JP7186249B2 - 光学フィルム、これを用いた表示装置、光学フィルムの製造に用いる着色層形成用組成物 - Google Patents
光学フィルム、これを用いた表示装置、光学フィルムの製造に用いる着色層形成用組成物 Download PDFInfo
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- JP7186249B2 JP7186249B2 JP2021006475A JP2021006475A JP7186249B2 JP 7186249 B2 JP7186249 B2 JP 7186249B2 JP 2021006475 A JP2021006475 A JP 2021006475A JP 2021006475 A JP2021006475 A JP 2021006475A JP 7186249 B2 JP7186249 B2 JP 7186249B2
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- 239000012788 optical film Substances 0.000 title claims description 81
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- 238000010521 absorption reaction Methods 0.000 claims description 31
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- 238000004040 coloring Methods 0.000 claims description 22
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- 239000003086 colorant Substances 0.000 claims description 12
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- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 8
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- QGKMIGUHVLGJBR-UHFFFAOYSA-M (4z)-1-(3-methylbutyl)-4-[[1-(3-methylbutyl)quinolin-1-ium-4-yl]methylidene]quinoline;iodide Chemical group [I-].C12=CC=CC=C2N(CCC(C)C)C=CC1=CC1=CC=[N+](CCC(C)C)C2=CC=CC=C12 QGKMIGUHVLGJBR-UHFFFAOYSA-M 0.000 claims description 2
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- DZVCFNFOPIZQKX-LTHRDKTGSA-M merocyanine Chemical group [Na+].O=C1N(CCCC)C(=O)N(CCCC)C(=O)C1=C\C=C\C=C/1N(CCCS([O-])(=O)=O)C2=CC=CC=C2O\1 DZVCFNFOPIZQKX-LTHRDKTGSA-M 0.000 claims description 2
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- MPIAGWXWVAHQBB-UHFFFAOYSA-N [3-prop-2-enoyloxy-2-[[3-prop-2-enoyloxy-2,2-bis(prop-2-enoyloxymethyl)propoxy]methyl]-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(COC(=O)C=C)(COC(=O)C=C)COCC(COC(=O)C=C)(COC(=O)C=C)COC(=O)C=C MPIAGWXWVAHQBB-UHFFFAOYSA-N 0.000 description 4
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- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 description 1
- FZJCXIDLUFPGPP-UHFFFAOYSA-N propan-2-ol;toluene Chemical compound CC(C)O.CC1=CC=CC=C1 FZJCXIDLUFPGPP-UHFFFAOYSA-N 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
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- 229910000275 saponite Inorganic materials 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
