JP6097473B2 - 光学フィルム用粘着剤組成物、光学フィルム用粘着剤層、粘着型光学フィルム、および画像表示装置 - Google Patents
光学フィルム用粘着剤組成物、光学フィルム用粘着剤層、粘着型光学フィルム、および画像表示装置 Download PDFInfo
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- JP6097473B2 JP6097473B2 JP2011119155A JP2011119155A JP6097473B2 JP 6097473 B2 JP6097473 B2 JP 6097473B2 JP 2011119155 A JP2011119155 A JP 2011119155A JP 2011119155 A JP2011119155 A JP 2011119155A JP 6097473 B2 JP6097473 B2 JP 6097473B2
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- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 125000004076 pyridyl group Chemical group 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 239000012966 redox initiator Substances 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000006884 silylation reaction Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 235000010378 sodium ascorbate Nutrition 0.000 description 1
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 description 1
- 229960005055 sodium ascorbate Drugs 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
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- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 239000005028 tinplate Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- WEAPVABOECTMGR-UHFFFAOYSA-N triethyl 2-acetyloxypropane-1,2,3-tricarboxylate Chemical compound CCOC(=O)CC(C(=O)OCC)(OC(C)=O)CC(=O)OCC WEAPVABOECTMGR-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 125000006617 triphenylamine group Chemical group 0.000 description 1
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- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 229960001939 zinc chloride Drugs 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
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- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- C09J175/04—Polyurethanes
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- G02B5/305—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks including organic materials, e.g. polymeric layers
