位相差板として適用させる際に特許文献２，３に記載の位相差板よりも薄膜化することが可能で液晶デバイスの軽量化が可能となるが、これまで具体的な実施例を伴う技術が公開されてこなかった。 On the other hand, films made of polyester resins such as polyethylene terephthalate, especially biaxially oriented polyester films, have excellent dimensional stability and rigidity, but their contribution to birefringence due to orientation is greater than other resins. The λ / 4 retardation plate and the λ / 2 retardation plate can be made thinner than the retardation plates described in Patent Documents 2 and 3, and the liquid crystal device can be reduced in weight. So far, no technology with specific examples has been disclosed.
二軸配向ポリエステルフィルムにおいては、端部を把持した状態での加熱延伸により、製造されるフィルムの中央部が自重や熱収縮応力によって重力方向や製造工程の進行方向に対して引っ張られ垂れ下がることにより、工程内のフィルムが懸垂線（カテナリー曲線）を構成することに起因するボーイング（ｂｏｗｉｎｇ）という現象が生じ、フィルム幅方向での複屈折のバラツキ、フィルム幅方向での配向主軸の傾き（以下 配向角と記す）のバラツキが発生する。 In the biaxially oriented polyester film, the center part of the film to be produced is pulled and drooped in the direction of gravity or the direction of progress of the production process by its own weight or heat shrinkage stress by heat stretching in the state of gripping the end part. , A phenomenon called bowing occurs due to the fact that the film in the process forms a catenary curve (catenary curve), variation in birefringence in the film width direction, inclination of the orientation main axis in the film width direction (hereinafter referred to as orientation) (Indicated as corners).
このため、光学位相差板として使用すると、面内位相差が位置毎に不均一となるため、色あいが不均一になる問題があるほか、フィルムの光軸が幅位置毎に角度がばらつくため、偏光板の軸との角度関係も一定にならなくなることから、λ／４位相差板として使用することができないという問題があった。 For this reason, when used as an optical retardation plate, the in-plane retardation is non-uniform for each position, so there is a problem that the hue is non-uniform, and the angle of the optical axis of the film varies for each width position. Since the angle relationship with the axis of the polarizing plate is not constant, there is a problem that it cannot be used as a λ / 4 retardation plate.
このボーイングによる配向角のバラツキは、製膜しているフィルムの中心からの距離に対応して２次関数的に大きくなるため、広い幅及びフィルム中心から離れた位置での配向角のバラツキを抑制することは大きな課題とされてきた。 This variation in orientation angle due to bowing increases as a quadratic function corresponding to the distance from the center of the film being formed, so it suppresses the variation in orientation angle at a wide width and at a position away from the film center. Doing it has been a major challenge.
このような課題に対して、二軸配向ポリエステルフィルムでは次のような技術で従来対策を講じてきている。特許文献４では延伸後のフィルムを長手方向に弛緩することでボーイングを抑制したフィルムが開示されている。しかしながら、特許文献４に記載されているフィルムは厚み３０μｍレベルのフィルムであり、薄膜化すると厚みムラが大きく、面内位相差が位置毎に不均一となるため適用が困難であった。 In response to such problems, the biaxially oriented polyester film has conventionally taken countermeasures by the following technique. Patent Document 4 discloses a film in which bowing is suppressed by relaxing the stretched film in the longitudinal direction. However, the film described in Patent Document 4 is a film having a thickness of 30 μm. When the film is thinned, the thickness unevenness is large, and the in-plane retardation is nonuniform for each position, so that the application is difficult.
また二軸配向ポリエステルフィルムにおける薄膜化されたフィルムとしては特許文献５に挙げたような磁気材料用途のポリエステルフィルムが挙げられるが、これらの技術では面内位相差をλ／４位相差板に適した条件とするには不十分であった。 In addition, examples of the thinned film in the biaxially oriented polyester film include polyester films for magnetic materials as described in Patent Document 5, but these techniques are suitable for in-plane retardation for λ / 4 retardation plates. It was not enough to meet the conditions.
これらの問題に対応するため、製膜したフィルムの中心部分のみを使用する方法が従来は偏光板離型用フィルムなどの用途ではなされているが、生産性が悪くなる上に液晶デバイスのサイズが大きくなるにつれ、対応する幅の広いフィルムを採取することは困難であった。 In order to cope with these problems, the method of using only the central portion of the film formed has been conventionally used for applications such as a film for releasing a polarizing plate, but the productivity is deteriorated and the size of the liquid crystal device is reduced. As it grew larger, it was difficult to collect corresponding wide films.
表示デバイスには上述した配向角や面内位相差の不均一によって発生する色ムラやコントラストのムラが生じ難いことが強く求められているが、近年普及しているスマートフォンやタブレットなどのデバイスにおいては、表示デバイスと視認者の距離が非常に近いため、局所的な色ムラが判別しやすくなり問題となっている。この局所的な色ムラを抑制するため、特許文献６のような熱可塑性樹脂フィルムの延伸方法を改良してフィルム面内の１ｃｍ離れた２点間の位相差ムラを抑制した技術が知られているが、実用上１ｃｍよりも狭い範囲の局所的な位相差ムラが問題となるため、未だ実用上満足できる位相差板を得ることはできなかった。 Display devices are strongly demanded to be resistant to color unevenness and contrast unevenness due to the above-mentioned non-uniformity of the orientation angle and in-plane retardation, but in devices such as smartphones and tablets that have become popular in recent years Since the distance between the display device and the viewer is very close, local color unevenness can be easily identified, which is a problem. In order to suppress this local color unevenness, a technique that improves the stretching method of the thermoplastic resin film as in Patent Document 6 to suppress the phase difference unevenness between two points 1 cm apart in the film surface is known. However, since the local retardation unevenness in a range narrower than 1 cm is a problem in practice, it has not been possible to obtain a retardation plate that is still satisfactory in practical use.
本発明における課題は、上記した背景技術の問題を解消し、光学位相差板用として好適に適用できるポリエステルフィルムロールを提供することにある。 The subject in this invention is providing the polyester film roll which can eliminate the above-mentioned problem of background art and can be applied suitably for optical phase difference plates.
上記課題を解決するために鋭意検討した結果、次の特性を有することで上記課題が解決できることを見いだし、本発明に至った。 As a result of intensive studies to solve the above problems, it has been found that the above problems can be solved by having the following characteristics, and the present invention has been achieved.
（１）フィルム幅方向に対する配向主軸の傾きの角度（配向角）バラツキが６°以内であり、幅が１，２００ｍｍ以上かつ２，０００ｍｍ未満であり、面内位相差値レターデーションが５０〜２００ｎｍであって、フィルム幅方向に対する面内位相差値レターデーションのバラツキが２０ｎｍ以下であり、厚みが２μｍ以上かつ１０μｍ以下であるフィルムを巻き取ってなることを特徴とする光学位相差板用ポリエステルフィルムロール。 (1) An inclination angle (orientation angle) of the orientation main axis with respect to the film width direction is within 6 °, a width is 1,200 mm or more and less than 2,000 mm, and an in-plane retardation value retardation is 50 to 200 nm. A polyester film for an optical phase difference plate, comprising a film having a variation in in-plane retardation value retardation in the film width direction of 20 nm or less and a thickness of 2 μm or more and 10 μm or less. roll.
（２）フィルム幅方向に対する配向主軸の傾きの角度（配向角）バラツキが１０°以内であり、幅が２，０００ｍｍ以上であり、面内位相差値レターデーションが５０〜２００ｎｍであって、フィルム幅方向に対する面内位相差値レターデーションのバラツキが２０ｎｍ以下であり、厚みが２μｍ以上かつ１０μｍ以下であるフィルムを巻き取ってなることを特徴とする光学位相差板用ポリエステルフィルムロール。 (2) The inclination angle (orientation angle) variation of the orientation main axis with respect to the film width direction is within 10 °, the width is 2,000 mm or more, the in-plane retardation value retardation is 50 to 200 nm, and the film A polyester film roll for an optical phase difference plate, comprising a film having a variation in in-plane retardation value retardation in the width direction of 20 nm or less and a thickness of 2 μm or more and 10 μm or less.
（３）フィルムロール全幅及び長手方向１，２００ｍｍ以上の範囲について、局所的な位相差ムラが１０ｎｍ未満である（１）または（２）に記載する光学位相差板用ポリエステルフィルムロール。 (3) The polyester film roll for optical phase difference plates according to (1) or (2), wherein the local retardation unevenness is less than 10 nm for the entire width of the film roll and the range of 1,200 mm or more in the longitudinal direction.
（４）フィルムロールを巻き取る工程におけるフィルムの搬送速度が５０ｍ／ｍｉｎ以上かつ２００ｍ／ｍｉｎ未満である（１）〜（３）のいずれかに記載する光学位相差板用ポリエステルフィルムロールの製造方法。 (4) The manufacturing method of the polyester film roll for optical phase difference plates as described in any one of (1)-(3) whose conveyance speed of the film in the process of winding up a film roll is 50 m / min or more and less than 200 m / min. .
本発明によれば、配向主軸の傾きの角度（配向角）、面内位相差値レターデーションのバラツキを抑え、局所的な面内位相差ムラを含めた位相差値の範囲を規定することで、生産収率性を向上できる光学位相差板用ポリエステルフィルムロールを提供することが可能となる。 According to the present invention, the variation of the tilt angle of the alignment main axis (alignment angle) and in-plane retardation value retardation is suppressed, and the range of the retardation value including local in-plane retardation unevenness is defined. It becomes possible to provide a polyester film roll for an optical phase difference plate that can improve production yield.