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- 230000003595 spectral effect Effects 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
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- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- LVEOKSIILWWVEO-UHFFFAOYSA-N tetradecyl 3-(3-oxo-3-tetradecoxypropyl)sulfanylpropanoate Chemical compound CCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCC LVEOKSIILWWVEO-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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- 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
- 229910052902 vermiculite Inorganic materials 0.000 description 1
- 239000010455 vermiculite Substances 0.000 description 1
- 235000019354 vermiculite Nutrition 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
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Description
透明基材20は、光学フィルム11~15の基体となるフィルムであり、可視光線の透過性に優れる材料により形成される。透明基材20の形成材料としては、ポリエチレン、ポリプロピレン等のポリオレフィン、ポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリエチレンナフタレート等のポリエステル、ポリメチルメタクリレート等のポリアクリレート、ナイロン6、ナイロン66等のポリアミド、ポリイミド、ポリアリレート、ポリカーボネート、トリアセチルセルロース、ポリアクリレート、ポリビニルアルコール、ポリ塩化ビニル、シクロオレフィンコポリマー、含ノルボルネン樹脂、ポリエーテルサルフォン、ポリサルフォン等の透明樹脂や無機ガラスを利用できる。この中でも、ポリエチレンテレフタレートからなるフィルムを好適に利用できる。透明基材20の厚みは、特に限定されないが、10~100μmとすることが好ましい。
紫外線遮蔽率(%)=100-波長290~400nmの紫外線の平均透過率(%)
着色層21は、光学フィルム11~15を透過する光、及び、表示パネル10の表面に存在する金属電極等や反射部材によって反射されて再射出される反射光を低減するための層であり、可視光線を吸収するための色素を含有する。本実施形態に係る着色層21は、色素として、第1の色材及び第2の色材を含有する。第1の色材は、極大吸収波長が470~530nmの範囲内にあり、吸光スペクトルの半値幅が15~45nmであるものであり、第2の色材は、極大吸収波長が560~620nmの範囲内にあり、吸光スペクトルの半値幅が15~55nmであるものである。着色層21に含有させる第1の色材及び第2の色材として、上記の吸収特性を有するものを使用することにより、表示パネル10が発光する可視光線のうち、相対的に発光強度が低い波長域の可視光線を着色層21に吸収させることができる。
ハードコート層22は、光学フィルム11及び12に硬度を付与するための層であり、活性エネルギー線硬化性樹脂、光重合開始剤、溶剤を少なくとも含有するハードコート層形成用組成物を塗布し硬化させることによって形成することができる。また、着色層21より上層にハードコート層22を積層することにより、酸素バリア性を向上させることもできる。ハードコート層22によって酸素バリア性を付与される場合、着色層21に含まれる色素の劣化を抑制できる。ハードコート層22の厚みは、特に限定されないが、2~10μmであることが好ましい。ハードコート層22の厚みが2μm未満の場合、ハードコート層26の硬度が不足する可能性がある。ハードコート層22の厚みが10μmを超える場合、光学フィルム11及び12の薄型化に不利となるため好ましくない。ただし、ハードコート層22の膜厚は、光学フィルムに求められる表面硬度及び全体の厚みに応じて適宜設定することができる。また、ハードコート層22は、屈折率調整や硬度付与を目的として、金属酸化物微粒子を含有しても良い。ハードコート層22に金属酸化物微粒子を配合して高屈折率化することにより、後述する低屈折率層23と共に反射防止層を構成することができる。
低屈折率層23は、活性エネルギー線硬化性樹脂を少なくとも含有する低屈折率層形成用組成物を透明基材に塗布し硬化させることによって形成することができる。低屈折率層形成用組成物に用いる活性エネルギー線硬化性樹脂としては、ハードコート層22で説明したものを使用することができる。低屈折率層形成用組成物には、屈折率調整のために、LiF、MgF、3NaF・AlF、AlF、Na3AlF6等の微粒子やシリカ微粒子を配合しても良い。また、シリカ微粒子として、多孔質シリカ微粒子や中空シリカ微粒子等の粒子内部に空隙を有するものを用いることが、低屈折率層の低屈折率化に有効である。また、低屈折率層形成用組成物には、ハードコート層22で説明した光重合開始剤や溶剤、その他の添加剤を適宜配合しても良い。低屈折率層23の屈折率は、1.20~1.55とすることが好ましい。また、低屈折率層23の膜厚は、特に限定されないが、40nm~1μmとすることが好ましい。