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- G—PHYSICS
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- 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
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/80—Constructional details
- H10K30/865—Intermediate layers comprising a mixture of materials of the adjoining active layers
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- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
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- 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
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Description
(i)偏光子の厚みが薄いため、物理的にマイクロゲルが表面に析出する(表面凹凸が形成される)。
(ii)偏光子の厚みが薄いため、反射でマイクロゲルに起因する欠点が見え易くなる。
上記(i)、(ii)に由来する外観不良を解消するためにも、厚みが10μm以下の薄型偏光子を備える偏光板用として使用される粘着剤組成物では、特にマイクロゲルを除去することが要求されている。
−SiRaM3−a (1)
(式中、Rは、置換基を有していてもよい、炭素数1〜20の1価の有機基であり、Mは水酸基または加水分解性基であり、aは1〜3の整数である。但し、Rが複数存在するとき複数のRは互いに同一であっても異なっていてもよく、Mが複数存在するとき複数のMは互いに同一であっても異なっていてもよい。)で表される反応性シリル基を有する。
(式中、R1、R2およびR3は、炭素数1〜6の1価の炭化水素基であり、同一分子中で同一であっても異なっていてもよい。)で表されるアルコキシシリル基が好ましい。
一般式(2):RaM3−aSi−X−Y−(AO)n−Z
(式中、Rは、置換基を有していてもよい、炭素数1〜20の1価の有機基であり、Mは水酸基または加水分解性基であり、aは1〜3の整数である。但し、Rが複数存在するとき複数のRは互いに同一であっても異なっていてもよく、Mが複数存在するとき複数のMは互いに同一であっても異なっていてもよい。AOは、直鎖または分岐鎖の炭素数1〜10のオキシアルキレン基を示し、nは1〜1700であり、オキシアルキレン基の平均付加モル数を示す。Xは、炭素数1〜20の直鎖または分岐鎖のアルキレン基を示す。Yは、エーテル結合、エステル結合、ウレタン結合、またはカーボネート結合を示す。
一般式(2A):−Y1−X−SiRaM3−a
(式中、R、M、Xは、前記と同じ。Y1は単結合、−CO−結合、−CONH−結合、または−COO−結合を示す。)、または、
一般式(2B):−Q{−(OA)n−Y−X−SiRaM3−a}m
(式中、R、M、X、Yは、前記と同じ。OAは前記のAOに同じで、nは前記と同じ。Qは、2価以上の炭素数1〜10の炭化水素基であり、mは当該炭化水素基の価数と同じ。)で表される基である。)で表される化合物が挙げられる。
一般式(4):Z0−A2−O−(A1O)n−Z1
(式中、A1Oは炭素数2〜6のオキシアルキレン基であり、nは1〜1700であり、A1Oの平均付加モル数を示す。Z1は、水素原子、または−A2−Z0である。A2は炭素数2〜6のアルキレン基である。);
一般式(5):Z0−A2−NHCOO−(A1O)n−Z2
(式中、A1Oは炭素数2〜6のオキシアルキレン基であり、nは1〜1700であり、A1Oの平均付加モル数を示す。Z2は、水素原子、または−CONH−A2−Z0である。A2は炭素数2〜6のアルキレン基である。);
