JP6453522B2 - 反射防止フィルム及びその製造方法 - Google Patents
反射防止フィルム及びその製造方法 Download PDFInfo
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- JP6453522B2 JP6453522B2 JP2018512616A JP2018512616A JP6453522B2 JP 6453522 B2 JP6453522 B2 JP 6453522B2 JP 2018512616 A JP2018512616 A JP 2018512616A JP 2018512616 A JP2018512616 A JP 2018512616A JP 6453522 B2 JP6453522 B2 JP 6453522B2
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- inorganic nanoparticles
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Description
本出願は、2015年11月4日付韓国特許出願第10−2015−0154591号及び2016年10月31日付韓国特許出願第10−2016−0142886号に基づく優先権の利益を主張し、当該韓国特許出願の文献に開示されたすべての内容は本明細書の一部として含まれる。
製造例:ハードコーティングフィルムの製造
共栄社化学株式会社製の塩タイプの帯電防止ハードコーティング液(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でコートし、90℃で1分乾燥した後、150mJ/cm2の紫外線を照射して約5〜6μmの厚みを有するハードコーティングフィルムを製造した。
(1)低屈折層製造用光硬化性コーティング組成物の製造
ペンタエリスリトールトリアクリレート(PETA)100重量部に対して、中空シリカナノ粒子(直径:約50〜60nm、密度:1.96g/cm3、JSC catalyst and chemicals社製)281重量部、ソリッドシリカナノ粒子(直径:約12nm、密度:2.65g/cm3)63重量部、第1含フッ素化合物(X−71−1203M、信越化学工業社製)131重量部、第2含フッ素化合物(RS−537、DIC社製)19重量部、開始剤(Irgacure 127、Ciba社製)31重量部を、MIBK(methyl isobutyl ketone)溶媒に固形分濃度3重量%になるように希釈した。
前記製造例のハードコーティングフィルム上に、前記で得られた光硬化性コーティング組成物を#4 mayer barで厚みが約110〜120nmになるようにコートし、下記表1の温度及び時間で乾燥及び硬化した。前記硬化時には窒素パージ下で前記乾燥されたコーティング物に252mJ/cm2の紫外線を照射した。
トリメチロールプロペイントリアクリレート(TMPTA)100重量部に対して、中空シリカナノ粒子(直径:約50〜60nm、密度:1.96g/cm3、JSC catalyst and chemicals社製)268重量部、ソリッドシリカナノ粒子(直径:約12nm、密度:2.65g/cm3)55重量部、第1含フッ素化合物(X−71−1203M、信越化学工業社製)144重量部、第2含フッ素化合物(RS−537、DIC社製)21重量部、開始剤(Irgacure 127、Ciba社製)31重量部を、MIBK(methyl isobutyl ketone)溶媒に固形分濃度3重量%になるように希釈した。
前記製造例のハードコーティングフィルム上に、前記で得られた光硬化性コーティング組成物を#4 mayer barで厚みが約110〜120nmになるようにコートし、下記表1の温度及び時間で乾燥及び硬化した。前記硬化時には窒素パージ下で前記乾燥されたコーティング物に252mJ/cm2の紫外線を照射した。
トリメチロールプロペイントリアクリレート(TMPTA)100重量部に対して、中空シリカナノ粒子(直径:約50〜60nm、密度:1.96g/cm3、JSC catalystand chemicals社製)268重量部、ソリッド二酸化チタン粒子(直径:約15nm、密度:4.3g/cm3)70重量部、第1含フッ素化合物(X−71−1203M、信越化学工業社製)149重量部、第2含フッ素化合物(RS−537、DIC社製)31重量部、開始剤(Irgacure 127、Ciba社製)31重量部を、MIBK(methyl isobutyl ketone)溶媒に固形分濃度3重量%になるように希釈した。
前記製造例のハードコーティングフィルム上に、前記で得られた光硬化性コーティング組成物を#4 mayer barで厚みが約110〜120nmになるようにコートし、下記表1の温度及び時間で乾燥及び硬化した。前記硬化時には窒素パージ下で前記乾燥されたコーティング物に252mJ/cm2の紫外線を照射した。
前記低屈折層製造用光硬化性コーティング組成物を塗布し、常温(25℃)で乾燥したことを除いては実施例1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1で用いたソリッドシリカナノ粒子63重量部をペンタエリスリトールトリアクリレート(PETA)63重量部にしたことを除いては、前記実施例1と同様の方法で低屈折層製造用光硬化性コーティング組成物を製造し、実施例1と同様の方法で反射防止フィルムを製造した。
前記実施例及び比較例で得られた反射防止フィルムに対し、次のような項目の実験を行った。
実施例及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Solidspec 3700(島津製作所株式会社製)装備を用いて測定した。
実施例及び比較例で得られた反射防止フィルムの表面に黒い色ネームペンで5cmの長さの直線を描いて、ポリエステルワイパーを用いて擦ったとき消える回数を確認して防汚性を測定した。