防眩層24は、表面に微細な凹凸を有し、この凹凸で外光を散乱させることにより外光の映り込みを低減する層である。防眩層24は、活性エネルギー線硬化性樹脂と、必要に応じて有機微粒子及び/または無機微粒子とを含有する防眩層形成用組成物を塗布し硬化させることによって形成することができる。防眩層形成用組成物に用いる活性エネルギー線硬化性樹脂としては、ハードコート層22で説明したものを使用することができる。防眩層24の膜厚は、特に限定されないが、1~10μmであることが好ましい。
酸素バリア層25の酸素透過度は、10cc/(m2・day・atm)以下であり、5cc/(m2・day・atm)以下であることがより好ましく、1cc/(m2・day・atm)以下であることがさらに好ましい。酸素バリア層25の酸素バリア性により、着色層21に含まれる色材の酸化劣化(退色)を抑制することができる。酸素バリア層25の形成材料は、ポリビニルアルコール(PVA)、エチレン-ビニルアルコール共重合体(EVOH)、塩化ビリニデン、シロキサン樹脂等を含有するのが好ましく、三菱ガス化学社製のマクシーブ(登録商標)、株式会社クラレ製のエバール、旭化成株式会社のサランラテックス、サランレジン等を用いることができる。また、酸素バリア層25の厚さは特に限定されず、所望の酸素バリア性が得られる厚さとすればよい。
上述した着色層21は、活性エネルギー線硬化性樹脂と、光重合開始剤と、色素と、溶剤と、必要に応じて配合される添加剤とを含有する着色層形成用組成物を透明基材20に塗布し、塗膜を硬化させることによって形成することができる。着色層形成用組成物に用いる活性エネルギー線硬化性樹脂、光重合開始剤、溶剤は、ハードコート層22で説明したものを使用することができる。また、色素としては、上述した吸収特性を有する第1の色材及び第2の色材を使用し、必要に応じて上述した吸収特性を有する第3の色材を更に配合しても良い。添加剤としては、ラジカル捕捉剤、一重項酸素クエンチャー及び過酸化物分解剤の少なくとも1種類を使用することができる。
以下、各層の形成方法を説明する。
(着色層形成用組成物 使用材料)
着色層形成に用いる着色層形成用組成物の使用材料として下記のものを用いた。
なお、色材の最大吸収波長及び半値幅は硬化塗膜での特性値を分光透過率より算出した。・第1色材:
Dye-1 後述する化学式1で示されるピロメテンコバルト錯体染料(最大吸収波長
493nm、半値幅 26nm)
・第2色材:
Dye-2 テトラアザポルフィリン銅錯体染料(山田化学社製 FDG-007、最
大吸収波長595nm、半値幅 22nm)
Dye-3 テトラアザポルフィリン銅錯体染料(山本化成社製 PD-311S、最大吸収波長 586nm、半値幅 22nm)
・第3色材:
Dye-4 フタロシアニン銅錯体染料(山田化学社製 FDN-002、最大吸収波長 800nm)
・添加剤:
ヒンダードアミン系光安定剤 Chimassorb944FDL(BASFジャパン社製、分子量 2000~3100)
ヒンダードアミン系光安定剤 Tinuvin249(BASFジャパン社製、分子量
482)
一重項酸素クエンチャー D1781(東京化成工業社製)
・紫外線吸収剤:
Tinuvin479(BASFジャパン社製、極大吸収波長 322nm)
LA-36(ADEKA社製、極大吸収波長 310nm、350nm)
・活性エネルギー線硬化性樹脂:
UA-306H(共栄社化学社製、ペンタエリスリトールトリアクリレート ヘキサメチレンジイソシアネート ウレタンプレポリマー)
DPHA(ジペンタエリスリトールヘキサアクリレート)
PETA(ペンタエリスリトールトリアクリレート)
・開始剤:Omnirad 184(IGM Resing B.V.社製)
・溶剤:
MEK(メチルエチルケトン)
酢酸メチル
透明基材としては、下記のものを用いた。
・TAC:トリアセチルセルロースフィルム(富士フィルム社製 TG60UL、基材厚60μm、紫外線遮蔽率92.9%)
・PMMA:ポリメチルメタクリレートフィルム(住友化学社製 W001U80、基材厚80μm、紫外線遮蔽率93.4%)
・PET1:ポリエチレンテレフタレートフィルム(東洋紡社製 SRF、基材厚80μm、紫外線遮蔽率 88.3%)
・PET2:ポリエチレンテレフタレートフィルム(SKC社製 TOR20、基材厚40μm、紫外線遮蔽率88.6%)
表1、2に示す基材上に、表3に示す着色層形成用組成物を塗布し、80℃のオーブンで60秒間乾燥させた。その後、紫外線照射装置を用いて照射線量150mJ/cm2(フュージョンUVシステムズジャパン社製、光源Hバルブ)で紫外線照射を行うことにより塗膜を硬化させ、硬化後の膜厚が5.0μmとなるよう着色層1~6を形成した。なお、添加量は質量比である。
・酸素バリア層形成組成物:
PVA117(クラレ社製)80%水溶液
表1に示す実施例8の透明基材上に、上記の酸素バリア層形成用組成物を塗布し、乾燥させ、酸素透過度が1cc/m2・day・atmである表1の酸素バリア層1を形成した。
ハードコート層形成に用いるハードコート層形成用組成物の使用材料として下記のものを用いた。