一般式(6):Z3−O−(A1O)n−CH{−CH2−(A1O)n−Z3}2
(式中、A1Oは炭素数2〜6のオキシアルキレン基であり、nは1〜1700であり、A1Oの平均付加モル数を示す。Z3は、水素原子、または−A2−Z0であり、いずれか少なくとも1つのZ3は−A2−Z0である。A2は炭素数2〜6のアルキレン基である。)で表される化合物が好ましい。Z0は、いずれも前記一般式(3)で表されるアルコキシシリル基である。A1Oのオキシアルキレン基は、直鎖または分岐鎖のいずれでもよく、特にオキシプロピレン基が好ましい。A2のアルキレン基は、直鎖または分岐鎖のいずれでもよく、特にプロピレン基が好ましい。
(式中、R1、R2およびR3は、炭素数1〜6の1価の炭化水素基であり、同一分子中で同一であっても異なっていてもよい。nは1〜1700であり、オキシプロピレン基の平均付加モル数を示す。
(式中、R1、R2およびR3は前記と同じ。)で表されるトリアルコキシシリル基である。)で表される化合物が好適に用いられる。
薄型偏光膜は、二色性物質を配向させたPVA系樹脂からなる連続ウェブの偏光膜であって、非晶性エステル系熱可塑性樹脂基材に製膜されたPVA系樹脂層を含む積層体が空中補助延伸とホウ酸水中延伸とからなる2段延伸工程で延伸されることにより、10μm以下の厚みにされたものである。かかる薄型偏光膜は、単体透過率をT、偏光度をPとしたとき、P>−(100.929T−42.4−1)×100(ただし、T<42.3)、およびP≧99.9(ただし、T≧42.3)の条件を満足する光学特性を有するようにされたものであることが好ましい。
更に具体的には、次のような方法により、薄型偏光膜を製造することができる。
上記の薄型偏光膜の製造方法は、上記工程以外に、その他の工程を含み得る。その他の工程としては、例えば、不溶化工程、架橋工程、乾燥(水分率の調節)工程等が挙げられる。その他の工程は、任意の適切なタイミングで行い得る。
上記不溶化工程は、代表的には、ホウ酸水溶液にPVA系樹脂層を浸漬させることにより行う。不溶化処理を施すことにより、PVA系樹脂層に耐水性を付与することができる。当該ホウ酸水溶液の濃度は、水100重量部に対して、好ましくは1重量部〜4重量部である。不溶化浴(ホウ酸水溶液)の液温は、好ましくは20℃〜50℃である。好ましくは、不溶化工程は、積層体作製後、染色工程や水中延伸工程の前に行う。
上記架橋工程は、代表的には、ホウ酸水溶液にPVA系樹脂層を浸漬させることにより行う。架橋処理を施すことにより、PVA系樹脂層に耐水性を付与することができる。当該ホウ酸水溶液の濃度は、水100重量部に対して、好ましくは1重量部〜4重量部である。また、上記染色工程後に架橋工程を行う場合、さらに、ヨウ化物を配合することが好ましい。ヨウ化物を配合することにより、PVA系樹脂層に吸着させたヨウ素の溶出を抑制することができる。ヨウ化物の配合量は、水100重量部に対して、好ましくは1重量部〜5重量部である。ヨウ化物の具体例は、上述のとおりである。架橋浴(ホウ酸水溶液)の液温は、好ましくは20℃〜50℃である。好ましくは、架橋工程は上記第2のホウ酸水中延伸工程の前に行う。好ましい実施形態においては、染色工程、架橋工程および第2のホウ酸水中延伸工程をこの順で行う。
式中、R1、R2およびR3は、それぞれ独立に、水素原子または炭素原子数1〜20の有機残基を示す。なお、有機残基は酸素原子を含んでいてもよい。
(メタ)アクリル系ポリマーの重量平均分子量および分散比(重量平均分子量/数平均分子量)は、GPC(ゲル・パーミエーション・クロマトグラフィー)により測定した。
・分析装置:東ソー(株)製、HLC−8120GPC
・カラム:東ソー社製、G7000HXL+GMHXL+GMHXL
・カラムサイズ:各7.8mmφ×30cm 計90cm
・カラム温度:40℃
・流量:0.8ml/min
・注入量:100μl
・溶離液:テトラヒドロフラン
・検出器:示差屈折計(RI)
・標準試料:ポリスチレン