以下、本発明の実施態様に係る光学位相差板用ポリエステルフィルムロールについてさらに詳細に説明する。本実施態様において好適に用いることのできるポリエステルは、分子配向により高強度フィルムとなるポリエステルであれば特に限定しないが、主としてポリエチレンテレフタレート、ポリエチレン−２，６−ナフタレートを含むことが好ましい。特に好ましくは価格的にも優位なポリエチレンテレフタレートである。ポリエチレンテレフタレートを用いる場合、エチレンテレフタレート以外のポリエステル共重合体成分としては、例えばジエチレングリコール、プロピレングリコール、ネオペンチルグリコール、ポリエチレングリコール、ｐ−キシリレングリコール、１，４−シクロヘキサンジメタノールなどのジオール成分、アジピン酸、セバシン酸、フタル酸、イソフタル酸、５−ナトリウムスルホイソフタル酸などのジカルボン成分、トリメリット酸、ピロメリット酸などの多官能ジカルボン酸成分、ｐ−オキシエトキシ安息香酸などが目的とするフィルム物性を阻害しない範囲で使用できる。 Hereinafter, the polyester film roll for an optical retardation plate according to an embodiment of the present invention will be described in more detail. The polyester that can be suitably used in the present embodiment is not particularly limited as long as it is a polyester that becomes a high-strength film by molecular orientation, but preferably mainly includes polyethylene terephthalate and polyethylene-2,6-naphthalate. Particularly preferred is polyethylene terephthalate which is superior in price. When polyethylene terephthalate is used, examples of polyester copolymer components other than ethylene terephthalate include diol components such as diethylene glycol, propylene glycol, neopentyl glycol, polyethylene glycol, p-xylylene glycol, and 1,4-cyclohexanedimethanol, adipine Film properties intended for dicarboxylic components such as acid, sebacic acid, phthalic acid, isophthalic acid, 5-sodium sulfoisophthalic acid, polyfunctional dicarboxylic acid components such as trimellitic acid and pyromellitic acid, and p-oxyethoxybenzoic acid Can be used as long as they do not hinder.
かかるポリエステルは、例えば以下に示す方法で製造することができる。たとえば、酸成分をジオール成分と直接エステル化反応させた後、この反応の生成物を減圧下で加熱して余剰のジオール成分を除去しつつ重縮合させることによって製造する方法や、酸成分としてジアルキルエステルを用い、これとジオール成分とでエステル交換反応させた後、上記と同様にして重縮合させることによって製造する方法等がある。この際、必要に応じて、反応触媒として例えばアルカリ金属、アルカリ土類金属、マンガン、コバルト、亜鉛、アンチモン、ゲルマニウム、チタン化合物を用いることもできる。上記ポリエステルは、固有粘度が０．４〜０．９、好ましくは０．５〜０．７、さらに好ましくは０．５５〜０．６５である。 Such a polyester can be produced, for example, by the method shown below. For example, a method in which an acid component is directly esterified with a diol component and then the product of this reaction is heated under reduced pressure to perform polycondensation while removing excess diol component, or a dialkyl as an acid component There is a method of producing an ester by transesterifying it with a diol component, followed by polycondensation in the same manner as described above. In this case, for example, an alkali metal, an alkaline earth metal, manganese, cobalt, zinc, antimony, germanium, or a titanium compound can be used as a reaction catalyst as necessary. The polyester has an intrinsic viscosity of 0.4 to 0.9, preferably 0.5 to 0.7, and more preferably 0.55 to 0.65.
本実施態様の光学位相差板用ポリエステルフィルムロール（以下、ポリエステルフィルムロール、または単にフィルムロールということがある）に適用されるポリエステルフィルムには、ポリエステル（ポリマー１）とポリイミド（ポリマー２）とを含んでいるポリマーアロイフィルムであってもよい。ここでいうポリマーアロイとは、高分子多成分系のことであり、共重合によるブロックコポリマーであってもよいし、混合などによるポリマーブレンドであってもよい。延伸性、生産性の観点からは、共重合など分子的な結合を有さないポリマーブレンドの方がより好ましい。 The polyester film applied to the polyester film roll for optical retardation plate of the present embodiment (hereinafter sometimes referred to as a polyester film roll or simply a film roll) includes polyester (polymer 1) and polyimide (polymer 2). The polymer alloy film may be included. The polymer alloy here refers to a polymer multi-component system, which may be a block copolymer by copolymerization or a polymer blend by mixing or the like. From the viewpoint of stretchability and productivity, a polymer blend having no molecular bond such as copolymerization is more preferable.
本実施態様に用いられるポリマー２は、分子鎖中にイミド基を有するポリイミドである。ポリイミドはポリエステルに対して、イミド環とベンゼン環の相互作用などに由来すると考えられる相互作用を有し、また、一般的にポリエステルよりも高いガラス転移温度を有する。このため、フィルムは製造工程において、主成分であるポリマー１のガラス転移温度に近い温度で延伸される場合に、延伸温度付近では分子運動性が低いポリイミドがポリマー１の配向結晶化による延伸性の低下をある程度阻害する働きをすることによって高倍率延伸を可能ならしめているものと推定される。 The polymer 2 used in this embodiment is a polyimide having an imide group in the molecular chain. Polyimide has an interaction considered to be derived from an interaction between an imide ring and a benzene ring or the like with respect to polyester, and generally has a glass transition temperature higher than that of polyester. For this reason, when the film is stretched at a temperature close to the glass transition temperature of polymer 1 as the main component in the production process, the polyimide having low molecular mobility near the stretching temperature has a stretchability due to orientation crystallization of polymer 1. It is presumed that high magnification stretching is made possible by acting to inhibit the decrease to some extent.
上記のポリイミドとしては、例えば、下記一般式で示されるような構造単位を含有するものが好ましい。 As said polyimide, what contains a structural unit as shown by the following general formula is preferable, for example.
また、式中のＲ２は、下記化学式で示されるような脂肪族炭化水素基、脂環族炭化水素基、芳香族炭化水素基から選ばれた一種もしくは二種以上の基を表す。R 2 in the formula represents one or more groups selected from an aliphatic hydrocarbon group, an alicyclic hydrocarbon group, and an aromatic hydrocarbon group represented by the following chemical formula.
溶融成形性やポリエステルとの親和性などの点から、下記一般式で示されるような、ポリイミド構成成分にエーテル結合を含有するポリエーテルイミドが特に好ましい。 From the viewpoints of melt moldability and affinity with polyester, a polyetherimide containing an ether bond in the polyimide component as shown by the following general formula is particularly preferred.
（ただし、上記式中Ｒ３は、６〜３０個の炭素原子を有する２価の芳香族または脂肪族残基、Ｒ４は６〜３０個の炭素原子を有する２価の芳香族残基、２〜２０個の炭素原子を有するアルキレン基、２〜２０個の炭素原子を有するシクロアルキレン基、および２〜８個の炭素原子を有するアルキレン基で連鎖停止されたポリジオルガノシロキサン基からなる群より選択された２価の有機基である。）(Wherein R 3 is a divalent aromatic or aliphatic residue having 6 to 30 carbon atoms, R 4 is a divalent aromatic residue having 6 to 30 carbon atoms, From the group consisting of alkylene groups having 2 to 20 carbon atoms, cycloalkylene groups having 2 to 20 carbon atoms, and polydiorganosiloxane groups chain-terminated with alkylene groups having 2 to 8 carbon atoms Selected divalent organic group.)
上記Ｒ３、Ｒ４としては、例えば、下記式群に示される芳香族残基を挙げることができる。As said R < 3 >, R < 4 >, the aromatic residue shown by the following formula group can be mentioned, for example.
（ｎは２以上の整数、好ましくは２０〜５０の整数） (N is an integer of 2 or more, preferably an integer of 20 to 50)
このポリエーテルイミドは、“ウルテム”（登録商標）の商品名で、ジーイープラスチックス社より入手可能である。 This polyetherimide is available from GE Plastics under the trade name “Ultem” (registered trademark).
本実施態様で用いるポリマー２は、上記のなかでも、ポリマー１と良好な親和性を有することが好ましい。なお、ここでいう良好な親和性（相溶性）を有するとは、例えば、ポリマー１とポリマー２とからなるポリマーアロイを用い、所定の混合比で溶融混合し未延伸または２軸延伸フィルムを作成し、該フィルム断面を透過型電子顕微鏡で３万〜５０万倍の倍率で観察した場合、有機粒子や無機粒子などの添加物に起因しない投影面積円相当径（以下、単に円相当径という）が５０ｎｍ以上の構造（例えば、分散不良のポリマードメインなど）が観察されないことをいう。ただし、親和性を判定する方法は特にこれに限定されるものではなく、必要に応じて、温度変調型ＤＳＣ（ＭＤＳＣ）によって単一のガラス転移点が観察されることによって良好な親和性があると判定してもよい。 Among the above, the polymer 2 used in this embodiment preferably has good affinity with the polymer 1. Here, having good affinity (compatibility) means, for example, using a polymer alloy composed of polymer 1 and polymer 2, and melt-mixing at a predetermined mixing ratio to create an unstretched or biaxially stretched film When the cross section of the film is observed with a transmission electron microscope at a magnification of 30,000 to 500,000, the projected area equivalent circle diameter (hereinafter simply referred to as equivalent circle diameter) that does not result from additives such as organic particles and inorganic particles Means that a structure of 50 nm or more (for example, a polymer domain having poor dispersion) is not observed. However, the method for determining affinity is not particularly limited to this, and if necessary, there is good affinity by observing a single glass transition point by a temperature modulation type DSC (MDSC). May be determined.
本実施態様の光学位相差板用ポリエステルフィルムロールに適用されるポリエステルフィルムは、ヘイズ値が３％以下であることが好ましい。好ましくは２％以下、さらに好ましくは１％以下である。ヘイズ値が３％より大きいと円偏光板における位相差フィルムとして使用した場合にフィルムからの散乱光が大きく、クロスニコル状態で光りモレの原因となるためである。 It is preferable that the polyester film applied to the polyester film roll for optical retardation plates of the present embodiment has a haze value of 3% or less. Preferably it is 2% or less, More preferably, it is 1% or less. This is because if the haze value is larger than 3%, the scattered light from the film is large when used as a retardation film in a circularly polarizing plate, causing light leakage in the crossed Nicol state.
