WO2023189797A1 - Method for manufacturing polarizing film - Google Patents
Method for manufacturing polarizing film Download PDFInfo
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- WO2023189797A1 WO2023189797A1 PCT/JP2023/010809 JP2023010809W WO2023189797A1 WO 2023189797 A1 WO2023189797 A1 WO 2023189797A1 JP 2023010809 W JP2023010809 W JP 2023010809W WO 2023189797 A1 WO2023189797 A1 WO 2023189797A1
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- WIPO (PCT)
- Prior art keywords
- polarizing film
- film
- transparent protective
- protective film
- polarizing
- Prior art date
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 15
- 230000001681 protective effect Effects 0.000 claims abstract description 66
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- QWMJEUJXWVZSAG-UHFFFAOYSA-N (4-ethenylphenyl)boronic acid Chemical compound OB(O)C1=CC=C(C=C)C=C1 QWMJEUJXWVZSAG-UHFFFAOYSA-N 0.000 description 1
- BTJPUDCSZVCXFQ-UHFFFAOYSA-N 2,4-diethylthioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC(CC)=CC(CC)=C3SC2=C1 BTJPUDCSZVCXFQ-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- RDFQSFOGKVZWKF-UHFFFAOYSA-N 3-hydroxy-2,2-dimethylpropanoic acid Chemical compound OCC(C)(C)C(O)=O RDFQSFOGKVZWKF-UHFFFAOYSA-N 0.000 description 1
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- KLDXJTOLSGUMSJ-JGWLITMVSA-N Isosorbide Chemical compound O[C@@H]1CO[C@@H]2[C@@H](O)CO[C@@H]21 KLDXJTOLSGUMSJ-JGWLITMVSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
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- 239000004743 Polypropylene Substances 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
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- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
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- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 description 1
- 229910000024 caesium carbonate Inorganic materials 0.000 description 1
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- 239000003054 catalyst Substances 0.000 description 1
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- 238000007796 conventional method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 description 1
- 210000002858 crystal cell Anatomy 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 125000004386 diacrylate group Chemical group 0.000 description 1
- ROORDVPLFPIABK-UHFFFAOYSA-N diphenyl carbonate Chemical compound C=1C=CC=CC=1OC(=O)OC1=CC=CC=C1 ROORDVPLFPIABK-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
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- 239000003112 inhibitor Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
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- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
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- 239000000314 lubricant Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
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- JFNLZVQOOSMTJK-KNVOCYPGSA-N norbornene Chemical compound C1[C@@H]2CC[C@H]1C=C2 JFNLZVQOOSMTJK-KNVOCYPGSA-N 0.000 description 1
- 125000003518 norbornenyl group Chemical group C12(C=CC(CC1)C2)* 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- OTLDLKLSNZMTTA-UHFFFAOYSA-N octahydro-1h-4,7-methanoindene-1,5-diyldimethanol Chemical compound C1C2C3C(CO)CCC3C1C(CO)C2 OTLDLKLSNZMTTA-UHFFFAOYSA-N 0.000 description 1
- 239000008188 pellet 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
- 239000000049 pigment Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
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- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
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- 239000009719 polyimide resin Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
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- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-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
Abstract
Provided is a method for manufacturing a polarizing film in which a polarizing membrane and a transparent protective film are directly joined without using a pressure-sensitive-adhesive layer or an adhesive layer, wherein the method for manufacturing a polarizing film includes: a step for producing a layered body by irradiating an affixing surface of at least one of the polarizing membrane and the transparent protective film with ultraviolet light to perform surface treatment thereof, and then affixing the polarizing membrane and the transparent protective film via a volatile solvent; and a step for heating the resultant layered body and thereby draying the volatile solvent to join the polarizing membrane and the transparent protective film. This method for manufacturing a polarizing film is able to suppress curl and has excellent bonding strength between the polarizing membrane and the transparent protective film despite not using a pressure-sensitive-adhesive layer or an adhesive layer.
Description
本発明は、偏光フィルムの製造方法に関する。
The present invention relates to a method for manufacturing a polarizing film.
従来、液晶表示装置や有機ＥＬ表示装置等の各種画像表示装置に用いる偏光膜としては、高透過率と高偏光度を兼ね備えていることから、染色処理された（ヨウ素や二色性染料等の二色性物質を含有する）ポリビニルアルコール系フィルムが用いられている。当該偏光膜は、ポリビニルアルコール系フィルムに、浴中にて、例えば、膨潤、染色、架橋、延伸等の各処理を施した後に、洗浄処理を施してから、乾燥することにより製造される。また前記偏光膜は、通常、その片面又は両面にトリアセチルセルロース等の透明保護フィルムが接着剤を用いて貼合された偏光フィルム（偏光板）として用いられている。
Conventionally, polarizing films used in various image display devices such as liquid crystal display devices and organic EL display devices have been dyed (using iodine, dichroic dyes, etc.) because they have both high transmittance and high degree of polarization. A polyvinyl alcohol film (containing a dichroic substance) is used. The polarizing film is manufactured by subjecting a polyvinyl alcohol film to various treatments such as swelling, dyeing, crosslinking, and stretching in a bath, followed by washing and drying. Further, the polarizing film is usually used as a polarizing film (polarizing plate) in which a transparent protective film such as triacetyl cellulose is bonded to one or both sides of the polarizing film using an adhesive.
前記偏光フィルムは、必要に応じ、他の光学層を積層して積層偏光フィルム（光学積層体）として用いられ、また、前記偏光フィルムあるいは前記積層偏光フィルム（光学積層体）は、液晶セルや有機ＥＬ素子等の画像表示セルに貼り合わされた画像表示パネルとして用いられ、さらに、前記画像表示パネルは、粘着剤層や接着剤層を介して、視認側における前面透明板（ウインドウ層）やタッチパネル等の前面透明部材に貼合されて、上記の各種画像表示装置として用いられる（特許文献１）。
The polarizing film is used as a laminated polarizing film (optical laminate) by laminating other optical layers as necessary, and the polarizing film or the laminated polarizing film (optical laminate) is used as a liquid crystal cell or an organic laminate. It is used as an image display panel bonded to an image display cell such as an EL element, and further, the image display panel is attached to a front transparent plate (window layer), a touch panel, etc. on the viewing side via an adhesive layer or an adhesive layer. It is bonded to the front transparent member of and used as the various image display devices mentioned above (Patent Document 1).
また、上記の偏光フィルム（偏光板）としては、偏光膜と透明保護フィルムが、接着剤層又は粘着剤層を介さずに、直接、貼合されている偏光フィルムも知られている（特許文献２－５）。
Furthermore, as the above-mentioned polarizing film (polarizing plate), there is also known a polarizing film in which a polarizing film and a transparent protective film are directly laminated without using an adhesive layer or a pressure-sensitive adhesive layer (Patent Document 2-5).
上記のように、偏光膜と透明保護フィルムが接着剤層や粘着剤層を介して貼り合わされている場合、接着剤層や粘着剤層は水分を蓄積し易いため、これら界面にて軽剥離が生じ、このような偏光フィルムを用いた画像表示装置では、表示不良が発生し易い懸念があった。また、特許文献２で具体的に開示された偏光フィルムの製造方法では、偏光膜と透明保護フィルムとの接着力が弱い問題があり、特許文献３－５で具体的に開示された偏光フィルムの製造方法では、１３５℃という高温での貼合工程を要するため、得られる偏光フィルムにカールが生じる問題があった。
As mentioned above, when a polarizing film and a transparent protective film are bonded together via an adhesive layer or a pressure-sensitive adhesive layer, the adhesive layer or pressure-sensitive adhesive layer tends to accumulate moisture, so light peeling is difficult at these interfaces. Therefore, there is a concern that display defects may easily occur in image display devices using such polarizing films. In addition, the method for producing a polarizing film specifically disclosed in Patent Document 2 has a problem in that the adhesive strength between the polarizing film and the transparent protective film is weak, and the method for producing a polarizing film specifically disclosed in Patent Documents 3-5 Since the manufacturing method requires a bonding step at a high temperature of 135° C., there is a problem in that the resulting polarizing film may curl.
以上のような事情に鑑み、本発明は、粘着剤層又は接着剤層を介さずとも、偏光膜と透明保護フィルムとの接着力に優れ、カールを抑制できる偏光フィルムの製造方法を提供することを目的とする。
In view of the above circumstances, an object of the present invention is to provide a method for producing a polarizing film that has excellent adhesive strength between a polarizing film and a transparent protective film and can suppress curling without using an adhesive layer or an adhesive layer. With the goal.
すなわち、本発明は、偏光膜と透明保護フィルムとを、粘着剤層又は粘着剤層を介さずに、直接、接合する偏光フィルムの製造方法であって、前記偏光膜、及び前記透明保護フィルムの少なくとも一方の貼合面に、紫外光を照射して表面処理をした後、前記偏光膜と前記透明保護フィルムとを揮発性媒体を介して貼合して積層体を製造する工程と、得られた積層体を加熱することにより、前記揮発性媒体を乾燥して、前記偏光膜と前記透明保護フィルムとを接合する工程を含む偏光フィルムの製造方法に関する。
That is, the present invention provides a method for producing a polarizing film in which a polarizing film and a transparent protective film are directly bonded without an adhesive layer or an adhesive layer, the method comprising: A step of manufacturing a laminate by irradiating at least one bonding surface with ultraviolet light and then bonding the polarizing film and the transparent protective film via a volatile medium; The present invention relates to a method for manufacturing a polarizing film, which includes a step of drying the volatile medium by heating a laminate obtained by heating the polarizing film and bonding the polarizing film and the transparent protective film.
本発明の偏光フィルムの製造方法における効果の作用メカニズムの詳細は以下のように推定される。ただし、本発明は、この作用メカニズムに限定して解釈されない。
The details of the mechanism of effect in the method for producing a polarizing film of the present invention are estimated as follows. However, the present invention is not construed as being limited to this mechanism of action.