厚さ80μmのポリビニルアルコールフィルムを、速度比の異なるロール間において、30℃、0.3%濃度のヨウ素溶液中で1分間染色しながら、3倍まで延伸した。その後、60℃、4%濃度のホウ酸、10%濃度のヨウ化カリウムを含む水溶液中に0.5分間浸漬しながら総合延伸倍率が6倍まで延伸した。次いで、30℃、1.5%濃度のヨウ化カリウムを含む水溶液中に10秒間浸漬することで洗浄した後、50℃で4分間乾燥を行い偏光子(厚み25μm)を得た。当該偏光子の視認側に、厚さ40μmのトリアセチルセルロースフィルムをポリビニルアルコール系接着剤により貼り合わせ、粘着剤塗布面側に、厚さ33μmのノルボルネン系樹脂フィルム(商品名「ゼオノアフィルムZD12」、日本ゼオン社製)からなる位相差板を透明保護フィルムとして貼り合わせて偏光板X(偏光度99.995)を作製した。
<アクリル系ポリマー(A)の調製>
攪拌羽根、温度計、窒素ガス導入管、冷却器を備えた4つ口フラスコに、ブチルアクリレート85.8重量%、ベンジルアクリレート13.2重量%、4−ヒドロキシブチルアクリレート1部、重合開始剤として2,2’−アゾビスイソブチロニトリル0.1部を酢酸エチル100部と共に仕込み、緩やかに攪拌しながら窒素ガスを導入して窒素置換した後、フラスコ内の液温を55℃付近に保って8時間重合反応を行い、重量平均分子量(Mw)75万、(重量平均分子量(Mw))/(数平均分子量(Mn))=4.1のアクリル系ポリマー(A)の溶液を調製した。
製造例1において、アクリル系ポリマーを形成するモノマーの種類またはその割合、さらにはアクリル系ポリマーの分子量を表1に示すように変えた他は製造例1と同様にして、アクリル系ポリマー(B)乃至(J)の溶液を調製した。
BA:ブチルアクリレート、BzA:ベンジルアクリレート、HBA:4−ヒドロキシブチルアクリレート、HEA:2−ヒドロキシエチルアクリレート、AA:アクリル酸、を示す。
(粘着剤組成物の調製)
製造例1で得られたアクリル系ポリマー(A)溶液の固形分100部に対して、0.3部のジベンゾイルパーオキシド(日本油脂社製のナイパーBMT(SV))、1部のイソシアネート架橋剤(日本ポリウレタン工業社製のコロネートL,トリメチロールプロパンのトリレンジイソシアネートのアダクト体)、0.5部のポリエーテル化合物(カネカ社製のサイリルSAT10)を配合して、実施例1に係るアクリル系粘着剤組成物(固形分20重量%)を調整した。
次いで、上記アクリル系粘着剤組成物Aを、シリコーン処理を施した、厚さ38μmのポリエチレンテレフタレート(PET)フィルム(三菱化学ポリエステルフィルム社製,MRF38)の片面に、乾燥後の粘着剤層の厚さが23μmになるように塗布し、155℃で1分間乾燥処理して粘着剤層を形成した。
上記偏光板の透明保護フィルム側(位相差板側)に、上記粘着剤層を形成したシリコーン処理を施したPETフィルムを、それぞれ転写し粘着型偏光板を作製した。
実施例1において、アクリル系ポリマーの種類、固形分含有量、添加剤の種類および配合量を表2に示すように変えた他は実施例1と同様にして、実施例2〜13、15〜17、比較例1〜3に係るアクリル系粘着剤組成物を調整した。次いで、各アクリル系粘着剤組成物を、実施例1と同様にシリコーン処理を施した、厚さ38μmのポリエチレンテレフタレート(PET)フィルム(三菱化学ポリエステルフィルム社製,MRF38)の片面に、乾燥後の粘着剤層の厚さが23μmになるように塗布し、155℃で1分間乾燥処理して粘着剤層を形成した。さらに、各偏光板の透明保護フィルム側(位相差板側)に、上記粘着剤層を形成したシリコーン処理を施したPETフィルムを、それぞれ転写し、実施例2〜13、15〜17、比較例1〜3に係る粘着型偏光板を作製した。
(粘着型偏光板の作製)
実施例1で使用した偏光板X(偏光度99.995)の粘着剤層を形成する透明保護フィルム側(位相差板側)に、ワイヤーバーにて下塗り剤を塗布して、下塗り層(厚さ100nm)を形成した。下塗り剤には、チオフェン系ポリマーを含む溶液(ナガセケムテックス社製,商品名「デナトロンP521−AC」)を水とイソプロピルアルコールの混合溶液で希釈し、固形分濃度が0.6重量%となるように調製したものを用いた。次いで、下塗り層に、実施例1と同様に粘着剤層を形成したシリコーン処理を施したPETフィルムを転写し、粘着型偏光板を作製した。
(薄型偏光膜の作製とそれを用いた偏光板の作製)