本実施態様に適用されるフィルムは単層であっても、２層以上からなる複合フィルムであってもよいが、フィルムのヘイズ値を上記範囲にするには、３層複合フィルムからなる場合特に好適である。この場合、両表面層側の積層部の粒子種あるいは粒子含有量が異なる、Ａ｜Ｂ｜Ｃの構成でもよいが、同一の組成とするＡ｜Ｂ｜Ａの構成が設備的に簡易であり、生産性の面からも好ましい。さらに、両層の積層厚さを実質的に同一にした場合、品質の設計が容易である。また、片面における積層厚さは、０．５〜２．５μｍが好ましく、特に０．８〜１．５μｍが好ましい。 The film applied to the present embodiment may be a single layer or a composite film composed of two or more layers. However, in order to make the haze value of the film within the above range, particularly when it is composed of a three-layer composite film. Is preferred. In this case, the structure of A | B | C in which the particle types or particle contents of the laminated parts on both surface layers are different may be used, but the structure of A | B | A having the same composition is simple in terms of equipment. This is also preferable from the viewpoint of productivity. Further, when the thickness of both layers is substantially the same, quality design is easy. Moreover, 0.5-2.5 micrometers is preferable and, as for the lamination | stacking thickness in one side, 0.8-1.5 micrometers is especially preferable.
さらに、積層面に不活性粒子を含有し、基層部（中心層）に含有する粒子を適正化することでフィルムの搬送性・表面の平滑性及びヘイズ値を所望の範囲とすることができる。含有させる粒子の種類としては、球状シリカ、ケイ酸アルミニウム、二酸化チタン、炭酸カルシウムなどの無機粒子、またその他有機系高分子粒子としては、架橋ポリスチレン樹脂粒子、架橋シリコーン樹脂粒子、架橋アクリル樹脂粒子、架橋スチレン−アクリル樹脂粒子、架橋ポリエステル粒子、ポリイミド粒子、メラミン樹脂粒子等が好ましい。これらの１種もしくは２種以上を選択して用いることもできる。 Furthermore, the inertness particle | grains are included in a lamination | stacking surface, and the conveyance property of a film, the smoothness of a surface, and a haze value can be made into a desired range by optimizing the particle | grains contained in a base layer part (center layer). As the kind of particles to be included, inorganic particles such as spherical silica, aluminum silicate, titanium dioxide, calcium carbonate, and other organic polymer particles include crosslinked polystyrene resin particles, crosslinked silicone resin particles, crosslinked acrylic resin particles, Crosslinked styrene-acrylic resin particles, crosslinked polyester particles, polyimide particles, melamine resin particles and the like are preferable. These 1 type (s) or 2 or more types can also be selected and used.
これらの不活性粒子は、ポリエステル重合工程の段階で添加することにより、不活性粒子含有ポリマーを準備することができる。例えば、ポリエステルのグリコール成分であるエチレングリコールのスラリーとし、重縮合前のエステル交換後、あるいはエステル化後のオリゴマーの段階で不活性粒子含有スラリーを添加し、引き続き、重縮合反応を行うことで、不活性粒子含有ポリマーを得ることができる。 These inert particles can be added at the stage of the polyester polymerization process to prepare an inert particle-containing polymer. For example, by making a slurry of ethylene glycol, which is a glycol component of polyester, adding an inert particle-containing slurry after transesterification before polycondensation or at the oligomer stage after esterification, and subsequently performing a polycondensation reaction, An inert particle-containing polymer can be obtained.
また、添加前の不活性粒子のスラリーは必要に応じ、サンドグラインダー等による分散処理、遠心沈降処理による粗大粒子の分離あるいは、高精度濾過を行うことが、粒径分布を均一化でき、粗大粒子を除去することができ、フィルムの粗大突起の減少に効果的に採用できる。 In addition, if necessary, the slurry of inert particles before addition can be dispersed by a sand grinder or the like, separated by coarse particles by centrifugal sedimentation, or subjected to high-precision filtration to make the particle size distribution uniform and coarse particles. Can be effectively removed to reduce the coarse protrusions of the film.
本実施態様に適用されるフィルムでは平均粒子径０．３〜１．５μｍ、好ましく０．８〜１．３μｍの不活性粒子を０．２〜１．０質量％、さらに好ましくは、０．３〜０．８質量％含有させることが好適である。併せて、基層部に同種の不活性粒子を０．０１〜０．１質量％含有させる、基層部の粒子含有量を調整する、などにより、フィルムの搬送性・表面の平滑性及びヘイズ値を適正化することができる。 In the film applied to this embodiment, 0.2 to 1.0% by mass of inert particles having an average particle size of 0.3 to 1.5 μm, preferably 0.8 to 1.3 μm, more preferably 0.3 It is preferable to contain -0.8 mass%. In addition, by including 0.01 to 0.1% by mass of the same kind of inert particles in the base layer part, adjusting the particle content of the base layer part, etc., the film transportability, surface smoothness and haze value are adjusted. Can be optimized.
本実施態様の光学位相差板用ポリエステルフィルムロールに適用されるフィルムは、面内位相差値レターデーション（面内位相差値Ｒｅ）が５０〜２００ｎｍ、好ましくは７０〜１８０ｎｍである。面内位相差値レターデーションが５０ｎｍ未満、または２００ｎｍを超える場合、可視光の波長範囲（３６０〜７５０ｎｍ）の１／４に相当しないため、λ／４位相差フィルムとしての機能を果たすことができない。 The film applied to the polyester film roll for an optical retardation plate of this embodiment has an in-plane retardation value retardation (in-plane retardation value Re) of 50 to 200 nm, preferably 70 to 180 nm. When the in-plane retardation value retardation is less than 50 nm or more than 200 nm, it does not correspond to ¼ of the visible light wavelength range (360 to 750 nm), and therefore cannot function as a λ / 4 retardation film. .
面内位相差Ｒｅ(ｎｍ)はフィルム長手方向の屈折率ｎｘと幅方向の屈折率ｎｙ及びフィルム厚みｄ(μｍ)から、以下の式（１）で定義することができる。 The in-plane retardation Re (nm) can be defined by the following formula (1) from the refractive index nx in the film longitudinal direction, the refractive index ny in the width direction, and the film thickness d (μm).
Ｒｅ＝｜ｎｘ−ｎｙ｜／ｄ ・・・ （１） Re = | nx−ny | / d (1)
式（１）から明らかなように、本実施態様に適用されるポリエステルフィルムにおいて面内位相差を所定の範囲内となるようにするためには、長手方向・幅方向の屈折率の差分及び厚みを制御できればよい。 As apparent from the formula (1), in order to make the in-plane retardation within the predetermined range in the polyester film applied to the present embodiment, the difference in the refractive index and the thickness in the longitudinal direction and the width direction. Can be controlled.
上述のことと、ポリエチレンテレフタレートなどのポリエステル樹脂からなるフィルム、特に二軸配向ポリエステルフィルムの屈折率の差分の観点から、本実施態様に適用されるフィルム厚みは２μｍ以上１０μｍ以下であることが重要である。好ましくは３μｍ以上８μｍ以下である。フィルム厚みが１０μｍより大きいと、本実施態様に適用されるポリエステルフィルムで求める面内位相差値レターデーションを達成することが困難となる。また、２μｍ未満ではフィルムの加工性が悪く、光学位相差板用としての適用が困難となる。 From the viewpoint of the above and the difference in refractive index of a film made of a polyester resin such as polyethylene terephthalate, particularly a biaxially oriented polyester film, it is important that the film thickness applied to this embodiment is 2 μm or more and 10 μm or less. is there. Preferably they are 3 micrometers or more and 8 micrometers or less. When the film thickness is larger than 10 μm, it is difficult to achieve the in-plane retardation value retardation required for the polyester film applied to this embodiment. On the other hand, if the thickness is less than 2 μm, the processability of the film is poor and application for an optical phase difference plate becomes difficult.
また、屈折率差及び厚みにバラツキがあるフィルムでは位相差板として使用したときに部位毎に見える色が異なる現象の原因となるため、本実施態様に適用されるポリエステルフィルムではフィルム幅方向に対する面内位相差値レターデーションのバラツキ（フィルム全幅での面内位相差レターデーション最大値と最小値の差分）が２０ｎｍ以下、好ましくは１０ｎｍ以下であり、局所的な位相差ムラ（任意の隣り合う１ｃｍ以内の２点間の面内位相差レターデーションの差）が１０ｎｍ未満である。局所的な位相差ムラが１０ｎｍ以上の場合、表示デバイスの視認者が局所的な色ムラを認識してしまい、実用上満足できる位相差板を得ることができない。 In addition, in the case of a film having a refractive index difference and a variation in thickness, it causes a phenomenon in which the color seen for each part differs when used as a phase difference plate. Therefore, in the polyester film applied to this embodiment, the surface with respect to the film width direction Variation in internal retardation value retardation (difference between maximum and minimum in-plane retardation retardation over the entire film width) is 20 nm or less, preferably 10 nm or less, and local retardation unevenness (arbitrary adjacent 1 cm The difference in in-plane retardation between two points is less than 10 nm. When the local phase difference unevenness is 10 nm or more, the viewer of the display device recognizes the local color unevenness, and a practically satisfactory retardation plate cannot be obtained.