本発明の偏光フィルムの製造方法は、偏光膜と透明保護フィルムとを、粘着剤層又は粘着剤層を介さずに、直接、接合する偏光フィルムの製造方法であって、前記偏光膜、及び前記透明保護フィルムの少なくとも一方の貼合面に、紫外光を照射して表面処理をした後、前記偏光膜と前記透明保護フィルムとを揮発性媒体を介して貼合して積層体を製造する工程と、得られた積層体を加熱することにより、前記揮発性媒体を乾燥して、前記偏光膜と前記透明保護フィルムとを接合する工程を含む。本発明の偏光フィルムの製造方法では、上記の表面処理面に、揮発性媒体が存在することにより、貼合面に気泡等が入らずに密着でき、さらに、揮発性媒体を加熱乾燥することにより、著しく接合面（界面）の接着力が高まる。また、活性エネルギー線硬化型接着剤に見られる収縮応力が接合界面に蓄積されづらく、貼合時に過剰な熱を必要としないことから熱による偏光膜の収縮も抑えられ、カールを抑制できる。
The method for producing a polarizing film of the present invention is a method for producing a polarizing film in which a polarizing film and a transparent protective film are directly bonded to each other without an adhesive layer or an adhesive layer. A step of surface-treating at least one bonding surface of the transparent protective film by irradiating ultraviolet light, and then bonding the polarizing film and the transparent protective film via a volatile medium to produce a laminate. and a step of drying the volatile medium by heating the obtained laminate and joining the polarizing film and the transparent protective film. In the method for producing a polarizing film of the present invention, the presence of a volatile medium on the above-mentioned surface-treated surface allows for close adhesion to the bonded surface without air bubbles, etc., and furthermore, by heating and drying the volatile medium, , the adhesive strength of the bonding surface (interface) increases significantly. In addition, the shrinkage stress found in active energy ray-curable adhesives is less likely to accumulate at the bonding interface, and excessive heat is not required during bonding, so shrinkage of the polarizing film due to heat is suppressed and curling can be suppressed.
また、本発明の偏光フィルムの製造方法は、偏光膜と透明保護フィルムとを、粘着剤層又は粘着剤層を介さずに、直接、接合できるため、粘着剤層又は接着剤層へのヨウ素等の二色性物質の拡散が抑えられることから、加湿信頼性にも優れる。
In addition, in the method for producing a polarizing film of the present invention, the polarizing film and the transparent protective film can be directly bonded without using an adhesive layer or an adhesive layer. Since the diffusion of dichroic substances is suppressed, humidification reliability is also excellent.
＜偏光フィルムの製造方法＞
本発明の偏光フィルムの製造方法は、偏光膜と透明保護フィルムとを、粘着剤層又は粘着剤層を介さずに、直接、接合する偏光フィルムの製造方法である。 <Production method of polarizing film>
The method for producing a polarizing film of the present invention is a method for producing a polarizing film in which a polarizing film and a transparent protective film are directly bonded to each other without an adhesive layer or an adhesive layer interposed therebetween.
本発明の偏光フィルムの製造方法は、偏光膜と透明保護フィルムとを、粘着剤層又は粘着剤層を介さずに、直接、接合する偏光フィルムの製造方法である。 <Production method of polarizing film>
The method for producing a polarizing film of the present invention is a method for producing a polarizing film in which a polarizing film and a transparent protective film are directly bonded to each other without an adhesive layer or an adhesive layer interposed therebetween.
＜偏光膜＞
前記偏光膜は、ポリビニルアルコール系フィルムにヨウ素や二色性染料等の二色性物質が吸着配向して形成される。前記偏光膜は、偏光膜の初期の偏光性能の観点から、前記二色性物質としてヨウ素を含む、ヨウ素系偏光膜が好ましい。 <Polarizing film>
The polarizing film is formed by adsorbing and aligning a dichroic substance such as iodine or a dichroic dye onto a polyvinyl alcohol film. The polarizing film is preferably an iodine-based polarizing film containing iodine as the dichroic substance from the viewpoint of initial polarization performance of the polarizing film.
前記偏光膜は、ポリビニルアルコール系フィルムにヨウ素や二色性染料等の二色性物質が吸着配向して形成される。前記偏光膜は、偏光膜の初期の偏光性能の観点から、前記二色性物質としてヨウ素を含む、ヨウ素系偏光膜が好ましい。 <Polarizing film>
The polarizing film is formed by adsorbing and aligning a dichroic substance such as iodine or a dichroic dye onto a polyvinyl alcohol film. The polarizing film is preferably an iodine-based polarizing film containing iodine as the dichroic substance from the viewpoint of initial polarization performance of the polarizing film.
前記ポリビニルアルコール（ＰＶＡ）系フィルムは、可視光領域において透光性を有し、ヨウ素や二色性染料等の二色性物質を分散吸着するものを特に制限なく使用できる。前記ポリビニルアルコール系フィルムの材料としては、ポリビニルアルコール又はその誘導体が挙げられる。前記ポリビニルアルコールの誘導体としては、例えば、ポリビニルホルマール、ポリビニルアセタール；エチレン、プロピレン等のオレフィン；アクリル酸、メタクリル酸、クロトン酸等の不飽和カルボン酸、及びそのアルキルエステル、アクリルアミド等で変性したもの等が挙げられる。前記ポリビニルアルコールは、平均重合度が１００～１０，０００程度であることが好ましく、１，０００～１０，０００程度であることがより好ましく、１，５００～４，５００程度であることがさらに好ましい。また、前記ポリビニルアルコールは、ケン化度が８０～１００モル％程度であることが好ましく、９５モル％～９９．９５モル程度であることがより好ましい。なお、前記平均重合度及び前記ケン化度は、ＪＩＳ Ｋ ６７２６に準じて求めることができる。
The polyvinyl alcohol (PVA)-based film can be used without any particular restriction, as long as it has transparency in the visible light region and disperses and adsorbs dichroic substances such as iodine and dichroic dyes. Examples of the material for the polyvinyl alcohol film include polyvinyl alcohol or derivatives thereof. Examples of the polyvinyl alcohol derivatives include polyvinyl formal, polyvinyl acetal; olefins such as ethylene and propylene; unsaturated carboxylic acids such as acrylic acid, methacrylic acid, and crotonic acid, and those modified with their alkyl esters, acrylamide, etc. can be mentioned. The average degree of polymerization of the polyvinyl alcohol is preferably about 100 to 10,000, more preferably about 1,000 to 10,000, and even more preferably about 1,500 to 4,500. . Further, the saponification degree of the polyvinyl alcohol is preferably about 80 to 100 mol%, more preferably about 95 mol% to 99.95 mol%. Note that the average degree of polymerization and the degree of saponification can be determined according to JIS K 6726.
前記偏光膜は、従前の偏光膜の製造方法により得られ、例えば、前記ポリビニルアルコール系フィルムに、任意の膨潤工程及び洗浄工程と、少なくとも、染色工程、架橋工程、及び延伸工程を施して得られる。
The polarizing film is obtained by a conventional method for producing a polarizing film, for example, by subjecting the polyvinyl alcohol film to an optional swelling process and washing process, and at least a dyeing process, a crosslinking process, and a stretching process. .
前記偏光膜は、偏光膜の初期の偏光度を向上させる観点から、厚みが１μｍ以上であることが好ましく、２μｍ以上であることがより好ましく、そして、パネルの反りを防止する観点から、１５μｍ以下であることが好ましく、１０μｍ以下であることがより好ましく、８μｍ以下であることがさらに好ましい。とくに、厚みが８μｍ程度以下の偏光膜を得るためには、前記ポリビニルアルコール系フィルムとして、熱可塑性樹脂基材上に製膜されたポリビニルアルコール系樹脂層を含む積層体を用いる、以下の薄型の偏光膜の製造方法が適用できる。
The thickness of the polarizing film is preferably 1 μm or more, more preferably 2 μm or more, from the viewpoint of improving the initial polarization degree of the polarizing film, and 15 μm or less from the viewpoint of preventing panel warpage. The thickness is preferably 10 μm or less, more preferably 8 μm or less. In particular, in order to obtain a polarizing film with a thickness of about 8 μm or less, the following thin film is used, in which a laminate including a polyvinyl alcohol resin layer formed on a thermoplastic resin base material is used as the polyvinyl alcohol film. A method for manufacturing a polarizing film can be applied.
偏光膜（薄型の偏光膜）は、従前の偏光膜の製造方法により得られ、例えば、長尺状の熱可塑性樹脂基材の片側に、ポリビニルアルコール系樹脂（ＰＶＡ系樹脂）を含むポリビニルアルコール系樹脂層（ＰＶＡ系樹脂層）を形成して積層体を準備する工程と、得られた積層体を長手方向に搬送しながら、前記積層体に、任意の不溶化処理工程、架橋処理工程、及び洗浄処理工程と、少なくとも、空中補助延伸処理工程、染色処理工程、及び水中延伸処理工程を施して得られる。
The polarizing film (thin polarizing film) is obtained by a conventional polarizing film manufacturing method. A step of forming a resin layer (PVA resin layer) to prepare a laminate, and while conveying the obtained laminate in the longitudinal direction, the laminate is subjected to an optional insolubilization treatment step, a crosslinking treatment step, and washing. It is obtained by performing a treatment step, and at least an in-air auxiliary stretching treatment step, a dyeing treatment step, and an underwater stretching treatment step.
＜透明保護フィルム＞
前記透明保護フィルムは、特に制限されず、偏光フィルムに用いられている各種の透明保護フィルムを用いることができる。前記透明保護フィルムを構成する材料としては、例えば、透明性、機械的強度、熱安定性、水分遮断性、等方性等に優れる熱可塑性樹脂が用いられる。前記熱可塑性樹脂としては、例えば、トリアセチルセルロール等のセルロールエステル系樹脂、ポリエチレンテレフタレートやポリエチレンナフタレート等のポリエステル系樹脂、ポリエーテルスルホン系樹脂、ポリスルホン系樹脂、ポリカーボネート系樹脂、ナイロンや芳香族ポリアミド等のポリアミド系樹脂、ポリイミド系樹脂、ポリエチレン、ポリプロピレン、エチレン・プロピレン共重合体の如きポリオレフィン系樹脂、（メタ）アクリル系樹脂、シクロ系ないしはノルボルネン構造を有する環状ポリオレフィン系樹脂（ノルボルネン系樹脂）、ポリアリレート系樹脂、ポリスチレン系樹脂、ポリビニルアルコール系樹脂、及びこれらの混合物があげられる。また、前記透明保護フィルムは、（メタ）アクリル系、ウレタン系、アクリルウレタン系、エポキシ系、シリコーン系等の熱硬化性樹脂又は紫外線硬化型樹脂から形成される硬化層を用いることができる。これらの中でも、セルロールエステル系樹脂、ポリカーボネート系樹脂、（メタ）アクリル系樹脂、環状ポリオレフィン系樹脂、ポリエステル系樹脂が好適である。 <Transparent protective film>
The transparent protective film is not particularly limited, and various transparent protective films used for polarizing films can be used. As the material constituting the transparent protective film, for example, a thermoplastic resin having excellent transparency, mechanical strength, thermal stability, moisture barrier properties, isotropy, etc. is used. Examples of the thermoplastic resin include cellulose ester resins such as triacetylcellulose, polyester resins such as polyethylene terephthalate and polyethylene naphthalate, polyether sulfone resins, polysulfone resins, polycarbonate resins, nylon, and aromatic resins. Polyamide resins such as group polyamides, polyimide resins, polyolefin resins such as polyethylene, polypropylene, and ethylene-propylene copolymers, (meth)acrylic resins, cyclic polyolefin resins having a cyclo or norbornene structure (norbornene resins) ), polyarylate resins, polystyrene resins, polyvinyl alcohol resins, and mixtures thereof. Further, the transparent protective film may include a cured layer formed from a thermosetting resin or an ultraviolet curable resin such as (meth)acrylic, urethane, acrylic urethane, epoxy, silicone, or the like. Among these, cellulose ester resins, polycarbonate resins, (meth)acrylic resins, cyclic polyolefin resins, and polyester resins are preferred.
