JP6690808B2 - 反射防止フィルムおよびその製造方法 - Google Patents
反射防止フィルムおよびその製造方法 Download PDFInfo
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- JP6690808B2 JP6690808B2 JP2018503479A JP2018503479A JP6690808B2 JP 6690808 B2 JP6690808 B2 JP 6690808B2 JP 2018503479 A JP2018503479 A JP 2018503479A JP 2018503479 A JP2018503479 A JP 2018503479A JP 6690808 B2 JP6690808 B2 JP 6690808B2
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920001197 polyacetylene Polymers 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920006294 polydialkylsiloxane Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
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- 229920000123 polythiophene Polymers 0.000 description 1
- ZGSOBQAJAUGRBK-UHFFFAOYSA-N propan-2-olate;zirconium(4+) Chemical compound [Zr+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] ZGSOBQAJAUGRBK-UHFFFAOYSA-N 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007764 slot die coating Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical group CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- ZUEKXCXHTXJYAR-UHFFFAOYSA-N tetrapropan-2-yl silicate Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)OC(C)C ZUEKXCXHTXJYAR-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-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
- 210000002268 wool Anatomy 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
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- G02B1/111—Anti-reflection coatings using layers comprising organic materials
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/113—Anti-reflection coatings using inorganic layer materials only
- G02B1/115—Multilayers
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Description
[数式1]
中空状無機ナノ粒子の半径に対するシェル層(2)の厚さの比率=(中空状無機ナノ粒子のシェル層(2)の厚さ)/(中空状無機ナノ粒子の半径)
[数式1]
中空状無機ナノ粒子の半径に対するシェル層(2)の厚さの比率=(中空状無機ナノ粒子のシェル層(2)の厚さ)/(中空状無機ナノ粒子の半径)
[数式1]
中空状無機ナノ粒子の半径に対するシェル層(2)の厚さの比率=(中空状無機ナノ粒子のシェル層(2)の厚さ)/(中空状無機ナノ粒子の半径)
[化学式1]
[化学式2]
[化学式3]
[化学式4]
[化学式5]
[数式1]
中空状無機ナノ粒子の半径に対するシェル層(2)の厚さの比率=(中空状無機ナノ粒子のシェル層(2)の厚さ)/(中空状無機ナノ粒子の半径)。
KYOEISHA社の塩タイプの帯電防止ハードコート液(固形分50重量%、製品名:LJD−1000)をトリアセチルセルロースフィルムに#10mayer barでコーティングし、90℃で1分間乾燥した後、150mJ/cm2の紫外線を照射して、約5〜6μmの厚さを有するハードコートフィルムを製造した。
ペンタエリスリトールトリアクリレート(PETA)、中空状シリカナノ粒子(半径:約35〜38nm、殻の厚さ:7〜9nm、殻の厚さ/半径:0.21〜0.29、密度:1.40g/cm3、JSC catalyst and chemicals社製品)、ソリッド状シリカナノ粒子(半径:約12nm、密度:2.65g/cm3)、含フッ素化合物(RS−537、DIC社)、開始剤(Irgacure127、Ciba社)を、全体固形分100重量部に対して、下記表1の重量比率でMIBK(methyl isobutyl ketone)溶媒に希釈した。
前記製造例のハードコートフィルム上に、前記得られた光硬化性コーティング組成物を#4mayer barで厚さが約110〜120nmとなるようにコーティングし、60℃の温度で1分間乾燥および硬化した。前記硬化時には、窒素パージング下、前記乾燥したコーティング物に252mJ/cm2の紫外線を照射した。
実施例のコーティング組成物の固形分の重量比率(単位:重量部)
半径が約22〜25nm、殻の厚さが7〜9nm、殻の厚さ/半径が0.32〜0.45、密度が1.86g/cm3の中空状シリカナノ粒子(JSC catalyst and chemicals社製品)を用いた点を除き、実施例1と同様の方法で反射防止フィルムを製造した。
半径が約19〜22nm、殻の厚さが7〜9nm、殻の厚さ/半径が0.36〜0.53、密度が2.07g/cm3の中空状シリカナノ粒子(JSC catalyst and chemicals社製品)を用いた点を除き、実施例1と同様の方法で反射防止フィルムを製造した。