本実施態様に適用されるポリエステルフィルムの幅方向に対する面内位相差を測定する装置の例として、後述する実施例で用いたＫＯＢＲＡ−ＷＰＲ（王子計測機器社製）を挙げることができる。本明細書でいう幅方向に対する面内位相差値レターデーションは、かかる測定装置を用いて測定したものであり、本実施態様における幅方向内の面内位相差値レターデーションのバラツキは、フィルム全幅について測定したときの最大値と最小値の差分として定義されたものである。 As an example of an apparatus for measuring the in-plane retardation with respect to the width direction of the polyester film applied to this embodiment, KOBRA-WPR (manufactured by Oji Scientific Instruments) used in Examples described later can be given. The in-plane retardation value retardation with respect to the width direction in the present specification is measured using such a measuring apparatus, and the variation in the in-plane retardation value retardation within the width direction in the present embodiment is the total film width. It is defined as the difference between the maximum value and the minimum value when measured for.
また、本実施態様に適用されるポリエステルフィルムの居所的な位相差ムラを測定する装置として、後述するＫＯＢＲＡ−ＣＣＤ（王子計測機器社製）を挙げることができる。本明細書でいう局所的な位相差ムラは、かかる測定装置を用いて測定したものであり、本実施態様における局所的な位相差ムラは、測定部位の任意の隣り合う１ｃｍ以内の２点間の面内位相差値レタデーションの最大値と最小値の差分として定義されたものである。 Moreover, as an apparatus for measuring the local phase difference unevenness of the polyester film applied to this embodiment, a KOBRA-CCD (manufactured by Oji Scientific Instruments) described later can be exemplified. The local phase difference unevenness referred to in the present specification is measured using such a measuring apparatus, and the local phase difference unevenness in the present embodiment is between two adjacent points within 1 cm of the measurement site. Is defined as the difference between the maximum value and the minimum value of the in-plane retardation value retardation.
本実施態様に適用されるポリエステルフィルムは、下記ａ〜ｂのいずれかの性質を有している。 The polyester film applied to the present embodiment has any of the following properties a to b.
ａ．幅方向に対する配向主軸の傾きの角度（配向角）バラツキが６°以内であり、かつ幅が１，２００ｍｍ以上２，０００ｍｍ未満である。 a. The inclination angle (orientation angle) variation of the orientation main axis with respect to the width direction is within 6 °, and the width is not less than 1,200 mm and less than 2,000 mm.
ｂ．同バラツキが１０°以内であり、かつ幅が２，０００ｍｍ以上である。 b. The variation is within 10 °, and the width is 2,000 mm or more.
ここで配向主軸の傾きは遅相軸の方向と定義することができるが、全方位にわたってフィルムに超音波パルスを透過させ、その伝播速度を測定することによって配向性を評価し、配向主軸の傾き（配向角）を測定することができる。また、配向主軸の傾きはフィルム幅方向と平行であるときを配向角０度とし、フィルム面について時計回りの傾きを＋、反時計回りを−として表す。この配向角のバラツキは上記した各幅において上記規定の範囲内であればよいが、この配向角は傾きの符号が同一であることも好ましい。なお、この「傾きの符号が同一」とは、幅取りしたフィルム両端において、上記測定で傾きが同符号を示す状態のことをいう。 Here, the tilt of the orientation main axis can be defined as the direction of the slow axis, but the orientation is evaluated by transmitting the ultrasonic pulse through the film in all directions and measuring its propagation speed, and the tilt of the orientation main axis. (Orientation angle) can be measured. Further, the inclination of the orientation main axis is expressed as 0 degree when the orientation angle is parallel to the film width direction, and + as the clockwise inclination and-as the counterclockwise direction with respect to the film surface. The variation in the orientation angle may be within the specified range in each of the widths described above, but it is also preferable that the orientation angle has the same sign of inclination. The phrase “same inclination sign” means a state where the inclination shows the same sign in the above measurement at both ends of the widened film.
配向角バラツキとは、前述の通り測定したフィルム内の任意の位置の配向角の最大値と最小値の差分の絶対値と定義されるが、配向角バラツキが６°を超える場合（幅が１，２００ｍｍ以上２，０００ｍｍ未満）または同バラツキが１０°を超える場合（幅が２，０００ｍｍ以上）には、偏光板と貼り合わせたときに偏光板の吸収軸と光学位相差用フィルムの遅相軸の角度関係が維持されないことにより光が透過しない箇所が発生する場合がある。 The orientation angle variation is defined as the absolute value of the difference between the maximum value and the minimum value of the orientation angle at an arbitrary position in the film measured as described above, but when the orientation angle variation exceeds 6 ° (the width is 1). , 200 mm or more and less than 2,000 mm) or when the variation exceeds 10 ° (width is 2,000 mm or more), the absorption axis of the polarizing plate and the retardation of the optical retardation film when bonded to the polarizing plate There may be a portion where light is not transmitted due to the fact that the angular relationship of the axes is not maintained.
また、配向角を生じさせるボーイング現象は、工程内のフィルムが懸垂線（カテナリー曲線）を構成することに起因する現象であるため、製膜したフィルム中心からの距離が離れるほど配向角は増加する挙動をとる。この挙動は通常２次関数で近似されることが多く、配向角バラツキを最も小さいフィルムとするには製膜した中間製品ロールの中心が幅方向中心となる幅取りを行い本実施態様のフィルムロールとすることが最も良い。しかしながら、この幅取りでは中心部分のみしか、製品採取できないこととなる。さらに、近年は液晶デバイスの大画面化に伴い、光学位相差用フィルムの幅取りも大きくなってきている。幅取りは液晶デバイスの画面サイズに依存するが、配向角バラツキが大きいと前述の通り偏光板と貼り合わせたときに偏光板の吸収軸と光学位相差用フィルムの遅相軸の角度関係が維持されないことから幅取りにおいて制約を受けることになる。具体的には光学位相差用フィルムロール上から偏光板と組み合わされるに際し、枚葉（シート）とされるときの長手方向は、遅相軸の角度（配向角）に合わせて決められるが、その角度は配向角バラツキが大きいと光学位相差用フィルムを製膜したときの幅位置によって変える必要が発生する。そのため、切り出す角度の変動が大きいとロールから切り出したときに余白となり光学用位相差フィルムとして使用できない面積の割合が大きくなるため、生産性が悪くなる問題が発生する。このことから、一定の幅以上における配向角のバラツキは一定の範囲に収めることが重要となる。本実施態様におけるフィルム幅とその配向角バラツキは前述の通り、幅が１，２００ｍｍ以上２，０００ｍｍ未満で配向角バラツキが６°以内、好ましくは５°以内、または幅が２，０００ｍｍ以上で同バラツキが１０°以内、好ましくは８°以内、であれば、上記問題の解決に寄与できる。幅の上限については、上述のとおり幅取りの影響を受けるものの、フィルム加工性及び加工後の生産性を考慮すると３，０００ｍｍ以下が好ましい。 In addition, the bowing phenomenon causing the orientation angle is a phenomenon caused by the film in the process forming a catenary line (catenary curve), so the orientation angle increases as the distance from the center of the formed film increases. Take behavior. This behavior is often approximated by a quadratic function, and in order to make the film having the smallest variation in the orientation angle, the film roll of the present embodiment is formed by chamfering the center of the formed intermediate product roll as the center in the width direction. And is best. However, the product can be collected only in the central part by this width. Furthermore, in recent years, the width of the optical retardation film has been increasing with the increase in the screen size of liquid crystal devices. The width depends on the screen size of the liquid crystal device, but if the orientation angle variation is large, the angular relationship between the absorption axis of the polarizing plate and the slow axis of the optical retardation film is maintained when bonded to the polarizing plate as described above. Because it is not done, the width is limited. Specifically, when combined with a polarizing plate from above the optical retardation film roll, the longitudinal direction when it is made into a sheet (sheet) is determined according to the angle (orientation angle) of the slow axis, When the orientation angle variation is large, it is necessary to change the angle depending on the width position when the optical retardation film is formed. Therefore, if the variation in the angle to be cut out is large, the ratio of the area that becomes a blank when cut out from the roll and cannot be used as the optical retardation film is increased, resulting in a problem that productivity is deteriorated. For this reason, it is important that the variation in the orientation angle over a certain width falls within a certain range. As described above, the film width and the orientation angle variation in this embodiment are the same when the width is 1,200 mm or more and less than 2,000 mm, the orientation angle variation is within 6 °, preferably within 5 °, or the width is 2,000 mm or more. If the variation is within 10 °, preferably within 8 °, it can contribute to the solution of the above problem. The upper limit of the width is preferably 3,000 mm or less in consideration of film processability and productivity after processing, although it is affected by the width as described above.
次に本実施態様に適用されるポリエステルフィルムの製造方法に関してさらに詳しく説明する。上述したポリエステルを必要に応じて乾燥し、押出機に供給して、ポリマーをフィルターにより濾過する。ごく小さな異物もフィルム欠陥となるため、このフィルターには例えば５μｍ以上の異物を９５％以上捕集する高精度のものを用いることが有効である。続いてＴ型口金等を用いてシート状に溶融押出し、キャスティングロール上で冷却固化せしめて未延伸フィルムとする。 Next, the manufacturing method of the polyester film applied to this embodiment is demonstrated in detail. The above-described polyester is dried as necessary, and supplied to an extruder, and the polymer is filtered through a filter. Since even a very small foreign matter becomes a film defect, it is effective to use a high-precision filter that collects 95% or more of a foreign matter of 5 μm or more, for example. Subsequently, it is melt-extruded into a sheet shape using a T-type die or the like, and cooled and solidified on a casting roll to obtain an unstretched film.