前記透明保護フィルムは、特に制限されず、偏光フィルムに用いられている各種の透明保護フィルムを用いることができる。前記透明保護フィルムを構成する材料としては、例えば、透明性、機械的強度、熱安定性、水分遮断性、等方性等に優れる熱可塑性樹脂が用いられる。前記熱可塑性樹脂としては、例えば、トリアセチルセルロール等のセルロールエステル系樹脂、ポリエチレンテレフタレートやポリエチレンナフタレート等のポリエステル系樹脂、ポリエーテルスルホン系樹脂、ポリスルホン系樹脂、ポリカーボネート系樹脂、ナイロンや芳香族ポリアミド等のポリアミド系樹脂、ポリイミド系樹脂、ポリエチレン、ポリプロピレン、エチレン・プロピレン共重合体の如きポリオレフィン系樹脂、（メタ）アクリル系樹脂、シクロ系ないしはノルボルネン構造を有する環状ポリオレフィン系樹脂（ノルボルネン系樹脂）、ポリアリレート系樹脂、ポリスチレン系樹脂、ポリビニルアルコール系樹脂、及びこれらの混合物があげられる。また、前記透明保護フィルムは、（メタ）アクリル系、ウレタン系、アクリルウレタン系、エポキシ系、シリコーン系等の熱硬化性樹脂又は紫外線硬化型樹脂から形成される硬化層を用いることができる。これらの中でも、セルロールエステル系樹脂、ポリカーボネート系樹脂、（メタ）アクリル系樹脂、環状ポリオレフィン系樹脂、ポリエステル系樹脂が好適である。 <Transparent protective film>
The transparent protective film is not particularly limited, and various transparent protective films used for polarizing films can be used. As the material constituting the transparent protective film, for example, a thermoplastic resin having excellent transparency, mechanical strength, thermal stability, moisture barrier properties, isotropy, etc. is used. Examples of the thermoplastic resin include cellulose ester resins such as triacetylcellulose, polyester resins such as polyethylene terephthalate and polyethylene naphthalate, polyether sulfone resins, polysulfone resins, polycarbonate resins, nylon, and aromatic resins. Polyamide resins such as group polyamides, polyimide resins, polyolefin resins such as polyethylene, polypropylene, and ethylene-propylene copolymers, (meth)acrylic resins, cyclic polyolefin resins having a cyclo or norbornene structure (norbornene resins) ), polyarylate resins, polystyrene resins, polyvinyl alcohol resins, and mixtures thereof. Further, the transparent protective film may include a cured layer formed from a thermosetting resin or an ultraviolet curable resin such as (meth)acrylic, urethane, acrylic urethane, epoxy, silicone, or the like. Among these, cellulose ester resins, polycarbonate resins, (meth)acrylic resins, cyclic polyolefin resins, and polyester resins are preferred.
前記透明保護フィルムの厚さは、適宜に決定しうるが、一般には強度や取扱性等の作業性、薄層性等の観点から、１～５００μｍ程度であることが好ましく、１～３００μｍ程度あることがより好ましく、５～１００μｍ程度であることがさらに好ましい。
The thickness of the transparent protective film can be determined as appropriate, but generally from the viewpoint of strength, workability such as handleability, thin layer property, etc., it is preferably about 1 to 500 μm, and about 1 to 300 μm. The thickness is more preferably about 5 to 100 μm.
前記透明保護フィルムを、前記偏光膜の両面に貼り合わせる場合、その両面の透明保護フィルムは、同じものであってもよく、異なっていてもよい。
When the transparent protective films are attached to both sides of the polarizing film, the transparent protective films on both sides may be the same or different.
前記透明保護フィルムは、正面位相差が４０ｎｍ以上及び／又は、厚み方向位相差が８０ｎｍ以上の位相差を有する位相差板を用いることができる。正面位相差は、通常、４０～２００ｎｍの範囲に、厚み方向位相差は、通常、８０～３００ｎｍの範囲に制御される。前記透明保護フィルムとして位相差板を用いる場合には、当該位相差板が透明保護フィルムとしても機能するため、薄型化を図ることができる。
As the transparent protective film, a retardation plate having a front retardation of 40 nm or more and/or a thickness direction retardation of 80 nm or more can be used. The frontal retardation is usually controlled in the range of 40 to 200 nm, and the thickness direction retardation is usually controlled in the range of 80 to 300 nm. When a retardation plate is used as the transparent protective film, the retardation plate also functions as a transparent protective film, so that it is possible to reduce the thickness.
前記位相差板としては、例えば、高分子素材を一軸又は二軸延伸処理してなる複屈折性フィルム、液晶ポリマーの配向フィルム、液晶ポリマーの配向層をフィルムにて支持したもの等が挙げられる。位相差板の厚さは特に制限されないが、１～１５０μｍ程度が一般的である。なお、位相差を有しない透明保護フィルムに前記位相板を貼り合わせて使用してもよい。
Examples of the retardation plate include a birefringent film formed by uniaxially or biaxially stretching a polymer material, an oriented film of a liquid crystal polymer, and an oriented layer of a liquid crystal polymer supported by a film. The thickness of the retardation plate is not particularly limited, but is generally about 1 to 150 μm. Note that the phase plate may be used by bonding it to a transparent protective film that does not have a phase difference.
前記透明保護フィルムには、紫外線吸収剤、酸化防止剤、滑剤、可塑剤、離型剤、着色防止剤、難燃剤、帯電防止剤、顔料、着色剤等の任意の適切な添加剤を含んでいてもよい。とくに、前記透明保護フィルムに紫外線吸収剤を含む場合、偏光フィルムの耐光性を向上できる。
The transparent protective film may contain any suitable additives such as ultraviolet absorbers, antioxidants, lubricants, plasticizers, mold release agents, color inhibitors, flame retardants, antistatic agents, pigments, colorants, etc. You can stay there. In particular, when the transparent protective film contains an ultraviolet absorber, the light resistance of the polarizing film can be improved.
前記透明保護フィルムの偏光膜を貼り合わせない面には、ハードコート層、反射防止層、スティッキング防止層、拡散層ないしアンチグレア層等の他の層を設けることができる。なお、上記ハードコート層、反射防止層、スティッキング防止層、拡散層やアンチグレア層等の他の層は、保護フィルムそのものに設けることができるほか、別途、保護フィルムとは別体のものとして設けることもできる。
Other layers such as a hard coat layer, an anti-reflection layer, an anti-sticking layer, a diffusion layer or an anti-glare layer can be provided on the surface of the transparent protective film on which the polarizing film is not attached. Note that other layers such as the hard coat layer, antireflection layer, antisticking layer, diffusion layer, and antiglare layer can be provided on the protective film itself, or may be provided separately from the protective film. You can also do it.
本発明の偏光フィルムの製造方法は、前記偏光膜、及び前記透明保護フィルムの少なくとも一方の貼合面に、紫外光を照射して表面処理をした後、前記偏光膜と前記透明保護フィルムとを揮発性媒体を介して貼合して積層体を製造する工程と、得られた積層体を加熱することにより、前記揮発性媒体を乾燥して、前記偏光膜と前記透明保護フィルムとを接合する工程を含む。
The method for producing a polarizing film of the present invention includes surface-treating the bonding surface of at least one of the polarizing film and the transparent protective film by irradiating ultraviolet light, and then bonding the polarizing film and the transparent protective film. A step of manufacturing a laminate by bonding via a volatile medium, and heating the obtained laminate to dry the volatile medium and bond the polarizing film and the transparent protective film. Including process.
上記の紫外光としては、例えば、波長が２５０－１００ｎｍであることが好ましく、２００－１００ｎｍであることがより好ましく、なかでもキセノンエキシマランプを使用した１７２ｎｍの波長が、量産性の観点から特に好ましい。
For example, the wavelength of the above-mentioned ultraviolet light is preferably 250-100 nm, more preferably 200-100 nm, and among them, a wavelength of 172 nm using a xenon excimer lamp is particularly preferable from the viewpoint of mass productivity. .
また、上記の紫外光は、照度が、処理能力の観点から、１ｍＷ／ｃｍ２以上であることが好ましく、５０ｍＷ／ｃｍ２以上であることがより好ましい。また、積算光量が、接着性の観点から、１ｍＪ／ｃｍ２以上であることが好ましく、５０ｍＪ／ｃｍ２以上であることがより好ましく、そして、フィルムへのダメージの観点から、５０００ｍＪ／ｃｍ２以下であることが好ましく、２０００ｍＪ／ｃｍ２以下であることがより好ましい。また、紫外光照射時における温度は、特に限定されず、表面改質の安定化の観点から、０～５０℃程度であることが好ましく、１０～４０℃程度であることがより好ましく、偏光フィルムの生産上、室温であることが簡便である。また、紫外光照射時における雰囲気は、酸素濃度が２１％以下であればよく、処理効率の観点から、酸素濃度は７．０％以下が好ましい。
Further, the illumination intensity of the ultraviolet light is preferably 1 mW/cm 2 or more, more preferably 50 mW/cm 2 or more from the viewpoint of processing capacity. Further, the cumulative light amount is preferably 1 mJ/cm 2 or more from the viewpoint of adhesiveness, more preferably 50 mJ/cm 2 or more, and 5000 mJ/cm 2 or less from the viewpoint of damage to the film. It is preferable that it is, and it is more preferable that it is 2000 mJ/cm 2 or less. Further, the temperature at the time of ultraviolet light irradiation is not particularly limited, and from the viewpoint of stabilizing surface modification, it is preferably about 0 to 50 °C, more preferably about 10 to 40 °C, and the polarizing film For production purposes, it is convenient to use room temperature. Further, the atmosphere during ultraviolet light irradiation only needs to have an oxygen concentration of 21% or less, and from the viewpoint of processing efficiency, the oxygen concentration is preferably 7.0% or less.