半径が約22〜25nm、殻の厚さが7〜9nm、殻の厚さ/半径が0.32〜0.45、密度が1.86g/cm3の中空状シリカナノ粒子(JSC catalyst and chemicals社製品)を用いた点を除き、実施例3と同様の方法で反射防止フィルムを製造した。
前記実施例および比較例で得られた反射防止フィルムに対して、次のような項目の実験を施した。
実施例および比較例で得られた反射防止フィルムが可視光線領域(380〜780nm)で示す平均反射率を、Solidspec3700(SHIMADZU)装備を用いて測定した。
実施例および比較例で得られた反射防止フィルムの表面に黒いネームペンで5cmの長さの直線を描き、無塵川を用いて擦った時に消される回数を確認して、防汚性を測定した。
<測定基準>
О:消される時点が10回以下
△:消される時点が11回〜20回
X:消される時点が20回超過
前記スチールウールに荷重をかけて27rpmの速度で10回往復し、実施例および比較例で得られた反射防止フィルムの表面を擦った。肉眼で観察される1cm以下のスクラッチ1個以下が観察される最大荷重を測定した。
実験例1〜3の結果
Claims (15)
- ハードコート層;並びに
前記ハードコート層の一面に形成され、バインダー樹脂と、該バインダー樹脂に分散した中空状無機ナノ粒子およびソリッド状無機ナノ粒子とを含む低屈折層;を含み、
前記中空状無機ナノ粒子は、下記数式1による粒子半径に対するシェル層の厚さの比率が0.3以下であり、
前記ハードコート層と前記低屈折層との界面から前記低屈折層全体厚さの30%以内に前記ソリッド状無機ナノ粒子全体中の70体積%以上が存在し、
前記ハードコート層と前記低屈折層との界面から上記低屈折層全体厚さの30%超過の領域に上記中空状無機ナノ粒子全体中の70体積%以上が存在し、
前記ソリッド状無機ナノ粒子が前記中空状無機ナノ粒子に比べて0.50g/cm3〜2.00g/cm3高い密度を有し、
前記ソリッド状無機ナノ粒子はソリッド状シリカナノ粒子である、
反射防止フィルム:
[数式1]
中空状無機ナノ粒子の半径に対するシェル層の厚さの比率=(中空状無機ナノ粒子のシェル層の厚さ)/(中空状無機ナノ粒子の半径)。 - 前記中空状無機ナノ粒子のシェル層の厚さは、0.1nm〜60nmである、
請求項1に記載の反射防止フィルム。 - 前記中空状無機ナノ粒子の粒子半径が35nm〜100nmである、
請求項1または2に記載の反射防止フィルム。 - 前記低屈折層は、
前記ソリッド状無機ナノ粒子全体中の70体積%以上が含まれている第1層と、
前記中空状無機ナノ粒子全体中の70体積%以上が含まれている第2層とを含み、
前記第1層が第2層に比べて前記ハードコート層および前記低屈折層の間の界面により近く位置する、
請求項1から3のいずれか1項に記載の反射防止フィルム。 - 前記反射防止フィルムは、380nm〜780nmの可視光線波長帯領域で0.8%以下の平均反射率を示す、
請求項1から4のいずれか1項に記載の反射防止フィルム。 - 前記ソリッド状無機ナノ粒子は、0.5nm〜100nmの半径を有する、
請求項1から5のいずれか1項に記載の反射防止フィルム。 - 前記低屈折層に含まれるバインダー樹脂は、光重合性化合物の(共)重合体および光反応性官能基を含む含フッ素化合物の間の架橋(共)重合体を含む、
請求項1から6のいずれか1項に記載の反射防止フィルム。 - 前記ハードコート層は、
光硬化性樹脂を含むバインダー樹脂;
および前記バインダー樹脂に分散した帯電防止剤を含む、
請求項1から7のいずれか1項に記載の反射防止フィルム。 - 前記ハードコート層の他の一面に結合された基材をさらに含む、
請求項1から8のいずれか1項に記載の反射防止フィルム。 - 光硬化型化合物またはその(共)重合体、光反応性官能基を含む含フッ素化合物、光開始剤、中空状無機ナノ粒子、およびソリッド状無機ナノ粒子を含む低屈折層形成用樹脂組成物をハードコート層上に塗布し、35℃〜100℃の温度で乾燥する段階と、
前記低屈折層形成用樹脂組成物の乾燥物を光硬化する段階と、を含み、
前記中空状無機ナノ粒子は、下記数式1による粒子半径に対するシェル層の厚さの比率が0.3以下であり、
前記ソリッド状無機ナノ粒子が前記中空状無機ナノ粒子に比べて0.50g/cm3〜2.00g/cm3高い密度を有し、
前記ソリッド状無機ナノ粒子はソリッド状シリカナノ粒子である、
反射防止フィルムの製造方法:
[数式1]
中空状無機ナノ粒子の半径に対するシェル層の厚さの比率=(中空状無機ナノ粒子のシェル層の厚さ)/(中空状無機ナノ粒子の半径)。 - 前記中空状無機ナノ粒子のシェル層の厚さは、0.1nm〜60nmである、
請求項10に記載の反射防止フィルムの製造方法。 - 前記ハードコート層上に塗布された低屈折層形成用樹脂組成物は、40℃〜80℃の温度で乾燥する、
請求項10または11に記載の反射防止フィルムの製造方法。 - 前記乾燥する段階は、10秒〜5分間行われる、
請求項10から12のいずれか1項に記載の反射防止フィルムの製造方法。 - 前記ソリッド状無機ナノ粒子は、2.00g/cm3〜4.00g/cm3の密度を有し、
前記中空状無機ナノ粒子は、1.20g/cm3〜3.50g/cm3の密度を有する、
請求項10から13のいずれか1項に記載の反射防止フィルムの製造方法。 - 光硬化型化合物またはその(共)重合体、光開始剤、および帯電防止剤を含むハードコート層形成用高分子樹脂組成物を基材上に塗布し、光硬化する段階をさらに含む、
請求項10から14のいずれか1項に記載の反射防止フィルムの製造方法。
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CN108025526B (zh) | 2020-06-09 |
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EP3385070A1 (en) | 2018-10-10 |
JP2018530770A (ja) | 2018-10-18 |
US10605960B2 (en) | 2020-03-31 |
US20180372917A1 (en) | 2018-12-27 |
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EP3385070A4 (en) | 2018-12-26 |
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