溶融押出しされたポリマーシートはキャスティングロール上に接地し冷却されるが、冷却できるポリマーの熱量はキャストロールの部材の熱伝導度のために制約があり、ポリマーシート内部まで完全に冷却されない場合には得られた未延伸フィルムに配向ムラ（非晶ムラ）が発生する。この配向ムラ（非晶ムラ）が局所的な位相差ムラの原因となるため、例えばキャスティングロール速度を低速にし、ポリマーシートの冷却時間を長くすることが有効である。キャストロール速度は、次工程以降で延伸されたフィルムを巻き取る工程のフィルムの搬送速度が５０ｍ／ｍｉｎ以上２００ｍ／ｍｉｎ未満となる範囲であることが好ましく、さらに好ましくは５０ｍ／ｍｉｎ以上１５０ｍ/ｍｉｎとなる範囲である。 The melt-extruded polymer sheet is grounded and cooled on the casting roll, but the amount of heat of the polymer that can be cooled is limited by the thermal conductivity of the members of the cast roll, and if it is not completely cooled to the inside of the polymer sheet Orientation unevenness (amorphous unevenness) occurs in the obtained unstretched film. Since this alignment unevenness (amorphous unevenness) causes local phase difference unevenness, it is effective to reduce the casting roll speed and elongate the cooling time of the polymer sheet, for example. The cast roll speed is preferably in a range in which the film transport speed in the step of winding the stretched film in the subsequent steps is 50 m / min or more and less than 200 m / min, more preferably 50 m / min or more and 150 m / min. This is the range.
この未延伸フィルムを９０〜１３０℃の延伸温度で延伸することで本実施態様の光学位相差板用二軸配向ポリエステルフィルムを得る。延伸工程においては逐次延伸でも同時２軸延伸でもよい。本実施態様に適用されるポリエステルフィルムの製造においては、面内位相差値のバラツキの要因となる厚みムラを抑制することが求められるため、特に低い縦延伸倍率での長手方向における厚みムラを抑制することができる同時２軸延伸プロセスが好ましい。 The unstretched film is stretched at a stretching temperature of 90 to 130 ° C. to obtain the biaxially oriented polyester film for an optical retardation plate of the present embodiment. The stretching step may be sequential stretching or simultaneous biaxial stretching. In the production of the polyester film applied to this embodiment, since it is required to suppress the thickness unevenness that causes variations in the in-plane retardation value, the thickness unevenness in the longitudinal direction at a particularly low longitudinal draw ratio is suppressed. A simultaneous biaxial stretching process is preferred.
本実施態様に適用されるポリエステルフィルムの製造に際しては、長手方向の延伸は１段階的に、もしくは多段階的に分けて２．５〜５倍で実施し、次いで又は同時２軸延伸プロセスでは同時に幅方向に３〜６倍に延伸する。ここで、各ステップ毎に実施される延伸工程の倍率の比率について、長手方向延伸倍率／幅方向延伸倍率が１．０未満となる工程であることが好ましい。この理由としては、幅方向の配向を高くすることによって延伸工程におけるボーイングを抑制することができるためである。 In the production of the polyester film applied to this embodiment, the stretching in the longitudinal direction is carried out by 2.5 to 5 times in one step or in multiple steps, and then or simultaneously in the simultaneous biaxial stretching process. Stretch 3 to 6 times in the width direction. Here, it is preferable that the ratio of the stretching ratio performed in each step is a process in which the stretching ratio in the longitudinal direction / the stretching ratio in the width direction is less than 1.0. This is because bowing in the stretching process can be suppressed by increasing the alignment in the width direction.
また、本実施態様に適用されるポリエステルフィルムを製造する際には、幅方向延伸中の長手方向への弛緩工程を含まないことが好ましい。長手方向への弛緩工程は特許文献４に記載されているようにボーイングを抑制するために有効な方法であるものの、本実施態様に適用されるポリエステルフィルムは厚み１０μｍ以下のフィルムであるため、適用すると厚みムラが大きく面内位相差が位置毎に不均一となるためである。 Moreover, when manufacturing the polyester film applied to this embodiment, it is preferable not to include a relaxation step in the longitudinal direction during stretching in the width direction. Although the relaxation process in the longitudinal direction is an effective method for suppressing bowing as described in Patent Document 4, the polyester film applied to the present embodiment is a film having a thickness of 10 μm or less. This is because the thickness unevenness is large and the in-plane retardation is non-uniform for each position.
本実施態様に適用されるポリエステルフィルムの製造に際しては、延伸工程における延伸温度が９０℃よりも低く延伸倍率が６倍よりも大きくなるとフィルムが破断しやすくなるため、延伸温度は９０℃以上、延伸倍率は６倍未満が好ましい。 In the production of the polyester film applied to the present embodiment, the stretching temperature in the stretching step is less than 90 ° C. and the stretching ratio is more than 6 times, so that the film is easily broken. The magnification is preferably less than 6 times.
更に、１回目の幅方向に延伸する際の延伸温度は９０℃以上１００℃未満、延伸開始後の延伸工程中における昇温速度は１０℃／秒未満であることが好ましい。この理由として横配向を形成し始める初期の段階で過剰な熱を与えると熱による配向が進行してしまい、十分に横配向を進行させることができなくなるため、幅方向の配向を高くすることによって延伸工程におけるボーイングを抑制する製造プロセスを取れなくなるためである。 Further, the stretching temperature at the first stretching in the width direction is preferably 90 ° C. or more and less than 100 ° C., and the temperature increase rate during the stretching step after the start of stretching is preferably less than 10 ° C./second. The reason for this is that if excessive heat is applied at the initial stage where the lateral orientation starts to be formed, the thermal orientation will proceed and the lateral orientation cannot be sufficiently advanced. This is because a manufacturing process that suppresses bowing in the stretching process cannot be obtained.
また、本実施態様に適用されるポリエステルフィルムの製造に際しては、１回目の延伸後から熱処理工程に入るまでには冷却工程を設けないことが好ましい。特許文献５に挙げたような磁気材料用途のポリエステルフィルムではボーイングに起因する品質バラツキを抑制する方法として、熱処理工程に入る前に冷却工程を設けているが、この方法では横方向の配向が強くなり過ぎ、面内位相差を光学位相差板用に適した範囲とさせるにはフィルムを薄くさせる必要があり、加工性を満たすことが困難になるためである。 Moreover, when manufacturing the polyester film applied to this embodiment, it is preferable not to provide a cooling step after the first stretching and before entering the heat treatment step. In the polyester film for magnetic material as described in Patent Document 5, a cooling process is provided before entering the heat treatment process as a method for suppressing the quality variation caused by the bowing, but this method has a strong lateral orientation. This is because it is necessary to make the film thin in order to make the in-plane retardation within the range suitable for the optical retardation plate, and it becomes difficult to satisfy the workability.
次いで熱処理工程を経て本実施態様に適用されるポリエステルフィルムを製造する。熱処理の雰囲気温度はフィルム物性を安定させるため、フィルム上下の温度差が１〜２０℃、好ましくは１〜１０℃、さらに好ましくは１〜５℃である。フィルム上下での温度差が２０℃よりも大きいと、フィルムの幅方向の物性、特に機械的特性あるいは熱収縮率が不均一になる場合がある。上記熱処理においては、必要に応じて弛緩処理を行ってもよい。この際、横方向・長手方向いずれの方向でも良いが、横方向・長手方向を同時に行っても、これらを組み合わせておこなってもよい。弛緩率はフィルムの全幅に対して好ましくは１〜２０％、さらに好ましくは１〜１０％が熱寸法安定性の優れたフィルムを得るのに有効である。 Subsequently, the polyester film applied to this embodiment is manufactured through a heat treatment process. In order to stabilize the film physical properties, the temperature difference of the heat treatment is 1-20 ° C, preferably 1-10 ° C, more preferably 1-5 ° C. When the temperature difference between the upper and lower sides of the film is larger than 20 ° C., the physical properties in the width direction of the film, particularly the mechanical properties or the heat shrinkage rate, may become non-uniform. In the heat treatment, a relaxation treatment may be performed as necessary. At this time, either the lateral direction or the longitudinal direction may be used, but the lateral direction and the longitudinal direction may be performed simultaneously or in combination. The relaxation rate is preferably 1 to 20%, more preferably 1 to 10%, based on the entire width of the film, and is effective for obtaining a film having excellent thermal dimensional stability.
その後、熱処理工程を経た前述のフィルムを巻き取った中間製品（中間製品ロール）を得て、最後に必要とする採取幅に合わせてスリットし、本実施態様のポリエステルフィルムロールを得る。 Then, the intermediate product (intermediate product roll) which wound up the above-mentioned film which passed through the heat treatment process is obtained, and it slits according to the collection width | variety required at the end, and obtains the polyester film roll of this embodiment.
本実施態様に適用されるポリエステルフィルムでは、上述したように配向角バラツキがポイントとなる。ボーイングにより配向角バラツキが発生するため、中間製品ロールの幅方向中心をフィルムロールの中心と一致させるようにして対称的に採取することが、最も配向角バラツキを小さくした採取方法となる。一方、中心位置を含まず、中間製品ロールのどちらかの端部を含むように非対称的にフィルムロールを採取すれば、最も配向角バラツキを大きくした取り方となる（この場合、配向角の符号は同一となる）。本実施態様に適用されるポリエステルフィルムは配向角バラツキが小さいため、製膜した中間製品ロールのフィルム幅において使用可能となる幅の割合が大きく、フィルムロールとしたときに生産性が高くなる。 In the polyester film applied to this embodiment, as described above, the orientation angle variation becomes a point. Since the orientation angle variation occurs due to the bowing, it is the sampling method that minimizes the orientation angle variation to collect symmetrically so that the center in the width direction of the intermediate product roll coincides with the center of the film roll. On the other hand, if the film roll is sampled asymmetrically so as to include one end of the intermediate product roll without including the center position, the orientation angle variation is maximized (in this case, the sign of the orientation angle). Are the same). Since the polyester film applied to this embodiment has a small orientation angle variation, the ratio of the width that can be used in the film width of the formed intermediate product roll is large, and the productivity becomes high when the film roll is formed.