前記揮発性媒体は、特に限定されず、乾燥効率の観点から、水、エタノール、トルエン、シクロヘキサン、アセトンなどの溶剤が好ましく、環境の観点から、水がより好ましい。
The volatile medium is not particularly limited, and from the viewpoint of drying efficiency, solvents such as water, ethanol, toluene, cyclohexane, acetone, etc. are preferred, and from the viewpoint of the environment, water is more preferred.
前記加熱の温度は、前記揮発性媒体を適切に乾燥できればよく、例えば、前記揮発性媒体が水の場合、４０～８０℃程度であることが好ましく、５０～７０℃程度であることがより好ましい。また、前記乾燥の時間は、偏光膜の温度の影響を受けるため一概に決定できないが、１分～６０分間程度であることが好ましく、３～１５分間程度であることがより好ましい。前記乾燥工程は１回だけ実施されてもよく、必要に応じて複数回実施されてもよい。
The heating temperature may be sufficient as long as it can appropriately dry the volatile medium; for example, when the volatile medium is water, it is preferably about 40 to 80°C, more preferably about 50 to 70°C. . Although the drying time cannot be absolutely determined because it is affected by the temperature of the polarizing film, it is preferably about 1 minute to 60 minutes, more preferably about 3 minutes to 15 minutes. The drying step may be performed only once, or may be performed multiple times as necessary.
上記の貼合は、ロールラミネーターなどにより行うことができる。
The above lamination can be performed using a roll laminator or the like.
前記偏光膜と前記透明保護フィルムの接合界面は、貼合時の処理に由来する改質層や高弾性層があってもよい。
The bonding interface between the polarizing film and the transparent protective film may include a modified layer or a high elastic layer resulting from the treatment during bonding.
前記偏光フィルムにおいて、前記透明保護フィルムと前記偏光膜との接着力（剥離強度）は、剥離角度９０°、剥離速度１０００ｍｍ／分の条件下の剥離強度測定で、０．５Ｎ／１５ｍｍ以上であることが好ましく、１．０Ｎ／１５ｍｍ以上であることがより好ましく、１．２Ｎ／１５ｍｍ以上であることがさらに好ましい。
In the polarizing film, the adhesive force (peel strength) between the transparent protective film and the polarizing film is 0.5 N/15 mm or more when peel strength is measured at a peel angle of 90° and a peel rate of 1000 mm/min. It is preferably 1.0 N/15 mm or more, more preferably 1.2 N/15 mm or more.
前記偏光フィルムにおいて、２０℃の水に２４時間浸漬前後おける、前記偏光膜と前記透明保護フィルムとの接合面の接着力の変化比（浸漬後の接着力／浸漬前の接着力）が、剥離角度９０°、剥離速度１０００ｍｍ／分の条件下で、０．５以上であることが好ましく、０．７以上であることがより好ましい。
In the polarizing film, the change ratio of the adhesive strength of the bonding surface between the polarizing film and the transparent protective film before and after being immersed in 20°C water for 24 hours (adhesive strength after immersion/adhesive strength before immersion) is the peeling rate. Under the conditions of an angle of 90° and a peeling rate of 1000 mm/min, it is preferably 0.5 or more, and more preferably 0.7 or more.
以下に実施例を挙げて本発明をさらに詳細に説明するが、本発明はこれらの実施例のみに限定されるものではない。
The present invention will be described in more detail with reference to Examples below, but the present invention is not limited to these Examples.
＜実施例１＞
＜偏光膜の準備＞
非晶性ＰＥＴ基材に９μｍ厚のＰＶＡ層が製膜された積層体を延伸温度１３０℃の空中補助延伸によって延伸積層体を生成し、次に、延伸積層体を染色によって着色積層体を生成し、さらに着色積層体を延伸温度６５度のホウ酸水中延伸によって総延伸倍率が５．９４倍になるように非晶性ＰＥＴ基材と一体に延伸された５μｍ厚の偏光膜を含む光学フィルム積層体を生成した。このような２段延伸によって非晶性ＰＥＴ基材に製膜されたＰＶＡ層のＰＶＡ分子が高次に配向され、染色によって吸着されたヨウ素がポリヨウ素イオン錯体として一方向に高次に配向された厚さ５μｍの偏光膜を含む光学フィルム積層体を得た。 <Example 1>
<Preparation of polarizing film>
A laminate in which a 9 μm thick PVA layer was formed on an amorphous PET base material was subjected to auxiliary stretching in the air at a stretching temperature of 130°C to produce a stretched laminate, and then the stretched laminate was dyed to produce a colored laminate. Then, the colored laminate was stretched in boric acid water at a stretching temperature of 65 degrees to obtain an optical film containing a 5 μm thick polarizing film, which was stretched together with the amorphous PET base material so that the total stretching ratio was 5.94 times. A laminate was produced. Through such two-step stretching, the PVA molecules of the PVA layer formed on the amorphous PET base material are highly oriented, and the iodine adsorbed by dyeing is oriented in one direction as a polyiodine ion complex. An optical film laminate containing a polarizing film with a thickness of 5 μm was obtained.
＜偏光膜の準備＞
非晶性ＰＥＴ基材に９μｍ厚のＰＶＡ層が製膜された積層体を延伸温度１３０℃の空中補助延伸によって延伸積層体を生成し、次に、延伸積層体を染色によって着色積層体を生成し、さらに着色積層体を延伸温度６５度のホウ酸水中延伸によって総延伸倍率が５．９４倍になるように非晶性ＰＥＴ基材と一体に延伸された５μｍ厚の偏光膜を含む光学フィルム積層体を生成した。このような２段延伸によって非晶性ＰＥＴ基材に製膜されたＰＶＡ層のＰＶＡ分子が高次に配向され、染色によって吸着されたヨウ素がポリヨウ素イオン錯体として一方向に高次に配向された厚さ５μｍの偏光膜を含む光学フィルム積層体を得た。 <Example 1>
<Preparation of polarizing film>
A laminate in which a 9 μm thick PVA layer was formed on an amorphous PET base material was subjected to auxiliary stretching in the air at a stretching temperature of 130°C to produce a stretched laminate, and then the stretched laminate was dyed to produce a colored laminate. Then, the colored laminate was stretched in boric acid water at a stretching temperature of 65 degrees to obtain an optical film containing a 5 μm thick polarizing film, which was stretched together with the amorphous PET base material so that the total stretching ratio was 5.94 times. A laminate was produced. Through such two-step stretching, the PVA molecules of the PVA layer formed on the amorphous PET base material are highly oriented, and the iodine adsorbed by dyeing is oriented in one direction as a polyiodine ion complex. An optical film laminate containing a polarizing film with a thickness of 5 μm was obtained.
＜偏光フィルムの製造＞
酸素濃度約２．５％の窒素置換雰囲気下において、上記で得られた偏光膜を含む光学フィルム積層体の偏光膜面、及び、透明保護フィルムとして、厚み２３μｍのシクロオレフィン系樹脂フィルム（日本ゼオン社製、ＺＦ１２）に、エキシマＵＶ処理装置（ウシオ電機社製、ＳＶＣ３４２Ｓ－１Ｎ２－ＭＮ３－ＫＷＯ１、キセノンエキシマランプ）を用い、エキシマＵＶ光（波長１７２ｎｍ、ピーク照度７５ｍＷ／ｃｍ２、積算光量４５０ｍＪ／ｃｍ２）を照射し、表面改質を施した。続いて、各フィルムの表面改質面に水を塗布し、水が乾燥する前に、ラミネーターを用いて偏光膜と透明保護フィルムを貼り合わせた後、６０℃のオーブンで５分３０秒間乾燥させ、偏光膜と透明保護フィルムが直接接合した偏光フィルムを得た。 <Manufacture of polarizing film>
In a nitrogen-substituted atmosphere with an oxygen concentration of about 2.5%, the polarizing film surface of the optical film laminate containing the polarizing film obtained above and a 23 μm thick cycloolefin resin film (Zeon Excimer UV light (wavelength 172 nm, peak illuminance 75 mW/cm 2 , cumulative light intensity 450 mJ/ cm 2 ) to perform surface modification. Next, water was applied to the surface-modified surface of each film, and before the water dried, the polarizing film and transparent protective film were pasted together using a laminator, and then dried in an oven at 60°C for 5 minutes and 30 seconds. A polarizing film in which a polarizing film and a transparent protective film were directly bonded was obtained.
酸素濃度約２．５％の窒素置換雰囲気下において、上記で得られた偏光膜を含む光学フィルム積層体の偏光膜面、及び、透明保護フィルムとして、厚み２３μｍのシクロオレフィン系樹脂フィルム（日本ゼオン社製、ＺＦ１２）に、エキシマＵＶ処理装置（ウシオ電機社製、ＳＶＣ３４２Ｓ－１Ｎ２－ＭＮ３－ＫＷＯ１、キセノンエキシマランプ）を用い、エキシマＵＶ光（波長１７２ｎｍ、ピーク照度７５ｍＷ／ｃｍ２、積算光量４５０ｍＪ／ｃｍ２）を照射し、表面改質を施した。続いて、各フィルムの表面改質面に水を塗布し、水が乾燥する前に、ラミネーターを用いて偏光膜と透明保護フィルムを貼り合わせた後、６０℃のオーブンで５分３０秒間乾燥させ、偏光膜と透明保護フィルムが直接接合した偏光フィルムを得た。 <Manufacture of polarizing film>
In a nitrogen-substituted atmosphere with an oxygen concentration of about 2.5%, the polarizing film surface of the optical film laminate containing the polarizing film obtained above and a 23 μm thick cycloolefin resin film (Zeon Excimer UV light (wavelength 172 nm, peak illuminance 75 mW/cm 2 , cumulative light intensity 450 mJ/ cm 2 ) to perform surface modification. Next, water was applied to the surface-modified surface of each film, and before the water dried, the polarizing film and transparent protective film were pasted together using a laminator, and then dried in an oven at 60°C for 5 minutes and 30 seconds. A polarizing film in which a polarizing film and a transparent protective film were directly bonded was obtained.