薄型偏光膜を作製するため、まず、非晶性PET基材に24μm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10μm厚のPVA層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高機能偏光膜を構成する、厚さ10μmのPVA層を含む光学フィルム積層体を生成することができた。更に、当該光学フィルム積層体の偏光膜の表面にポリビニルアルコール系接着剤を塗布しながら、けん化処理した80μm厚のトリアセチルセルロースフィルムを貼合せたのち、非晶性PET基材を剥離した。その後、非晶性PET基材を剥離した側の偏光膜の表面にポリビニルアルコール系接着剤を塗布しながら、厚さ33μmのノルボルネン系樹脂フィルム(商品名「ゼオノアフィルムZD12」、日本ゼオン社製)からなる位相差板を透明保護フィルムとして貼り合わせて、薄型偏光膜を用いた偏光板Iを作製した。
実施例1において、偏光板の種類、アクリル系ポリマーの種類、固形分含有量、添加剤の種類および配合量を表2に示すように変えた他は実施例1と同様にして、実施例18および比較例4に係る粘着型偏光板を作製した。
(偏光板の作製)
実施例18において、粘着剤塗布面側に、ノルボルネン系樹脂フィルムからなる位相差板を貼り合わせないこと以外は、実施例18と同様にして偏光板J(偏光度99.995)を作製した。
実施例18において、偏光板の種類、アクリル系ポリマーの種類、固形分含有量、添加剤の種類および配合量を表2に示すように変えた他は実施例18と同様にして、実施例19に係る粘着型偏光板を作製した。
精秤したブリキシャーレ(A)に粘着剤組成物を1g程度入れ、合計重量を精秤した後(B)、100℃で4時間加熱した。その後、加熱後の合計重量を精秤した(C)。得られた重量値を用いて下記式から固形分含有量(ベース)を算出した。
(ベース(%))=100×[(加熱後重量(C−A))/(加熱前重量(B−A))]
粘着剤塗工液の粘度(P)は、東機産業(株)製のVISCOMETER modelBHを用いて下記の条件で測定した。
ローター:No.4
回転数:20rpm
測定温度:30℃
(メタ)アクリル系ポリマー重合後の粘着剤組成物を粗さ1μmのろ過メッシュにてろ過し、ろ過メッシュ上に残ったゲルの量を目視で観察し、以下の基準に従って評価した。
○:ゲルが全く残ってなかった
△:微量のゲルが残存していた
×:多量のゲルが残存していた
シリコーン処理を施した、38μmのPETフィルム(三菱化学ポリエステルフィルム社製、MRF38)の片面に、乾燥後の粘着剤層厚みが20μmとなるようにファウンテンダイコーターを用いて、粗さ1μmのろ過メッシュにてろ過した粘着剤溶液を塗工した。その塗工直後の外観を目視にて観察した。
◎:塗工スジ、気泡、白化など一切なく、実用上問題ない非常に良好な塗工外観
○:微弱な塗工スジ、気泡、白化などがあるが、実用上問題ない良好な塗工外観
△:塗工スジ、気泡、白化などが所々あるが、実用上問題ない塗工外観
×:塗工スジ、気泡、白化などが多発しており、実用上問題がある
液晶パネルの片側にタッチパネル層が形成された、タッチパネル層付き液晶パネルにおいて、そのタッチパネル層の最表面(ITO処理面)に、10mm×150mmに切りだした粘着型偏光板を粘着剤層を介して貼着した。次いで、長辺の両端部5mm幅に銀インクを印刷し電極を形成した。その後、室温で24時間静置し、銀印刷を乾燥させた。作製したサンプルの初期抵抗値(R0)を測定した後、65℃・95%RH条件下で150時間放置し、耐久性後の抵抗値(R1)を測定した。次いで、初期抵抗値(R0)に対する変化率(R1/R0)を求め、ITO劣化性を評価した。なお、抵抗値は、日置電機(株)製「デジタルミリオームハイテスター 品番3540」を用いて、両端の銀ペースト部分に電極をつけて測定した。抵抗値の変化率が20%未満であれば腐食性が良好と言える。
○:ほとんど劣化せず、実用上問題がない
△:多少の劣化が認められるが、実用上問題がない
×:劣化が激しく、実用上問題がある
サンプルを縦420mm×横320mmに裁断し、表面にITO処理を施した液晶パネル上に、ラミネーターを用いて貼着した。次いで、50℃、5atmで15分間オートクレーブ処理して、上記サンプルを完全に無アルカリガラス板に密着させた。かかる処理の施されたサンプルに、80℃で500時間処理(加熱試験)を施し、さらに、60℃90%RHで500時間処理(加湿試験)を施した後、発泡、剥がれ、浮きの状態を下記基準で目視にて評価した。
◎:発泡、剥がれ、浮きなしなどの外観上の変化が全くない
○:わずかながら端部に剥がれ、または発泡があるが、実用上問題なし
△:端部に剥がれ、または発泡があるが、特別な用途でなければ、実用上問題なし