本実施態様のポリエステルフィルムロールから得られるポリエステルフィルムは、二軸延伸による薄膜化と強力化により、従来よりもはるかに薄い厚みの位相差板となり、各種液晶ディスプレイ機器への組み込み時の省スペース化を実現できる。さらには、液晶ディスプレイから放出される偏光を楕円偏光または円偏光にすることにより、偏光眼鏡をかけた状態で液晶ディスプレイ機器を用いても、その機器の回転方向（縦型や横型での使用）の変化に対しても、光量のムラや色合いの変化を抑えることができ、機器操作時の視認性を確保し続けることができる。 The polyester film obtained from the polyester film roll of this embodiment becomes a retardation film with a much thinner thickness than before by thinning and strengthening by biaxial stretching, saving space when incorporated into various liquid crystal display devices. Can be realized. Furthermore, the polarized light emitted from the liquid crystal display is made elliptical or circularly polarized, so even if the liquid crystal display device is used with polarized glasses, the direction of rotation of the device (use in vertical or horizontal) Therefore, it is possible to suppress unevenness in the amount of light and change in hue, and to keep visibility during device operation.
実施例および比較例における特性値の測定方法は次の通りである。 The measuring method of the characteristic value in an Example and a comparative example is as follows.
（１）採取幅
採取した測定対象のフィルムを台に広げ、幅を金尺（ＪＩＳ１級）で測定した。(1) Sampling width The sampled film to be measured was spread on a table, and the width was measured with a metal scale (JIS class 1).
（２）配向主軸の傾き（配向角）、配向角バラツキ
野村商事製ＳＯＮＩＣ ＳＨＥＥＴ ＴＥＳＴＥＲ（ＳＳＴ−２５０）を用いて測定を行った。試料となるフィルムの幅に対して同じ位置になるように３０枚重ねで両端部からＡ４サイズに切り出したサンプルの中点（１０５ｍｍ）を測定した。サンプル切り出し時の角度誤差を補正するため、測定は表裏で行い、表裏での測定結果の絶対値を平均した値を測定値とし、配向主軸がフィルム幅方向と平行である時を配向角０度とし、フィルム面に対して時計回りの傾きを＋、反時計回りを−として評価した。(2) Tilt of orientation main axis (orientation angle), variation in orientation angle Measurement was carried out using a SONIC SHEET TESTER (SST-250) manufactured by Nomura Corporation. The midpoint (105 mm) of a sample cut into A4 size from both ends in a stack of 30 sheets so as to be at the same position as the width of the film as a sample was measured. In order to correct the angle error at the time of cutting out the sample, the measurement is performed on the front and back sides, the average value of the measurement results on the front and back sides is taken as the measurement value, and the orientation angle is 0 degree when the orientation main axis is parallel to the film width direction. The clockwise inclination with respect to the film surface was evaluated as +, and the counterclockwise direction was evaluated as-.
配向角バラツキは対象となる採取幅取りにおいて、最大値と最小値の差分の絶対値を測定結果とした。 For the orientation angle variation, the absolute value of the difference between the maximum value and the minimum value was taken as the measurement result in the sampling width measurement.
（３）フィルム厚み
ＪＩＳ Ｃ２１５１（１９９０）に準じ、マイクロメーター（ミツトヨＯＭＭ−２５）を用いて測定をした。試料となるフィルムの幅方向に対して均等に３点測定し、その平均値を測定結果とした。(3) Film thickness According to JIS C2151 (1990), the film thickness was measured using a micrometer (Mitutoyo OMM-25). Three points were measured evenly in the width direction of the film as a sample, and the average value was taken as the measurement result.
（４）フィルム幅方向に対する面内位相差値レターデーション（ｎｍ）
王子計測機器社製ＫＯＢＲＡ−ＷＰＲを用いて測定を行った。対象となる採取幅取りにおいて、試料となるフィルムを切り出し、装置にセットした。位相差測定ソフトＫＯＢＲＡ−ＲＥを起動し、“測定法”を“標準”として、波長５８６．９ｎｍの光にて測定を実施し、入力するフィルム厚みは上述の（３）で測定した値を入力して算出させたＲｅ（ｎｍ）を測定値とした。測定は対象となる採取幅取りにおいて、両端及び中央より切り出したサンプルで行い、その測定値の変動範囲を確認した。(4) In-plane retardation value retardation in the film width direction (nm)
Measurement was performed using KOBRA-WPR manufactured by Oji Scientific Instruments. In the sampling width of the object, a film as a sample was cut out and set in the apparatus. Start the phase difference measurement software KOBRA-RE, set the “measurement method” to “standard”, measure the light with a wavelength of 586.9 nm, and enter the value measured in (3) above for the input film thickness. The Re (nm) calculated in this way was taken as the measured value. Measurement was performed on samples cut from both ends and the center in the sampling width measurement, and the fluctuation range of the measured values was confirmed.
面内位相差値レターデーションのバラツキは対象となる採取幅取りにおいて、最大値と最小値の差分を測定結果とした。 The variation in the in-plane retardation value retardation was determined by measuring the difference between the maximum value and the minimum value in the target sampling width.
（５）局所的な面内位相差値レターデーション（ｎｍ）
王子計測機器社製ＫＯＢＲＡ−ＣＣＤを用いて測定を行った。対象となる採取幅取りにおいて、フィルムロール全幅から採取したサンプルをクロスニコル状態及びパラニコル状態に対峙させた２枚の偏光板の間に配置し、一方の側からフィルムに直角に光をあて、光の投射方向の反対側から目視で観察し、色ムラの有無を確認した。色ムラが確認された部位のフィルムを切り出し、ＫＯＢＲＡ−ＣＣＤを用いて色ムラ部分と正常部分の面内位相差値レターデーションを測定した。
局所的な位相差ムラは、測定部位の任意の隣り合う１ｃｍ以内の２点間の面内位相差値レターデーションの最大値と最小値の差分とした。(5) Local in-plane retardation value retardation (nm)
Measurement was performed using a KOBRA-CCD manufactured by Oji Scientific Instruments. In the sampling width of the target, the sample collected from the entire width of the film roll is placed between two polarizing plates facing the crossed Nicol state and the Paranicol state, and light is projected from one side at a right angle to the film. The presence or absence of color unevenness was confirmed by visual observation from the opposite side of the direction. The film of the portion where the color unevenness was confirmed was cut out, and the in-plane retardation value retardation of the color uneven portion and the normal portion was measured using KOBRA-CCD.
The local retardation unevenness was defined as the difference between the maximum value and the minimum value of the in-plane retardation value retardation between two points within 1 cm adjacent to each other at the measurement site.
（６）フィルム長手方向の厚みむら
安立電気製フィルム厚み連続測定器を用いて、長手方向に１５ｍ測定し、記録されたフィルム厚さチャートから、最大厚みと最小厚みの差を厚みむら（μｍ）として測定した。測定条件は下記の通り。(6) Uneven thickness in the longitudinal direction of the film Using a continuous film thickness measuring instrument manufactured by Anritsu Electric Co., Ltd., measured for 15 m in the longitudinal direction, and from the recorded film thickness chart, the thickness unevenness (μm) As measured. The measurement conditions are as follows.
構成：Ｋ−３０６Ｃ広範囲電子マイクロメータ、Ｋ−３１０Ｃレコーダー、フィルム送り装置
検出器：３Ｒルビー端子、測定力：１５ｇ±５ｇ
フィルム幅：４５ｍｍ、測定長：１５ｍ、フィルム送り速度：３ｍ／分Configuration: K-306C Wide Range Electronic Micrometer, K-310C Recorder, Film Feeder Detector: 3R Ruby Terminal, Measuring Force: 15g ± 5g
Film width: 45 mm, measurement length: 15 m, film feed rate: 3 m / min
（７）フィルムのヘイズ値
ＪＩＳ Ｋ７１０５（１９８１）に準じ、フィルム長手方向４ｃｍ×フィルム幅方向３．５ｃｍの寸法に切り出したものをサンプルとし、ヘイズメータ（スガ試験機製ＨＧＭ−２ＤＰ（Ｃ光用））を用いて測定した。フィルム幅方向に対して均等に３点測定し、その平均値を測定結果とした。(7) Haze value of film According to JIS K7105 (1981), a sample cut into a dimension of 4 cm in the longitudinal direction of the film and 3.5 cm in the width direction of the film is used as a sample, and a haze meter (HGM-2DP manufactured by Suga Test Instruments (for C light)) It measured using. Three points were measured uniformly in the film width direction, and the average value was taken as the measurement result.
（８）熱収縮率
フィルム表面に、幅１０ｍｍ、測定長約１００ｍｍとなるように２本のラインを引き、この２本のライン間の距離を２３℃で測定しこれをＬ０とする。このフィルムサンプルを１００℃のオーブン中に３０分間、１．５ｇの荷重下で放置した後、再び２本のライン間の距離を２３℃で測定しこれをＬ１とし、下式により熱収縮率を求めた。(8) Heat shrinkage rate Two lines are drawn on the film surface so as to have a width of 10 mm and a measurement length of about 100 mm, and the distance between the two lines is measured at 23 ° C. and is defined as L0. This film sample was left in an oven at 100 ° C. for 30 minutes under a load of 1.5 g, and then the distance between the two lines was measured again at 23 ° C., and this was taken as L1. Asked.
熱収縮率（％）＝｛（Ｌ０−Ｌ１）／Ｌ０｝×１００ Thermal contraction rate (%) = {(L0−L1) / L0} × 100
フィルムの長手方法および幅方向についてそれぞれ３カ所の測定を行い、平均値を求めた。 Measurement was carried out at three points for the longitudinal direction and the width direction of the film, and the average value was obtained.