＜接着力（剥離強度）の評価＞
上記の偏光膜と透明保護フィルムが直接接合した偏光フィルムのＰＥＴ基材を剥離し、剥離面に両面テープ（Ｎｏ．５００、日東電工社製）を貼り合わせた。さらに、偏光膜の延伸方向と平行に２００ｍｍ、直行方向に１５ｍｍの大きさに切り出し、偏光膜と透明保護フィルムとの間にカッターナイフで切り込みを入れた後、両面テープの剥離フィルムを剥がし、粘着剤面をガラス板に貼り合わせた。角度自在タイプ粘着・皮膜剥離解析装置（ＶＰＡ－２、協和界面化学社製）により、９０度方向に偏光膜と透明保護フィルムとを剥離速度１０００ｍｍ／ｍｉｎで剥離し、その剥離強度（Ｎ／１５ｍｍ）を測定した。 <Evaluation of adhesive strength (peel strength)>
The PET base material of the polarizing film to which the above-mentioned polarizing film and transparent protective film were directly bonded was peeled off, and a double-sided tape (No. 500, manufactured by Nitto Denko Corporation) was bonded to the peeled surface. Furthermore, the polarizing film was cut out to a size of 200 mm in parallel to the stretching direction and 15 mm in the orthogonal direction, and a cut was made between the polarizing film and the transparent protective film using a cutter knife, and then the release film of the double-sided tape was peeled off and the adhesive was removed. The drug surface was attached to a glass plate. The polarizing film and the transparent protective film were peeled in a 90 degree direction at a peeling speed of 1000 mm/min using a flexible angle adhesive/film peeling analyzer (VPA-2, manufactured by Kyowa Interface Science Co., Ltd.), and the peel strength (N/15 mm) was measured. ) was measured.
上記の偏光膜と透明保護フィルムが直接接合した偏光フィルムのＰＥＴ基材を剥離し、剥離面に両面テープ（Ｎｏ．５００、日東電工社製）を貼り合わせた。さらに、偏光膜の延伸方向と平行に２００ｍｍ、直行方向に１５ｍｍの大きさに切り出し、偏光膜と透明保護フィルムとの間にカッターナイフで切り込みを入れた後、両面テープの剥離フィルムを剥がし、粘着剤面をガラス板に貼り合わせた。角度自在タイプ粘着・皮膜剥離解析装置（ＶＰＡ－２、協和界面化学社製）により、９０度方向に偏光膜と透明保護フィルムとを剥離速度１０００ｍｍ／ｍｉｎで剥離し、その剥離強度（Ｎ／１５ｍｍ）を測定した。 <Evaluation of adhesive strength (peel strength)>
The PET base material of the polarizing film to which the above-mentioned polarizing film and transparent protective film were directly bonded was peeled off, and a double-sided tape (No. 500, manufactured by Nitto Denko Corporation) was bonded to the peeled surface. Furthermore, the polarizing film was cut out to a size of 200 mm in parallel to the stretching direction and 15 mm in the orthogonal direction, and a cut was made between the polarizing film and the transparent protective film using a cutter knife, and then the release film of the double-sided tape was peeled off and the adhesive was removed. The drug surface was attached to a glass plate. The polarizing film and the transparent protective film were peeled in a 90 degree direction at a peeling speed of 1000 mm/min using a flexible angle adhesive/film peeling analyzer (VPA-2, manufactured by Kyowa Interface Science Co., Ltd.), and the peel strength (N/15 mm) was measured. ) was measured.
＜水の浸漬前後における接着力（剥離強度）の評価＞
上記の偏光膜と透明保護フィルムが直接接合した偏光フィルムのＰＥＴ基材を剥離し、剥離面に両面テープ（Ｎｏ．５００、日東電工社製）を貼り合わせた。さらに、偏光膜の延伸方向と平行に２００ｍｍ、直行方向に１５ｍｍの大きさに切り出し、偏光膜と透明保護フィルムとの間にカッターナイフで切り込みを入れた後、両面テープの剥離フィルムを剥がし、粘着剤面をガラス板に貼り合わせた。次いで、得られたガラス板に貼り合わせられた偏光フィルムを、２０℃の水に２４時間浸漬させて取り出した後、余分な水分を除去した。水の浸漬前後おける接着力について、角度自在タイプ粘着・皮膜剥離解析装置（ＶＰＡ－２、協和界面化学社製）により、９０度方向に偏光膜と透明保護フィルムとを剥離速度１０００ｍｍ／ｍｉｎで剥離し、その剥離強度（Ｎ／１５ｍｍ）を測定し、接合面の接着力（剥離強度）の変化比（浸漬後の接着力／浸漬前の接着力）を算出した。 <Evaluation of adhesive strength (peel strength) before and after immersion in water>
The PET base material of the polarizing film to which the above-mentioned polarizing film and transparent protective film were directly bonded was peeled off, and a double-sided tape (No. 500, manufactured by Nitto Denko Corporation) was bonded to the peeled surface. Furthermore, the polarizing film was cut out to a size of 200 mm in parallel to the stretching direction and 15 mm in the orthogonal direction, and a cut was made between the polarizing film and the transparent protective film using a cutter knife, and then the release film of the double-sided tape was peeled off and the adhesive was removed. The drug surface was attached to a glass plate. Next, the polarizing film bonded to the obtained glass plate was immersed in water at 20° C. for 24 hours, taken out, and excess moisture was removed. Regarding the adhesive strength before and after immersion in water, the polarizing film and transparent protective film were peeled in a 90-degree direction at a peeling speed of 1000 mm/min using a flexible angle adhesive/film peeling analyzer (VPA-2, manufactured by Kyowa Interface Science Co., Ltd.). Then, the peel strength (N/15 mm) was measured, and the change ratio (adhesion strength after dipping/adhesion strength before dipping) of the adhesive strength (peel strength) of the bonding surface was calculated.
上記の偏光膜と透明保護フィルムが直接接合した偏光フィルムのＰＥＴ基材を剥離し、剥離面に両面テープ（Ｎｏ．５００、日東電工社製）を貼り合わせた。さらに、偏光膜の延伸方向と平行に２００ｍｍ、直行方向に１５ｍｍの大きさに切り出し、偏光膜と透明保護フィルムとの間にカッターナイフで切り込みを入れた後、両面テープの剥離フィルムを剥がし、粘着剤面をガラス板に貼り合わせた。次いで、得られたガラス板に貼り合わせられた偏光フィルムを、２０℃の水に２４時間浸漬させて取り出した後、余分な水分を除去した。水の浸漬前後おける接着力について、角度自在タイプ粘着・皮膜剥離解析装置（ＶＰＡ－２、協和界面化学社製）により、９０度方向に偏光膜と透明保護フィルムとを剥離速度１０００ｍｍ／ｍｉｎで剥離し、その剥離強度（Ｎ／１５ｍｍ）を測定し、接合面の接着力（剥離強度）の変化比（浸漬後の接着力／浸漬前の接着力）を算出した。 <Evaluation of adhesive strength (peel strength) before and after immersion in water>
The PET base material of the polarizing film to which the above-mentioned polarizing film and transparent protective film were directly bonded was peeled off, and a double-sided tape (No. 500, manufactured by Nitto Denko Corporation) was bonded to the peeled surface. Furthermore, the polarizing film was cut out to a size of 200 mm in parallel to the stretching direction and 15 mm in the orthogonal direction, and a cut was made between the polarizing film and the transparent protective film using a cutter knife, and then the release film of the double-sided tape was peeled off and the adhesive was removed. The drug surface was attached to a glass plate. Next, the polarizing film bonded to the obtained glass plate was immersed in water at 20° C. for 24 hours, taken out, and excess moisture was removed. Regarding the adhesive strength before and after immersion in water, the polarizing film and transparent protective film were peeled in a 90-degree direction at a peeling speed of 1000 mm/min using a flexible angle adhesive/film peeling analyzer (VPA-2, manufactured by Kyowa Interface Science Co., Ltd.). Then, the peel strength (N/15 mm) was measured, and the change ratio (adhesion strength after dipping/adhesion strength before dipping) of the adhesive strength (peel strength) of the bonding surface was calculated.
＜カールの評価＞
上記の偏光膜と透明保護フィルムが直接接合した偏光フィルムのＰＥＴ基材を剥離した後、２３℃相対湿度５５％環境で７２時間調湿し、１００ｍｍ×１００ｍｍで切り出し、樹脂フィルムの面を上にしてフィルムの４隅それぞれの水平面からの高さを測定し、４点の平均値を、フィルムのカールとした。表では、カールが２ｍｍ未満のものを◎、２ｍｍ以上３ｍｍ未満のものを〇、３ｍｍ以上５ｍｍ未満のものを△、５ｍｍ以上のものを×で示している。 <Evaluation of curl>
After peeling off the PET base material of the polarizing film to which the above polarizing film and transparent protective film were directly bonded, the humidity was controlled at 23°C and 55% relative humidity for 72 hours, and cut into 100 mm x 100 mm, with the resin film side facing up. The height from the horizontal plane of each of the four corners of the film was measured, and the average value of the four points was taken as the curl of the film. In the table, those with a curl of less than 2 mm are indicated by ◎, those with a curl of 2 mm or more but less than 3 mm are indicated by ○, those with a curl of 3 mm or more and less than 5 mm are indicated by △, and those with a curl of 5 mm or more are indicated by ×.
上記の偏光膜と透明保護フィルムが直接接合した偏光フィルムのＰＥＴ基材を剥離した後、２３℃相対湿度５５％環境で７２時間調湿し、１００ｍｍ×１００ｍｍで切り出し、樹脂フィルムの面を上にしてフィルムの４隅それぞれの水平面からの高さを測定し、４点の平均値を、フィルムのカールとした。表では、カールが２ｍｍ未満のものを◎、２ｍｍ以上３ｍｍ未満のものを〇、３ｍｍ以上５ｍｍ未満のものを△、５ｍｍ以上のものを×で示している。 <Evaluation of curl>
After peeling off the PET base material of the polarizing film to which the above polarizing film and transparent protective film were directly bonded, the humidity was controlled at 23°C and 55% relative humidity for 72 hours, and cut into 100 mm x 100 mm, with the resin film side facing up. The height from the horizontal plane of each of the four corners of the film was measured, and the average value of the four points was taken as the curl of the film. In the table, those with a curl of less than 2 mm are indicated by ◎, those with a curl of 2 mm or more but less than 3 mm are indicated by ○, those with a curl of 3 mm or more and less than 5 mm are indicated by △, and those with a curl of 5 mm or more are indicated by ×.