・活性エネルギー線硬化性樹脂:
UA-306H(共栄社化学社製、ペンタエリスリトールトリアクリレートヘキサメチレンジイソシアネート ウレタンプレポリマー)
DPHA(ジペンタエリスリトールヘキサアクリレート)
PETA(ペンタエリスリトールトリアクリレート)
・開始剤:
Omnirad TPO(IGM Resins B.V.社製、吸収波長ピーク 2
75nm,379nm)
・溶剤:
MEK(メチルエチルケトン)
酢酸メチル
表1及び表2に示す透明基材または酸素バリア層上に、表4に示すハードコート層形成用組成物を塗布し、80℃のオーブンで60秒間乾燥させ、その後、紫外線照射装置を用いて照射線量150mJ/cm2で紫外線照射(フュージョンUVシステムズジャパン社製、光源Hバルブ)を行うことにより塗膜を硬化させ、硬化後の膜厚が5.0μmである表1及び2のハードコート層1を形成した。
防眩層形成に用いる防眩層形成用組成物の使用材料として下記のものを用いた。
・活性エネルギー線硬化性樹脂:
ライトアクリレートPE-3A(共栄社化学株式会社製、屈折率1.52)
・光重合開始剤:
Omnirad TPO(IGM Resins B.V.社製、吸収波長ピーク 275nm,379nm)
・樹脂粒子:
スチレン-メタクリル酸メチル共重合体粒子(屈折率1.515、平均粒径2.0μm)
・無機微粒子1:
合成スメクタイト
・無機微粒子2:
アルミナナノ粒子、平均粒径40nm
・溶剤
トルエン
イソプロピルアルコール
表5に示す防眩層形成用組成物を表1に示す実施例2の透明基材上に塗布し、80℃のオーブンで60秒間乾燥させ、その後、紫外線照射装置を用いて照射線量150mJ/cm2で紫外線照射(フュージョンUVシステムズジャパン社製、光源Hバルブ)を行うことにより塗膜を硬化させ、硬化後の膜厚が5.0μmである表1の防眩層1を形成した。
低屈折率層形成に用いる低屈折層形成用組成物として下記のものを用いた。
・屈折率調整剤:
多孔質シリカ微粒子分散液(平均粒子径75nm、固形分20%、溶剤メチルイソブチ
ルケトン) 8.5質量部
・防汚性付与剤:
オプツールAR-110(ダイキン工業社製、固形分15%、溶剤メチルイソブチルケトン) 5.6質量部
・活性エネルギー線硬化性樹脂:
ペンタエリスリトールトリアクリレート 0.4質量部
・開始剤:
Omnirad 184(IGM Resins B.V.社製) 0.07質量部、
・レベリング剤:
RS-77(DIC社製) 1.7質量部
・溶剤:
メチルイソブチルケトン 83.73質量部
表1及び表2で示した構成上に、上記組成の低屈折率層形成用組成物を塗布し、80℃のオーブンで60秒間乾燥させ、その後、紫外線照射装置(フュージョンUVシステムズジャパン社製、光源Hバルブ)を用いて照射線量200mJ/cm2で紫外線照射を行うことにより塗膜を硬化させて、硬化後の膜厚が100nmである表1及び表2の低屈折率層を形成した。
(着色層上 紫外線遮蔽率)
着色層より上層に基材がくる実施例1~10と、着色層のない比較例3は、基材を自動分光光度計((株)日立製作所製、U-4100)を用いて透過率を測定した。また、着色層が基材より上層にくる比較例1、2については、JIS-K5600付着性試験準拠のセロハンテープを用いて着色層より上層を剥離し、自動分光光度計((株)日立製作所製、U-4100)を用い、粘着テープをリファレンスとして着色層上層の透過率を測定した。これらの透過率を用いて、紫外域(290~400nm)の平均透過率を算出し、式(1)に示す紫外線遮蔽率を算出した。
式(1)
紫外線遮蔽率(%)=100-紫外域(290~400nm)の平均透過率(%)
光学フィルムの表面に、クレメンス型引掻き硬度試験機(テスター産業株式会社製、HA-301)を用いて、JIS-K5400-1990に準拠して、500gの荷重をかけた鉛筆(三菱鉛筆社製 UNI、鉛筆硬度H)を用いて試験を行い、キズによる外観の変化を目視で評価し、キズが観察されない場合を〇、キズが観察される場合を×とした。
得られた着色層を含む光学フィルムの信頼性試験として、キセノンウェザーメーター試験機(スガ試験機株式会社製、X75)を用い、キセノンランプ照度60W/cm2(300~400nm)、試験機内温度45℃・湿度50%RH条件にて120時間試験し、試験前後に自動分光光度計((株)日立製作所製、U-4100)を用いて透過率測定を行い、波長範囲470~530nmにて試験前の最小透過率を示す波長λ1での試験前後透過率差ΔTλ1、波長範囲560~620nmにて試験前の最小透過率を示す波長λ2での試験前後透過率差ΔTλ2、試験前後でのC光源での色差ΔEabを算出した。透過率差及び色差はゼロに近い方が良好であり、ΔEab≦5となるものが好ましい。
(透過特性)
得られた光学フィルムの透過率を自動分光光度計((株)日立製作所製、U-4100)を用いて測定し、この透過率を用いて、白表示時に光学フィルムを透過した光の効率を算出し、白表示透過特性として評価した。基準として、図6に示すスペクトルの白色有機EL光源とカラーフィルタを通して出力される白表示時のスペクトルの効率を100とした。
得られた光学フィルムの透過率を自動分光光度計((株)日立製作所製、U-4100)を用いて測定した。表示パネル反射率を40%とし、光学フィルムに低屈折率層又は防眩層などの反射防止層が観察側最表層に設けられている場合の表面反射率Rを1%、設けられていない場合の表面反射率Rを4%とし、他の各層での界面反射及び表面反射は考慮せず、光学フィルムの無い状態でのD65光源に対する表示装置反射値を100とした際の相対反射値を式(2)に基づいて算出し、表示装置反射特性として評価した。