実施例１：
テレフタル酸４１．１質量部とエチレングリコールの反応物であるビス−β−ヒドロキシエチルテレフタレート（以下、ＢＨＴという）４６．４質量部を、予め２５５℃の溶融状態で貯留させ、さらにテレフタル酸４５．３質量部とエチレングリコール１９．５質量部からなるスラリーを、反応槽の温度を保ち定量供給しながら、水を留出させ、エステル化反応をさせた。反応を開始してから４時間４０分後にエステル化を終了し、この反応生成物であるＢＨＴを重縮合反応槽に移し、トリメチルフォスフェート０．０２質量部添加した。次いで、酢酸マグネシウム０．０６質量部、酢酸リチウム０．００１質量部、三酸化アンチモン０．０２質量部を添加して、４０分で２５Ｐａになるまで減圧するとともに２９０℃まで加熱、昇温して重縮合反応を行い、固有粘度０．６２に到達まで実施した。反応終了後、重縮合反応槽底部にある口金より冷水中にストランド状に吐出し、押し出しカッターによって円柱状にペレット化したホモポリエステルペレット１を得た。Example 1:
46.4 parts by mass of bis-β-hydroxyethyl terephthalate (hereinafter referred to as BHT), which is a reaction product of 41.1 parts by mass of terephthalic acid and ethylene glycol, was previously stored in a molten state at 255 ° C., and 45. While the slurry consisting of 3 parts by mass and 19.5 parts by mass of ethylene glycol was quantitatively supplied while maintaining the temperature of the reaction vessel, water was distilled off to cause esterification. Esterification was completed 4 hours and 40 minutes after the start of the reaction, and BHT as this reaction product was transferred to a polycondensation reaction tank, and 0.02 part by mass of trimethyl phosphate was added. Next, 0.06 parts by mass of magnesium acetate, 0.001 parts by mass of lithium acetate, and 0.02 parts by mass of antimony trioxide are added, and the pressure is reduced to 25 Pa in 40 minutes, and the temperature is increased to 290 ° C. A polycondensation reaction was carried out until the intrinsic viscosity reached 0.62. After completion of the reaction, a homopolyester pellet 1 was discharged in the form of a strand into cold water from the die at the bottom of the polycondensation reaction tank and pelletized into a cylindrical shape by an extrusion cutter.
このホモポリエステルペレット１を固相重合することで得られた固有粘度０．８５（ｄｌ／ｇ）のポリエチレンテレフタレート（ＰＥＴ）のペレット（Ｔｇ８０℃）５０質量部とＧｅｎｅｒａｌ Ｅｌｅｃｔｒｉｃ（ＧＥ）社製の固有粘度０．６８（ｄｌ／ｇ）の”ウルテム”１０１０（Ｔｇ２１６℃）（ＰＥＩ）５０質量部とを、２９０℃に加熱された同方向回転タイプのベント式２軸混練押出機に供給して、ＰＥＩを５０質量％含有したＰＥＴ／ＰＥＩブレンドチップを作製した。 50 parts by mass of polyethylene terephthalate (PET) pellets (Tg 80 ° C.) having an intrinsic viscosity of 0.85 (dl / g) obtained by solid-phase polymerization of the homopolyester pellets 1 and a specific product manufactured by General Electric (GE) 50 parts by weight of “Ultem” 1010 (Tg 216 ° C.) (PEI) having a viscosity of 0.68 (dl / g) is supplied to a bent-type twin-screw kneading extruder of the same direction rotation type heated to 290 ° C. A PET / PEI blend chip containing 50% by mass of PEI was prepared.
また、ジメチルテレフタレート１００質量部とエチレングリコール７０質量部とに、エステル交換反応触媒として、酢酸マグネシウム４水塩をマグネシウム原子数換算として４０ｐｐｍとなるように添加し、１５０℃から２２５℃に徐々に昇温しながら反応させ、その後、ジエチルホスホノ酢酸エチルをリン原子数換算で１０ｐｐｍ添加した。更に、５分後に平均粒径が０．０６μｍで、あらかじめ粒子のＥＧ溶液をプレフィルターとして絶対濾過精度３．０μｍ、メインフィルターとして絶対濾過精度１．０μｍのフィルターで濾過した球状シリカ粒子ＥＧスラリーを反応組成物に対して１．０質量％となるように１５分かけて添加した。更に、５分後に三酸化アンチモン０．０３質量部を加え、重縮合反応容器に移し、２９０℃まで昇温し最終的に２５Ｐａの高減圧下にて重縮合反応を行い、ＩＶ０．６１のポリエステルペレット２を得た。 Further, magnesium acetate tetrahydrate was added to 100 parts by mass of dimethyl terephthalate and 70 parts by mass of ethylene glycol as a transesterification reaction catalyst so as to be 40 ppm in terms of the number of magnesium atoms, and gradually increased from 150 ° C. to 225 ° C. The reaction was conducted while warming, and then 10 ppm of ethyl diethylphosphonoacetate was added in terms of the number of phosphorus atoms. Further, after 5 minutes, a spherical silica particle EG slurry having an average particle size of 0.06 μm, filtered in advance with a filter having an absolute filtration accuracy of 1.0 μm as a main filter and an absolute filtration accuracy of 3.0 μm as a pre-filter of the particle EG solution. It added over 15 minutes so that it might become 1.0 mass% with respect to the reaction composition. Further, 0.05 parts by mass of antimony trioxide was added after 5 minutes, transferred to a polycondensation reaction vessel, heated to 290 ° C., and finally subjected to a polycondensation reaction under a high vacuum of 25 Pa. Pellets 2 were obtained.
また、２８０℃に加熱された同方向回転タイプのベント式２軸混練押出機に、上述のホモポリエステルペレット１を９８質量部と平均径０．３μｍの球状架橋ポリスチレン粒子の１０質量％水スラリーを２０質量部（球状架橋ポリスチレンとして２質量部）供給し、ベント孔を１ｋＰａ以下の減圧度に保持し水分を除去し、平均径０．３μｍの球状架橋ポリスチレン粒子を２質量部含有する固有粘度０．６１のポリエステルペレット３を得た。 In addition, 98 parts by mass of the homopolyester pellet 1 and 10 mass% water slurry of spherical cross-linked polystyrene particles having an average diameter of 0.3 μm were added to a vent-type biaxial kneading extruder of the same direction rotation type heated to 280 ° C. 20 parts by mass (2 parts by mass as spherical cross-linked polystyrene) is supplied, the vent hole is maintained at a reduced pressure of 1 kPa or less, moisture is removed, and 2 parts by mass of spherical cross-linked polystyrene particles having an average diameter of 0.3 μm are contained. .61 polyester pellets 3 were obtained.
次いで、２７０℃に加熱された押出機Ａには、上記ペレタイズ操作により作製したＰＥＴ／ＰＥＩブレンドチップ６質量部と上述のホモポリエステルペレット１を７４質量部と上述のポリエステルペレット２を２０質量部との混合原料を、１６０℃で３時間減圧乾燥した後に供給した。 Next, in Extruder A heated to 270 ° C., 6 parts by mass of the PET / PEI blend chip prepared by the above pelletizing operation, 74 parts by mass of the above-mentioned homopolyester pellet 1 and 20 parts by mass of the above-mentioned polyester pellet 2 were obtained. The mixed raw materials were supplied after drying under reduced pressure at 160 ° C. for 3 hours.
なお、上記した球状シリカ粒子は、ナトリウム水ガラスと水とを投入して珪酸ナトリウム水溶液を調製した後に還流下硫酸水溶液を加え、引き続還流下熟成することにより得たシリカゾルを限外濾過膜を使用して濃縮後、エチレングリコールを加えロータリーエバポレーターにて１００℃で溶媒置換を行いシリカゾルとして得たものを使用した。 The spherical silica particles described above were prepared by adding sodium water glass and water to prepare a sodium silicate aqueous solution, adding a sulfuric acid aqueous solution under reflux, and subsequently aging under reflux to obtain a silica sol as an ultrafiltration membrane. After concentration by use, ethylene glycol was added, and solvent substitution was performed at 100 ° C. with a rotary evaporator to obtain a silica sol.
また、上述の球状架橋ポリスチレン粒子はソープフリー乳化重合によりシード粒子を合成し、膨潤助剤を用いて膨潤させ、重合性モノマーを吸収して重合させる方法で製造した。重合性モノマーを吸収させる方法としては、シード粒子を合成した水溶性分散体に対してこれらを一括添加する方法を採用した。 The spherical crosslinked polystyrene particles described above were produced by a method in which seed particles were synthesized by soap-free emulsion polymerization, swollen with a swelling aid, and absorbed and polymerized. As a method for absorbing the polymerizable monomer, a method of collectively adding these to the water-soluble dispersion synthesized with the seed particles was adopted.
一方、押出機Ｂも同様に２７０℃に加熱し、上記ペレタイズ操作により作製したＰＥＴ／ＰＥＩブレンドチップ６質量部と上述のホモポリエステルペレット１を７８質量部と上述のポリエステルペレット３を２０質量部との混合原料を、１６０℃で３時間減圧乾燥した後に供給した。 On the other hand, the extruder B is similarly heated to 270 ° C., and 6 parts by mass of the PET / PEI blend chip prepared by the above pelletizing operation, 78 parts by mass of the above-mentioned homopolyester pellet 1 and 20 parts by mass of the above-mentioned polyester pellet 3 The mixed raw materials were supplied after drying under reduced pressure at 160 ° C. for 3 hours.