＜加湿信頼性の評価＞
上記偏光フィルムのＰＥＴ基材を剥離した後、偏光膜側に粘着剤層（厚み２０μｍ）を介して、厚さ０．７ｍｍの無アルカリガラスの一方に貼り合わせた偏光フィルム（加湿耐久性試験評価用サンプル）を準備した。得られた偏光フィルムの透過率Ｔｓについて、紫外可視分光光度計（日本分光社製Ｖ－７１００）を用いて測定し、単体透過率Ｔｓ、平行透過率Ｔｐ、直交透過率Ｔｃをそれぞれ、偏光フィルムのＴｓ、ＴｐおよびＴｃとした。これらのＴｓ、ＴｐおよびＴｃは、ＪＩＳ Ｚ８７０１の２度視野（Ｃ光源）により測定して視感度補正を行なったＹ値である。６０℃９５％ＲＨの環境下に１２０時間曝露し、投入後の偏光フィルムについても同様の方法で透過率Ｔｓを測定し、透過率変化ΔＴ（％）＝｜（投入前の透過率Ｔｓ（％））－（投入後の透過率Ｔｓ（％））｜を求めた。透過率変化ΔＴ（％）が小さいほど、湿熱環境下での耐久性に優れると判断した。ΔＴ（％）は、好ましくは、０．４以下であり、より好ましくは、０．３以下である。 <Evaluation of humidification reliability>
After peeling off the PET base material of the above polarizing film, the polarizing film was laminated to one side of a 0.7 mm thick alkali-free glass via an adhesive layer (thickness 20 μm) on the polarizing film side (humidification durability test evaluation sample) was prepared. The transmittance Ts of the obtained polarizing film was measured using an ultraviolet-visible spectrophotometer (V-7100 manufactured by JASCO Corporation), and the single transmittance Ts, parallel transmittance Tp, and orthogonal transmittance Tc were determined for the polarizing film. Ts, Tp and Tc of These Ts, Tp, and Tc are Y values measured using a 2-degree visual field (C light source) according to JIS Z8701 and subjected to visibility correction. The transmittance Ts of the polarizing film after being exposed to an environment of 60°C and 95% RH for 120 hours was measured in the same manner, and the transmittance change ΔT (%) = | (transmittance Ts (% )) - (transmittance Ts (%) after injection) | was determined. It was determined that the smaller the transmittance change ΔT (%), the more excellent the durability in a moist heat environment. ΔT (%) is preferably 0.4 or less, more preferably 0.3 or less.
上記偏光フィルムのＰＥＴ基材を剥離した後、偏光膜側に粘着剤層（厚み２０μｍ）を介して、厚さ０．７ｍｍの無アルカリガラスの一方に貼り合わせた偏光フィルム（加湿耐久性試験評価用サンプル）を準備した。得られた偏光フィルムの透過率Ｔｓについて、紫外可視分光光度計（日本分光社製Ｖ－７１００）を用いて測定し、単体透過率Ｔｓ、平行透過率Ｔｐ、直交透過率Ｔｃをそれぞれ、偏光フィルムのＴｓ、ＴｐおよびＴｃとした。これらのＴｓ、ＴｐおよびＴｃは、ＪＩＳ Ｚ８７０１の２度視野（Ｃ光源）により測定して視感度補正を行なったＹ値である。６０℃９５％ＲＨの環境下に１２０時間曝露し、投入後の偏光フィルムについても同様の方法で透過率Ｔｓを測定し、透過率変化ΔＴ（％）＝｜（投入前の透過率Ｔｓ（％））－（投入後の透過率Ｔｓ（％））｜を求めた。透過率変化ΔＴ（％）が小さいほど、湿熱環境下での耐久性に優れると判断した。ΔＴ（％）は、好ましくは、０．４以下であり、より好ましくは、０．３以下である。 <Evaluation of humidification reliability>
After peeling off the PET base material of the above polarizing film, the polarizing film was laminated to one side of a 0.7 mm thick alkali-free glass via an adhesive layer (thickness 20 μm) on the polarizing film side (humidification durability test evaluation sample) was prepared. The transmittance Ts of the obtained polarizing film was measured using an ultraviolet-visible spectrophotometer (V-7100 manufactured by JASCO Corporation), and the single transmittance Ts, parallel transmittance Tp, and orthogonal transmittance Tc were determined for the polarizing film. Ts, Tp and Tc of These Ts, Tp, and Tc are Y values measured using a 2-degree visual field (C light source) according to JIS Z8701 and subjected to visibility correction. The transmittance Ts of the polarizing film after being exposed to an environment of 60°C and 95% RH for 120 hours was measured in the same manner, and the transmittance change ΔT (%) = | (transmittance Ts (% )) - (transmittance Ts (%) after injection) | was determined. It was determined that the smaller the transmittance change ΔT (%), the more excellent the durability in a moist heat environment. ΔT (%) is preferably 0.4 or less, more preferably 0.3 or less.
＜実施例２＞
透明保護フィルムとして、厚み１３μｍのシクロオレフィン系樹脂フィルム（日本ゼオン社製、ＺＦ１４）を用いたこと以外は、実施例１と同様の操作にて、偏光膜と透明保護フィルムが直接接合した偏光フィルムを得た。 <Example 2>
A polarizing film in which a polarizing film and a transparent protective film were directly bonded was prepared in the same manner as in Example 1, except that a 13 μm thick cycloolefin resin film (Nippon Zeon Co., Ltd., ZF14) was used as the transparent protective film. I got it.
透明保護フィルムとして、厚み１３μｍのシクロオレフィン系樹脂フィルム（日本ゼオン社製、ＺＦ１４）を用いたこと以外は、実施例１と同様の操作にて、偏光膜と透明保護フィルムが直接接合した偏光フィルムを得た。 <Example 2>
A polarizing film in which a polarizing film and a transparent protective film were directly bonded was prepared in the same manner as in Example 1, except that a 13 μm thick cycloolefin resin film (Nippon Zeon Co., Ltd., ZF14) was used as the transparent protective film. I got it.
＜実施例３＞
透明保護フィルムとして、以下の厚み２０μｍのポリカーボネート系樹脂フィルムを用い、各フィルムの表面改質面に水の替わりにアセトンを塗布したこと以外は、実施例１と同様の操作にて、偏光膜と透明保護フィルムが直接接合した偏光フィルムを得た。ポリカーボネート系樹脂フィルムは、以下のようにして作製した。すなわち、イソソルビド８１．９８質量部に対して、トリシクロデカンジメタノール４７．１９質量部、ジフェニルカーボネート１７５．１質量部、及び触媒として、炭酸セシウム０．２質量％水溶液０．９７９質量部を反応容器に投入し、窒素雰囲気下にて、反応の第１段目の工程として、加熱槽温度を１５０℃に加熱し、必要に応じて攪拌しながら、原料を溶解させた（約１５分）。次いで、圧力を常圧から１３．３ｋＰａにし、加熱槽温度を１９０℃まで１時間で上昇させながら、発生するフェノールを反応容器外へ抜き出した。反応容器全体を１９０℃で１５分保持した後、第２段目の工程として、反応容器内の圧力を６．６７ｋＰａとし、加熱槽温度を２３０℃まで、１５分で上昇させ、発生するフェノールを反応容器外へ抜き出した。攪拌機の攪拌トルクが上昇してくるので、８分で２５０℃まで昇温し、さらに発生するフェノールを取り除くため、反応容器内の圧力を０．２００ｋＰａ以下に到達させた。所定の攪拌トルクに到達後、反応を終了し、生成した反応物を水中に押し出して、ポリカーボネート樹脂のペレットを得た。得られたポリカーボネート樹脂を８０℃で５時間真空乾燥をした後、単軸押出機（東芝機械社製、シリンダー設定温度：２５０℃）、Ｔダイ（幅３００ｍｍ、設定温度：２５０℃）、チルロール（設定温度：１２０～１３０℃）および巻取機を備えたフィルム製膜装置を用いて、ポリカーボネート樹脂から構成される光学フィルムを作製した。 <Example 3>
As a transparent protective film, the following polycarbonate resin films with a thickness of 20 μm were used, and a polarizing film and a A polarizing film to which a transparent protective film was directly bonded was obtained. A polycarbonate resin film was produced as follows. That is, 81.98 parts by mass of isosorbide was reacted with 47.19 parts by mass of tricyclodecane dimethanol, 175.1 parts by mass of diphenyl carbonate, and 0.979 parts by mass of a 0.2% by mass aqueous solution of cesium carbonate as a catalyst. The mixture was placed in a container, and as the first step of the reaction, the heating tank temperature was heated to 150° C., and the raw materials were dissolved with stirring as necessary (about 15 minutes). Next, the pressure was raised from normal pressure to 13.3 kPa, and the temperature of the heating tank was raised to 190° C. over 1 hour, while the generated phenol was extracted out of the reaction vessel. After holding the entire reaction vessel at 190°C for 15 minutes, in the second step, the pressure inside the reaction vessel was set to 6.67 kPa, and the heating tank temperature was raised to 230°C in 15 minutes to remove the generated phenol. It was taken out of the reaction vessel. As the stirring torque of the stirrer increased, the temperature was raised to 250° C. in 8 minutes, and in order to further remove the generated phenol, the pressure inside the reaction vessel was brought to 0.200 kPa or less. After reaching a predetermined stirring torque, the reaction was terminated and the generated reaction product was extruded into water to obtain polycarbonate resin pellets. The obtained polycarbonate resin was vacuum-dried at 80°C for 5 hours, and then put into a single-screw extruder (manufactured by Toshiba Machine Co., Ltd., cylinder set temperature: 250°C), a T-die (width 300mm, set temperature: 250°C), a chill roll ( An optical film made of polycarbonate resin was produced using a film forming apparatus equipped with a winder and a set temperature of 120 to 130°C.