得られた光学フィルムの透過率を自動分光光度計((株)日立製作所製、U-4100)を用いて測定し、図6に示すスペクトルの白色EL光源とカラーフィルタを通して出力される図7の赤色表示、緑色表示、青色表示スペクトルを測定した。測定した透過率と図7の赤色表示、緑色表示、青色表示スペクトルとを用いて算出されるCIE1931色度値からNTSC比を算出し、NTSC比を色再現性の指標として評価した。
5 表示パネル
11、12、13 光学フィルム
20 透明基材
21 着色層
22 ハードコート層
23 低屈折率層
24 防眩層
25 酸素バリア層
30 機能層
Claims (12)
- 透明基材と、
前記透明基材の一方面側に積層され、色素を含有する着色層と、
前記透明基材の他方面側に積層される機能層とを備え、
前記色素は、
極大吸収波長が470~530nmの範囲内にあり、吸光スペクトルの半値幅が15~45nmである第1の色材と、
極大吸収波長が560~620nmの範囲内にあり、吸光スペクトルの半値幅が15~55nmである第2の色材とを含有し、
前記透明基材のJIS L 1925に準拠した紫外線遮蔽率が85%以上であり、
前記着色層が、分子量2000以上のヒンダードアミン系光安定剤を含有し、
温度45℃・湿度50%RH条件にて、波長300~400nmでの照度が60W/cm 2 のキセノンランプの光を120時間照射する耐光性試験の前後の色差であるΔEabが3.3以下であることを特徴とする光学フィルム。 - 表面の500g荷重での鉛筆硬度がH以上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。
- 前記着色層が、過酸化物分解剤、一重項酸素クエンチャーの少なくとも1種類以上を含有す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。
- 前記耐光性試験の前後の色差ΔEabが2.0~3.3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。
- 前記着色層に含まれる、一重項酸素クエンチャーがジアルキルホスフェイト、ジアルキルジチオカルバネートまたはベンゼンジチオールあるいはその類似ジチオールの遷移金属錯体であることを特徴とする、請求項3に記載の光学フィルム。
- 前記着色層が、前記色素として、極大吸収波長が650~800nmの範囲内にある第3の色材を更に含有することを特徴とする、請求項1~5のいずれかに記載の光学フィルム。
- 前記着色層に含まれる色素が、ポルフィリン構造、メロシアニン構造、フタロシアニン構造、アゾ構造、シアニン構造、スクアリリウム構造、クマリン構造、ポリエン構造、キノン構造、テトラジポルフィリン構造、ピロメテン構造及びインジゴ構造のいずれかを有する化合物及びその金属錯体からなる群から選択される1以上の化合物を含むことを特徴とする、請求項1~6のいずれかに記載の光学フィルム。
- 前記透明基材と前記着色層との間、または、前記透明基材の前記他方面側に、酸素透過度が10cc/m2・day・atm以下の酸素バリア層を更に備えることを特徴とする、請求項1~7のいずれかに記載の光学フィルム。
- 前記機能層が、高屈折率層及び低屈折率層を含む反射防止層、または、防眩層を含むことを特徴とする、請求項1~8のいずれかに記載の光学フィルム。
- 帯電防止層または防汚層を更に含むことを特徴とする、請求項1~9のいずれかに記載の光学フィルム。
- 請求項1~10のいずれかに記載の光学フィルムを備える表示装置。
- 透明基材の一方面側に着色層が積層された光学フィルムを形成するために用いられ、着色活性エネルギー線硬化性樹脂と、光重合開始剤と、色素と、添加剤と、溶剤とを含有する着色層形成用組成物であって、
前記色素が、
極大吸収波長が470~530nmの範囲内にあり、吸光スペクトルの半値幅が15~45nmである第1の色材と、
極大吸収波長が560~620nmの範囲内にあり、吸光スペクトルの半値幅が15~55nmである第2の色材とを含有し、
前記添加剤が、分子量2000以上のヒンダードアミン系光安定剤を含有し、
温度45℃・湿度50%RH条件にて、波長300~400nmでの照度が60W/cm 2 のキセノンランプの光を前記光学フィルムに対して120時間照射する、耐光性試験の前後の色差であるΔEabが3.3以下であることを特徴とする、着色層形成用組成物。
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CN202180090800.5A CN116710814A (zh) | 2021-01-19 | 2021-09-22 | 光学膜、使用了该光学膜的显示装置、用于光学膜的制造的着色层形成用组合物 |
EP21921150.5A EP4279963A1 (en) | 2021-01-19 | 2021-09-22 | Optical film, display device using same, and composition for forming colored layer used for manufacturing optical film |
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