×:端部に著しい剥がれ、または発泡があり、実用上問題あり
サンプルを縦420mm×横320mmに裁断し、表面にITO処理を施した液晶パネル上に、ラミネーターを用いて貼り付け、次いで、50℃、5atmで15分間オートクレーブ処理して完全に密着させた。その後、人の手によって無アルカリガラス板からサンプルを剥がし、下記基準でリワーク性を評価した。
○:フィルムの破断がなく良好に剥離可能
△:フィルム破断したが、再度の剥離によって剥がせた
×:フィルム破断し、再度の剥離によっても剥がせなかった
粘着型偏光板を、コントラスト5000:1の液晶パネルの上下にクロスニコルになるように貼り分け、LEDバックライトモジュールの輝度を10000カンデラとし、黒表示時の粘着剤ゲル起因の異物による表示不良について目視で観察した。なお、評価は、SONY社製BRAVIA 46インチTV(KDL−46HX900)を用いて実施した。
◎:異物欠点が全く見られず実用上問題がない
○:異物欠点がわずかに見られるものの実用上問題がない
△:異物欠点が多少あるが、実用上問題がない
×:多くの異物欠点が見られ実用上問題がある
「ナイパー」:ジベンゾイルパーオキシド(日本油脂社製のナイパーBMT(SV))、「C/L」:日本ポリウレタン工業社製のコロネートL(トリメチロールプロパンのトリレンジイソシアネートのアダクト体)、「OL−1」:架橋促進剤(ジオクチルスズラウレート(東京ファインケミカル社製、商品名エンビライザーOL−1))、「SAT10」:ポリエーテル化合物(カネカ社製のサイリルSAT10)、「B/L輝度」:LEDバックライトの輝度を示す。
Claims (6)
- (メタ)アクリル系ポリマー、ラジカル発生剤および溶剤を含有し、前記(メタ)アクリル系ポリマー100重量部に対するラジカル発生剤の含有量が0.02〜2重量部である光学フィルム用粘着剤組成物であって、
前記(メタ)アクリル系ポリマー100重量部に対して、イソシアネート系架橋剤を0.01〜5重量部含有し、
前記(メタ)アクリル系ポリマーが、モノマー単位としてカルボキシル基含有モノマーを含まず、アルキル(メタ)アクリレート30〜98.9重量%、重合性芳香環含有モノマー1〜50重量%、ヒドロキシル基含有モノマー0.1〜5重量%を共重合してなる、ゲルパーミエーションクロマトグラフィーによる重量平均分子量が30万〜95万の(メタ)アクリル系ポリマーであり、
前記(メタ)アクリル系ポリマーを含む固形分含有量が20重量%以上であり、前記溶剤の含有量が80重量%以下であり、かつ23℃でのB型粘度計100rpmでの粘度が1〜12Pa・sであることを特徴とする光学フィルム用粘着剤組成物。 - 前記重合性芳香環含有モノマーが、ベンジル(メタ)アクリレートであることを特徴とする請求項1に記載の光学フィルム用粘着剤組成物。
- 前記ヒドロキシル基含有モノマーが、4−ヒドロキシブチルアクリレートであることを特徴とする請求項1または2に記載の光学フィルム用粘着剤組成物。
- 請求項1〜3のいずれかに記載の光学フィルム用粘着剤組成物により形成されていることを特徴とする光学フィルム用粘着剤層。
- 光学フィルムの少なくとも片側に、請求項4に記載の光学フィルム用粘着剤層が形成されていることを特徴とする粘着型光学フィルム。
- 前記光学フィルムが、偏光子の片側または両側に透明保護フィルムを有する偏光板であることを特徴とする請求項5に記載の粘着型光学フィルム。
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US13/993,256 US20130280529A1 (en) | 2010-12-13 | 2011-12-12 | Adhesive composition for optical films, adhesive layer for optical films, pressure-sensitive adhesive layer-carrying optical film, and image display device |
CN201180059964.8A CN103261351B (zh) | 2010-12-13 | 2011-12-12 | 光学薄膜用粘合剂组合物、光学薄膜用粘合剂层、粘合型光学薄膜及图像显示装置 |
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