透明保護フィルムとして、以下の厚み２０μｍのポリカーボネート系樹脂フィルムを用い、各フィルムの表面改質面に水の替わりにアセトンを塗布したこと以外は、実施例１と同様の操作にて、偏光膜と透明保護フィルムが直接接合した偏光フィルムを得た。ポリカーボネート系樹脂フィルムは、以下のようにして作製した。すなわち、イソソルビド８１．９８質量部に対して、トリシクロデカンジメタノール４７．１９質量部、ジフェニルカーボネート１７５．１質量部、及び触媒として、炭酸セシウム０．２質量％水溶液０．９７９質量部を反応容器に投入し、窒素雰囲気下にて、反応の第１段目の工程として、加熱槽温度を１５０℃に加熱し、必要に応じて攪拌しながら、原料を溶解させた（約１５分）。次いで、圧力を常圧から１３．３ｋＰａにし、加熱槽温度を１９０℃まで１時間で上昇させながら、発生するフェノールを反応容器外へ抜き出した。反応容器全体を１９０℃で１５分保持した後、第２段目の工程として、反応容器内の圧力を６．６７ｋＰａとし、加熱槽温度を２３０℃まで、１５分で上昇させ、発生するフェノールを反応容器外へ抜き出した。攪拌機の攪拌トルクが上昇してくるので、８分で２５０℃まで昇温し、さらに発生するフェノールを取り除くため、反応容器内の圧力を０．２００ｋＰａ以下に到達させた。所定の攪拌トルクに到達後、反応を終了し、生成した反応物を水中に押し出して、ポリカーボネート樹脂のペレットを得た。得られたポリカーボネート樹脂を８０℃で５時間真空乾燥をした後、単軸押出機（東芝機械社製、シリンダー設定温度：２５０℃）、Ｔダイ（幅３００ｍｍ、設定温度：２５０℃）、チルロール（設定温度：１２０～１３０℃）および巻取機を備えたフィルム製膜装置を用いて、ポリカーボネート樹脂から構成される光学フィルムを作製した。 <Example 3>
As a transparent protective film, the following polycarbonate resin films with a thickness of 20 μm were used, and a polarizing film and a A polarizing film to which a transparent protective film was directly bonded was obtained. A polycarbonate resin film was produced as follows. That is, 81.98 parts by mass of isosorbide was reacted with 47.19 parts by mass of tricyclodecane dimethanol, 175.1 parts by mass of diphenyl carbonate, and 0.979 parts by mass of a 0.2% by mass aqueous solution of cesium carbonate as a catalyst. The mixture was placed in a container, and as the first step of the reaction, the heating tank temperature was heated to 150° C., and the raw materials were dissolved with stirring as necessary (about 15 minutes). Next, the pressure was raised from normal pressure to 13.3 kPa, and the temperature of the heating tank was raised to 190° C. over 1 hour, while the generated phenol was extracted out of the reaction vessel. After holding the entire reaction vessel at 190°C for 15 minutes, in the second step, the pressure inside the reaction vessel was set to 6.67 kPa, and the heating tank temperature was raised to 230°C in 15 minutes to remove the generated phenol. It was taken out of the reaction vessel. As the stirring torque of the stirrer increased, the temperature was raised to 250° C. in 8 minutes, and in order to further remove the generated phenol, the pressure inside the reaction vessel was brought to 0.200 kPa or less. After reaching a predetermined stirring torque, the reaction was terminated and the generated reaction product was extruded into water to obtain polycarbonate resin pellets. The obtained polycarbonate resin was vacuum-dried at 80°C for 5 hours, and then put into a single-screw extruder (manufactured by Toshiba Machine Co., Ltd., cylinder set temperature: 250°C), a T-die (width 300mm, set temperature: 250°C), a chill roll ( An optical film made of polycarbonate resin was produced using a film forming apparatus equipped with a winder and a set temperature of 120 to 130°C.
＜比較例１＞
透明保護フィルムとして、厚み２３μｍのシクロオレフィン系樹脂フィルム（日本ゼオン社製、ＺＦ１２）に、下記の活性エネルギー線硬化型接着剤をバーコーターで塗布し、ラミネーターを用いて、実施例１で得られた厚さ５μｍの偏光膜を含む光学フィルム積層体の偏光膜面と貼り合わせた。その状態で透明保護フィルム側から、活性エネルギー線照射を行い、接着剤を硬化させ、偏光膜に透明保護フィルムが活性エネルギー線接着剤を介して接合している偏光フィルムを得た。
［活性エネルギー線硬化型接着剤］
２－ヒドロキシエチルアクリルアミド（ＫＪケミカルズ社製、商品名：ＨＥＡＡ）１６．５重量部、４－ビニルフェニルボロン酸（東京化成工業社製）１重量部、２－ヒドロキシ－３－フェノキシプロピルアクリレート（東亞合成社製、商品名：アロニックスＭ－５７００）３０．５重量部、１，９－ノナンジオールジアクリレート（共栄社化学社製、商品名：ライトアクリレート１，９ＮＤ－Ａ）２５重量部、ヒドロキシピバリン酸ジアクリレート（共栄社化学社製、商品名：ライトアクリレートＨＰＰ－Ａ）１３重量部、（メタ）アクリレートを重合してなるオリゴマー（東亞合成社製、商品名：ＡＲＦＯＮ ＵＰ－１１９０）１５重量部、２－メチル－１－［４－（メチルチオ）フェニル］－２－モルフォニルプロパン－１－オン（ＩＧＭ ｒｅｓｉｎｓ社製、商品名：Ｏｍｎｉｒａｄ ９０７）３重量部、２，４－ジエチルチオキサントン（日本化薬社製、商品名：ＫＡＹＡＣＵＲＥ－ＤＥＴＸ－Ｓ）３重量部
［活性エネルギー線］
活性エネルギー線として、可視光線（ガリウム封入メタルハライドランプ） 照射装置：Ｈｅｒａｅｕｓ社製Ｌｉｇｈｔ ＨＡＭＭＥＲ１０ バルブ：Ｖバルブ ピーク照度：８００ｍＷ／ｃｍ２、積算照射量８００／ｍＪ／ｃｍ２（波長３８０～４４０ｎｍ）を使用した。なお、可視光線の照度は、Ｓｏｌａｔｅｌｌ社製Ｓｏｌａ－Ｃｈｅｃｋシステムを使用して測定した。 <Comparative example 1>
As a transparent protective film, the following active energy ray-curable adhesive was applied with a bar coater to a 23 μm thick cycloolefin resin film (Nippon Zeon Co., Ltd., ZF12), and a laminator was used to apply the adhesive obtained in Example 1. The film was bonded to the polarizing film surface of an optical film laminate containing a polarizing film with a thickness of 5 μm. In this state, active energy rays were irradiated from the transparent protective film side to cure the adhesive, thereby obtaining a polarizing film in which the transparent protective film was bonded to the polarizing film via the active energy ray adhesive.
[Active energy ray curable adhesive]
16.5 parts by weight of 2-hydroxyethyl acrylamide (manufactured by KJ Chemicals, trade name: HEAA), 1 part by weight of 4-vinylphenylboronic acid (manufactured by Tokyo Chemical Industry Co., Ltd.), 2-hydroxy-3-phenoxypropyl acrylate (manufactured by Toa) 30.5 parts by weight of 1,9-nonanediol diacrylate (manufactured by Kyoeisha Chemical Co., Ltd., trade name: Aronix M-5700), 25 parts by weight of 1,9-nonanediol diacrylate (manufactured by Kyoeisha Chemical Co., Ltd., trade name: Light Acrylate 1,9ND-A), hydroxypivalic acid 13 parts by weight of diacrylate (manufactured by Kyoeisha Chemical Co., Ltd., trade name: Light Acrylate HPP-A), 15 parts by weight of oligomer formed by polymerizing (meth)acrylate (manufactured by Toagosei Co., Ltd., trade name: ARFON UP-1190), 2 - 3 parts by weight of methyl-1-[4-(methylthio)phenyl]-2-morphonylpropan-1-one (manufactured by IGM resins, trade name: Omnirad 907), 2,4-diethylthioxanthone (Nippon Kayaku Co., Ltd.) manufactured by KAYACURE-DETX-S) 3 parts by weight [Active energy ray]
Visible light (gallium-filled metal halide lamp) Irradiation device: Light HAMMER10 manufactured by Heraeus Bulb: V bulb Peak illuminance: 800 mW/cm 2 , cumulative irradiation amount 800/mJ/cm 2 (wavelength 380 to 440 nm) was used as the active energy ray. did. Note that the illuminance of visible light was measured using a Sola-Check system manufactured by Solatell.
透明保護フィルムとして、厚み２３μｍのシクロオレフィン系樹脂フィルム（日本ゼオン社製、ＺＦ１２）に、下記の活性エネルギー線硬化型接着剤をバーコーターで塗布し、ラミネーターを用いて、実施例１で得られた厚さ５μｍの偏光膜を含む光学フィルム積層体の偏光膜面と貼り合わせた。その状態で透明保護フィルム側から、活性エネルギー線照射を行い、接着剤を硬化させ、偏光膜に透明保護フィルムが活性エネルギー線接着剤を介して接合している偏光フィルムを得た。
［活性エネルギー線硬化型接着剤］
２－ヒドロキシエチルアクリルアミド（ＫＪケミカルズ社製、商品名：ＨＥＡＡ）１６．５重量部、４－ビニルフェニルボロン酸（東京化成工業社製）１重量部、２－ヒドロキシ－３－フェノキシプロピルアクリレート（東亞合成社製、商品名：アロニックスＭ－５７００）３０．５重量部、１，９－ノナンジオールジアクリレート（共栄社化学社製、商品名：ライトアクリレート１，９ＮＤ－Ａ）２５重量部、ヒドロキシピバリン酸ジアクリレート（共栄社化学社製、商品名：ライトアクリレートＨＰＰ－Ａ）１３重量部、（メタ）アクリレートを重合してなるオリゴマー（東亞合成社製、商品名：ＡＲＦＯＮ ＵＰ－１１９０）１５重量部、２－メチル－１－［４－（メチルチオ）フェニル］－２－モルフォニルプロパン－１－オン（ＩＧＭ ｒｅｓｉｎｓ社製、商品名：Ｏｍｎｉｒａｄ ９０７）３重量部、２，４－ジエチルチオキサントン（日本化薬社製、商品名：ＫＡＹＡＣＵＲＥ－ＤＥＴＸ－Ｓ）３重量部
［活性エネルギー線］
活性エネルギー線として、可視光線（ガリウム封入メタルハライドランプ） 照射装置：Ｈｅｒａｅｕｓ社製Ｌｉｇｈｔ ＨＡＭＭＥＲ１０ バルブ：Ｖバルブ ピーク照度：８００ｍＷ／ｃｍ２、積算照射量８００／ｍＪ／ｃｍ２（波長３８０～４４０ｎｍ）を使用した。なお、可視光線の照度は、Ｓｏｌａｔｅｌｌ社製Ｓｏｌａ－Ｃｈｅｃｋシステムを使用して測定した。 <Comparative example 1>
As a transparent protective film, the following active energy ray-curable adhesive was applied with a bar coater to a 23 μm thick cycloolefin resin film (Nippon Zeon Co., Ltd., ZF12), and a laminator was used to apply the adhesive obtained in Example 1. The film was bonded to the polarizing film surface of an optical film laminate containing a polarizing film with a thickness of 5 μm. In this state, active energy rays were irradiated from the transparent protective film side to cure the adhesive, thereby obtaining a polarizing film in which the transparent protective film was bonded to the polarizing film via the active energy ray adhesive.