押出機Ａ、Ｂではそれぞれ、５μｍ以上の捕集効率９５％の高精度フィルターで濾過した後、矩形の２層用合流ブロックで合流積層し、前述の押出機Ａから供給されたポリエステル：前述の押出機Ｂから供給されたポリエステルが厚み比で６：１となるように２層積層とした。その後、２８５℃に保ったスリットダイを介し静電印加キャスト法を用いて表面温度２５℃のキャスティングロール上に冷却固化し、未延伸フィルムを得た。この未延伸フィルムを同時２軸延伸テンターに導き、長手方向および幅方向に同時に、温度９５℃、３．５０倍×３．６５倍延伸した。この延伸工程における昇温速度は１℃／秒以下であった。続いて、冷却工程を経ることなく温度１９０℃で長手方向および幅方向に同時に１．２０倍×１．３５倍に再延伸した。その後、温度２１５℃で５．５秒間熱処理後、幅方向に１．７５％の弛緩処理を行った。その後、１３０ｍ／ｍｉｎのフィルム搬送速度で巻き取って５ｍ幅の中間製品ロールを作成した。中間製品ロールから、表１に記載の評価ロール採取幅にスリットして巻き取り、厚さ５μｍのポリエステルフィルムロールを評価用に作製した。作製した評価ロール（本実施態様のポリエステルフィルムロール）の特性評価を行うに際しては５ｍ幅の中間製品ロールからその端部を含むように表１に記載の幅で評価ロールを採取し、サンプルフィルムを切り出して採取して特性値の測定や評価を行い、得られた結果を表１に示した。 In each of the extruders A and B, after filtering with a high-precision filter having a collection efficiency of 95% of 5 μm or more, the layers are merged and stacked in a rectangular two-layer merge block, and the polyester supplied from the aforementioned extruder A: Two layers were laminated so that the polyester supplied from the extruder B had a thickness ratio of 6: 1. Thereafter, the film was cooled and solidified on a casting roll having a surface temperature of 25 ° C. using an electrostatic application casting method through a slit die maintained at 285 ° C. to obtain an unstretched film. This unstretched film was led to a simultaneous biaxial stretching tenter and stretched at a temperature of 95 ° C. and 3.50 times × 3.65 times at the same time in the longitudinal and width directions. The temperature rising rate in this stretching step was 1 ° C./second or less. Subsequently, the film was re-stretched at a temperature of 190 ° C. in the longitudinal direction and the width direction simultaneously at 1.20 times × 1.35 times without passing through a cooling step. Thereafter, after heat treatment at a temperature of 215 ° C. for 5.5 seconds, 1.75% relaxation treatment was performed in the width direction. Then, it wound up with the film conveyance speed of 130 m / min, and created the intermediate product roll of 5 m width. From the intermediate product roll, it was slit and wound into the evaluation roll collection width shown in Table 1, and a 5 μm thick polyester film roll was prepared for evaluation. When evaluating the characteristics of the prepared evaluation roll (polyester film roll of the present embodiment), an evaluation roll was collected with a width shown in Table 1 so as to include the end portion of the 5 m wide intermediate product roll, and a sample film was prepared. It cut out and extract | collected, the characteristic value was measured and evaluated, and the obtained result was shown in Table 1.
実施例２，比較例１：
延伸条件、冷却条件、熱処理温度などの製膜条件を表１記載の通りに変更したほかは実施例１と同様に実施した。得られたフィルムの特性を表１に示した。Example 2, Comparative Example 1:
The same procedure as in Example 1 was performed except that the film forming conditions such as stretching conditions, cooling conditions, and heat treatment temperature were changed as shown in Table 1. The properties of the obtained film are shown in Table 1.
実施例３〜４，比較例２：
押出機Ａに上述のホモポリエステルペレット１を９９質量部と上述のポリエステルペレット２を２０質量部との混合原料を、１６０℃で３時間減圧乾燥した後に供給し、逐次２軸方式にて表１に従って延伸条件、冷却条件、熱処理温度などの製膜条件を変え、その他は実施例１と同様に実施し、二軸配向ポリエステルフィルムを得た。得られたフィルムの特性を表１に示した。Examples 3-4, Comparative Example 2:
A mixed raw material of 99 parts by mass of the above-described homopolyester pellets 1 and 20 parts by mass of the above-described polyester pellets 2 is supplied to the extruder A after being dried under reduced pressure at 160 ° C. for 3 hours, and successively in a biaxial manner. The film forming conditions such as stretching conditions, cooling conditions, and heat treatment temperature were changed according to the same procedures as in Example 1 to obtain a biaxially oriented polyester film. The properties of the obtained film are shown in Table 1.
実施例、比較例におけるフィルムの位相差板用としての評価：
フラットイルミネーター（ＨＦ−ＳＬ−１００ＷＬＣＧ；電通産業製）の発光面に合う大きさの偏光板１枚を乗せ、観察対象とした同じサイズの実施例及び比較例のフィルムを積層した状態とし、フラットイルミネーターの電源を入れ、直線偏光が対象フィルムを通過した状態を作った。この状態で更に別の同じ大きさの偏光板を乗せ、対象フィルムの上に乗せた偏光板だけを０〜３６０°回転させて観察し、回転させている最中に評価対象のフィルムを通した光について位置毎のムラ及び色合いの変化を観察した。Evaluation as films for retardation films of Examples and Comparative Examples:
Put one polarizing plate of a size that fits the light emitting surface of a flat illuminator (HF-SL-100WLCG; manufactured by Dentsu Sangyo), and laminate the films of the same size examples and comparative examples to be observed. The illuminator was turned on and the linearly polarized light passed through the target film. In this state, another polarizing plate of the same size was placed, and only the polarizing plate placed on the target film was observed by rotating it by 0 to 360 °, and the evaluation target film was passed through while rotating. The light was observed for unevenness and color change at each position.
実施例１〜４のフィルムでは位置毎のムラや色合いの変化が少なく、光学位相差用フィルムとして好適に利用できることを確認した。一方で比較例１、２のフィルムでは位置毎のムラや色合いの変化が大きいため、光学位相差用フィルムとして利用するには不適であることを確認した。 In the films of Examples 1 to 4, it was confirmed that there was little unevenness and color change at each position, and the film could be suitably used as an optical retardation film. On the other hand, it was confirmed that the films of Comparative Examples 1 and 2 are unsuitable for use as an optical retardation film because of unevenness and color change at each position.
本発明に係る光学位相差板用ポリエステルフィルムロールは、液晶表示用部材等を構成する材料として広く利用可能である。 The polyester film roll for an optical retardation plate according to the present invention can be widely used as a material constituting a liquid crystal display member or the like.
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| JP6163867B2 (en) * | 2013-05-18 | 2017-07-19 | 三菱ケミカル株式会社 | Optical polyester film |
| JP6442869B2 (en) * | 2014-05-21 | 2018-12-26 | 大日本印刷株式会社 | Hard coat film, front plate and display device of display element using the same, and method for improving peeling resistance of thin hard coat film |
| JP6732407B2 (en) * | 2015-03-20 | 2020-07-29 | 日東電工株式会社 | Optical laminate, method for manufacturing the same, and image display device using the optical laminate |
| JP7086519B2 (en) * | 2015-11-20 | 2022-06-20 | 東レ株式会社 | Biaxially oriented polyester film |
| JP6806082B2 (en) * | 2015-12-01 | 2021-01-06 | Ａｇｃ株式会社 | Transparent screen sheet, transparent screen, and video display system |
| TWI649591B (en) * | 2016-05-31 | 2019-02-01 | 南韓商Ｓｋｃ股份有限公司 | Protective film for polarizing member, polarizing plate including the same, and display device having the same |
| KR101694258B1 (en) * | 2016-06-20 | 2017-01-09 | 에스케이씨 주식회사 | A protective film for a polarizer, a polarizing plate comprising the same, and a display device with the polarizing plate |
| KR101694257B1 (en) * | 2016-06-20 | 2017-01-10 | 에스케이씨 주식회사 | A protective film for a polarizer, a polarizing plate comprising the same, and a display device with the polarizing plate |
| JP6957885B2 (en) * | 2017-01-31 | 2021-11-02 | 東レ株式会社 | Films and laminated sheets for organic electroluminescence display devices |
| KR102438415B1 (en) * | 2020-09-03 | 2022-08-30 | 도레이첨단소재 주식회사 | Optical polyester protection film |
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| WO2007023929A1 (en) * | 2005-08-26 | 2007-03-01 | Konica Minolta Opto, Inc. | Film and method for producing same, polarizing plate using same, and liquid crystal display |
| JP2009139753A (en) * | 2007-12-07 | 2009-06-25 | Nitto Denko Corp | Polarizing plate, optical film and image display device |
| WO2010082620A1 (en) * | 2009-01-19 | 2010-07-22 | 株式会社カネカ | Method for manufacturing phase difference film, optical film, image display apparatus, liquid crystal display apparatus, and phase difference film |
-
2013
- 2013-02-25 CN CN201380012301.XA patent/CN104160306A/en active Pending
- 2013-02-25 JP JP2013544954A patent/JPWO2013133064A1/en active Pending
- 2013-02-25 KR KR1020147026532A patent/KR20140143370A/en not_active Application Discontinuation
- 2013-02-25 WO PCT/JP2013/054712 patent/WO2013133064A1/en active Application Filing
- 2013-03-06 TW TW102107818A patent/TW201347963A/en unknown
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007023929A1 (en) * | 2005-08-26 | 2007-03-01 | Konica Minolta Opto, Inc. | Film and method for producing same, polarizing plate using same, and liquid crystal display |
| JP2009139753A (en) * | 2007-12-07 | 2009-06-25 | Nitto Denko Corp | Polarizing plate, optical film and image display device |
| WO2010082620A1 (en) * | 2009-01-19 | 2010-07-22 | 株式会社カネカ | Method for manufacturing phase difference film, optical film, image display apparatus, liquid crystal display apparatus, and phase difference film |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20140143370A (en) | 2014-12-16 |
| WO2013133064A1 (en) | 2013-09-12 |
| CN104160306A (en) | 2014-11-19 |
| TW201347963A (en) | 2013-12-01 |
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