[Active energy ray curable adhesive]
16.5 parts by weight of 2-hydroxyethyl acrylamide (manufactured by KJ Chemicals, trade name: HEAA), 1 part by weight of 4-vinylphenylboronic acid (manufactured by Tokyo Chemical Industry Co., Ltd.), 2-hydroxy-3-phenoxypropyl acrylate (manufactured by Toa) 30.5 parts by weight of 1,9-nonanediol diacrylate (manufactured by Kyoeisha Chemical Co., Ltd., trade name: Aronix M-5700), 25 parts by weight of 1,9-nonanediol diacrylate (manufactured by Kyoeisha Chemical Co., Ltd., trade name: Light Acrylate 1,9ND-A), hydroxypivalic acid 13 parts by weight of diacrylate (manufactured by Kyoeisha Chemical Co., Ltd., trade name: Light Acrylate HPP-A), 15 parts by weight of oligomer formed by polymerizing (meth)acrylate (manufactured by Toagosei Co., Ltd., trade name: ARFON UP-1190), 2 - 3 parts by weight of methyl-1-[4-(methylthio)phenyl]-2-morphonylpropan-1-one (manufactured by IGM resins, trade name: Omnirad 907), 2,4-diethylthioxanthone (Nippon Kayaku Co., Ltd.) manufactured by KAYACURE-DETX-S) 3 parts by weight [Active energy ray]
Visible light (gallium-filled metal halide lamp) Irradiation device: Light HAMMER10 manufactured by Heraeus Bulb: V bulb Peak illuminance: 800 mW/cm 2 , cumulative irradiation amount 800/mJ/cm 2 (wavelength 380 to 440 nm) was used as the active energy ray. did. Note that the illuminance of visible light was measured using a Sola-Check system manufactured by Solatell.
＜比較例２＞
３０μｍの偏光膜（ポリビニルアルコール系フィルム）の片面に、厚み４０μｍのシクロオレフィン系樹脂フィルム（日本ゼオン社製、ＺＦ１４）を、１４５℃の温度にてロールラミネーターを用いて圧着して積層し、偏光膜と樹脂フィルムが直接接合された偏光フィルムを得た。 <Comparative example 2>
A 40 μm thick cycloolefin resin film (Nippon Zeon Co., Ltd., ZF14) was laminated on one side of a 30 μm polarizing film (polyvinyl alcohol film) using a roll laminator at a temperature of 145°C. A polarizing film in which the membrane and resin film were directly bonded was obtained.
３０μｍの偏光膜（ポリビニルアルコール系フィルム）の片面に、厚み４０μｍのシクロオレフィン系樹脂フィルム（日本ゼオン社製、ＺＦ１４）を、１４５℃の温度にてロールラミネーターを用いて圧着して積層し、偏光膜と樹脂フィルムが直接接合された偏光フィルムを得た。 <Comparative example 2>
A 40 μm thick cycloolefin resin film (Nippon Zeon Co., Ltd., ZF14) was laminated on one side of a 30 μm polarizing film (polyvinyl alcohol film) using a roll laminator at a temperature of 145°C. A polarizing film in which the membrane and resin film were directly bonded was obtained.
＜比較例３＞
酸素濃度約２．５％の窒素置換雰囲気下において、上記で得られた偏光膜を含む光学フィルム積層体の偏光膜面、及び、透明保護フィルムとして、厚み２３μｍのシクロオレフィン系樹脂フィルム（日本ゼオン社製、ＺＦ１２）に、エキシマＵＶ処理装置（ウシオ電機社製、ＳＶＣ３４２Ｓ－１Ｎ２－ＭＮ３－ＫＷＯ１、キセノンエキシマランプ）を用い、エキシマＵＶ光（波長１７２ｎｍ、ピーク照度７５ｍＷ／ｃｍ２、積算光量４５０ｍＪ／ｃｍ２）を照射し、表面改質を施した。続いて、各フィルムの表面改質面に水を塗布し、水を風乾で乾燥させた。続いてラミネーターを用いて偏光膜と透明保護フィルムを貼り合わせ、偏光膜と透明保護フィルムが直接接合した偏光フィルムを得た。 <Comparative example 3>
In a nitrogen-substituted atmosphere with an oxygen concentration of about 2.5%, the polarizing film surface of the optical film laminate containing the polarizing film obtained above and a 23 μm thick cycloolefin resin film (Zeon Excimer UV light (wavelength 172 nm, peak illuminance 75 mW/cm 2 , cumulative light intensity 450 mJ/ cm 2 ) to perform surface modification. Subsequently, water was applied to the surface-modified surface of each film, and the water was air-dried. Subsequently, the polarizing film and the transparent protective film were bonded together using a laminator to obtain a polarizing film in which the polarizing film and the transparent protective film were directly bonded.
酸素濃度約２．５％の窒素置換雰囲気下において、上記で得られた偏光膜を含む光学フィルム積層体の偏光膜面、及び、透明保護フィルムとして、厚み２３μｍのシクロオレフィン系樹脂フィルム（日本ゼオン社製、ＺＦ１２）に、エキシマＵＶ処理装置（ウシオ電機社製、ＳＶＣ３４２Ｓ－１Ｎ２－ＭＮ３－ＫＷＯ１、キセノンエキシマランプ）を用い、エキシマＵＶ光（波長１７２ｎｍ、ピーク照度７５ｍＷ／ｃｍ２、積算光量４５０ｍＪ／ｃｍ２）を照射し、表面改質を施した。続いて、各フィルムの表面改質面に水を塗布し、水を風乾で乾燥させた。続いてラミネーターを用いて偏光膜と透明保護フィルムを貼り合わせ、偏光膜と透明保護フィルムが直接接合した偏光フィルムを得た。 <Comparative example 3>
In a nitrogen-substituted atmosphere with an oxygen concentration of about 2.5%, the polarizing film surface of the optical film laminate containing the polarizing film obtained above and a 23 μm thick cycloolefin resin film (Zeon Excimer UV light (wavelength 172 nm, peak illuminance 75 mW/cm 2 , cumulative light intensity 450 mJ/ cm 2 ) to perform surface modification. Subsequently, water was applied to the surface-modified surface of each film, and the water was air-dried. Subsequently, the polarizing film and the transparent protective film were bonded together using a laminator to obtain a polarizing film in which the polarizing film and the transparent protective film were directly bonded.
上記の各実施例及び比較例で得た偏光フィルムを用い、実施例１と同様の評価を行った。結果を表１に示す。
The same evaluation as in Example 1 was performed using the polarizing films obtained in each of the above Examples and Comparative Examples. The results are shown in Table 1.
Claims (4)
- 偏光膜と透明保護フィルムとを、粘着剤層又は粘着剤層を介さずに、直接、接合する偏光フィルムの製造方法であって、
前記偏光膜、及び前記透明保護フィルムの少なくとも一方の貼合面に、紫外光を照射して表面処理をした後、前記偏光膜と前記透明保護フィルムとを揮発性媒体を介して貼合して積層体を製造する工程と、
得られた積層体を加熱することにより、前記揮発性媒体を乾燥して、前記偏光膜と前記透明保護フィルムとを接合する工程を含むことを特徴とする偏光フィルムの製造方法。 A method for producing a polarizing film in which a polarizing film and a transparent protective film are directly bonded without an adhesive layer or an adhesive layer, the method comprising:
After surface-treating the bonding surface of at least one of the polarizing film and the transparent protective film by irradiating ultraviolet light, the polarizing film and the transparent protective film are bonded via a volatile medium. A process of manufacturing a laminate;
A method for producing a polarizing film, comprising the step of drying the volatile medium by heating the obtained laminate and joining the polarizing film and the transparent protective film. - 前記接合する工程において、前記積層体を加熱する温度が８０℃以下であることを特徴とする請求項１に記載の偏光フィルムの製造方法。 The method for producing a polarizing film according to claim 1, wherein in the joining step, the temperature at which the laminate is heated is 80° C. or less.
- 前記偏光膜と前記透明保護フィルムとの接合面の接着力が、剥離角度９０°、剥離速度１０００ｍｍ／分の条件下で、０．５Ｎ／１５ｍｍ以上であることを特徴とする請求項１又は２に記載の偏光フィルムの製造方法。 2. The adhesive force of the bonding surface between the polarizing film and the transparent protective film is 0.5 N/15 mm or more under conditions of a peeling angle of 90° and a peeling speed of 1000 mm/min. A method for producing a polarizing film as described in .
- ２０℃の水に２４時間浸漬前後おける、前記偏光膜と前記透明保護フィルムとの接合面の接着力の変化比（浸漬後の接着力／浸漬前の接着力）が、剥離角度９０°、剥離速度１０００ｍｍ／分の条件下で、０．５以上であることを特徴とする請求項１～３のいずれかに記載の偏光フィルムの製造方法。 The change ratio of the adhesive strength of the bonding surface between the polarizing film and the transparent protective film before and after immersion in water at 20°C for 24 hours (adhesion strength after immersion/adhesion strength before immersion) was determined at a peeling angle of 90° and a peeling angle of 90°. The method for producing a polarizing film according to any one of claims 1 to 3, wherein the polarizing film is 0.5 or more at a speed of 1000 mm/min.
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