O:消える時点が10回以下
△:消える時点が11回〜20回
X:消える時点が20回超過
前記スチールウール(横*縦:2.5cm*2.5cm)に荷重をかけて27rpmの速度で10回往復し、実施例及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。
図1〜7の反射防止フィルムの断面で、ハードコーティング層から30nm以内に用いたソリッド無機ナノ粒子(ソリッドナノシリカ粒子)全体中の70体積%が存在する場合、相分離が起こったものとして決定した。
Claims (17)
- ハードコーティング層と、
前記ハードコーティング層の一面に形成され、バインダー樹脂と前記バインダー樹脂に分散された中空無機ナノ粒子及びソリッド無機ナノ粒子を含む低屈折層と、を含み、
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)重合体を含み、
前記光重合性化合物は、(メタ)アクリレートまたはビニル基を含む単量体またはオリゴマーを含み、
前記ハードコーティング層と前記低屈折層との界面から前記低屈折層全体の厚みの30%以内に前記ソリッド無機ナノ粒子全体中の70体積%以上が存在し、
前記ハードコーティング層と前記低屈折層との界面から前記低屈折層全体の厚みの30%超過の領域に前記中空無機ナノ粒子全体中の70体積%以上が存在し、
前記ソリッド無機ナノ粒子と前記中空無機ナノ粒子との密度差が、0.30g/cm 3 〜3.00g/cm 3 である、反射防止フィルム。 - 前記中空無機ナノ粒子全体中の30体積%以上が、前記ソリッド無機ナノ粒子全体より前記ハードコーティング層と前記低屈折層との間の界面から前記低屈折層の厚み方向により遠距離に存在する、請求項1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ティング層と前記低屈折層との間の界面により近く位置する、請求項1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0.7%以下の平均反射率を示す、請求項1に記載の反射防止フィルム。
- 前記ソリッド無機ナノ粒子及び前記中空無機ナノ粒子それぞれは、表面に(メタ)アクリレート基、エポキシド基、ビニル基(Vinyl)及びチオール基(Thiol)からなる群より選ばれた1種以上の反応性官能基を含有する、請求項1に記載の反射防止フィルム。
- 前記ソリッド無機ナノ粒子は、2.00g/cm3〜5.00g/cm3の密度を有し、
前記中空無機ナノ粒子は、1.50g/cm3〜3.50g/cm3の密度を有する、請求項1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)重合体及び光反応性官能基を含む含フッ素化合物間の架橋(共)重合体を含む、請求項1に記載の反射防止フィルム。
- 前記低屈折層は、前記光重合性化合物の(共)重合体100重量部に対して前記中空無機ナノ粒子10〜400重量部及び前記ソリッド無機ナノ粒子10〜400重量部を含む、請求項7に記載の反射防止フィルム。
- 前記光反応性官能基を含む含フッ素化合物は、それぞれ2,000〜200,000の重量平均分子量を有する、請求項7に記載の反射防止フィルム。
- 前記バインダー樹脂は、前記光重合性化合物の(共)重合体100重量部に対して前記光反応性官能基を含む含フッ素化合物を20〜300重量部含む、請求項7に記載の反射防止フィルム。
- 前記含フッ素化合物に含まれる光反応性官能基は、(メタ)アクリレート基、エポキシド基、ビニル基(Vinyl)及びチオール基(Thiol)からなる群より選ばれた1種以上である、請求項7に記載の反射防止フィルム。
- 前記光反応性官能基を含む含フッ素化合物は、i)一つ以上の光反応性官能基が置換され、少なくとも1つの炭素に1以上のフッ素が置換された脂肪族化合物または脂肪族環化合物と、ii)1以上の光反応性官能基に置換され、少なくとも1つの水素がフッ素に置換され、一つ以上の炭素がケイ素に置換されたヘテロ(hetero)脂肪族化合物またはヘテロ(hetero)脂肪族環化合物と、iii)一つ以上の光反応性官能基が置換され、少なくとも1つのシリコーンに1以上のフッ素が置換されたポリジアルキルシロキサン系高分子と、iv)1以上の光反応性官能基に置換されて少なくとも1つの水素がフッ素に置換されたポリエーテル化合物からなる群より選ばれた1種以上とを含む、請求項7に記載の反射防止フィルム。
- 前記中空無機ナノ粒子及びソリッド無機ナノ粒子それぞれの表面には、反応性官能基またはシランカップリング剤が置換される、請求項1に記載の反射防止フィルム。
- 前記反応性官能基は、アルコール、アミン、カルボン酸、エポキシド、イミド、(メタ)アクリレート、ニトリル、ノルボルネン、オレフィン、ポリエチレングリコール、チオール、シラン及びビニル基からなる群より選ばれた1種以上の官能基を含み、
前記シランカップリング剤は、ビニルクロロシラン、ビニルトリメトキシシラン、ビニルトリエトキシシラン、2−(3,4−エポキシシクロヘキシル)エチルトリメトキシシラン、3−グリシドキシプロピルトリメトキシシラン、3−グリシドキシプロピルメチルジエトキシシラン、3−グリシドキシプロピルジエトキシシラン、3−グリシドキシプロピルトリエトキシシラン、p−スチリルトリメトキシシラン、3−(メタ)アクリルオキシプロピルトリエトキシシラン、3−(メタ)アクリルオキシプロピルトリメトキシシラン、3−(メタ)アクリルオキシプロピルメチルジメトキシシラン、3−(メタ)アクリルオキシプロピルメチルジエトキシシラン、3−アクリルオキシプロピルトリメトキシシラン、N−2−(アミノエチル)−3−アミノプロピルメチルジメトキシシラン、N−2−(アミノエチル)−3−アミノプロピルトリメトキシシラン、N−2−(アミノエチル)−3−アミノプロピルメチルトリエトキシシラン、3−アミノプロピルトリメトキシシラン、3−アミノプロピルトリエトキシシラン、3−トリエトキシシリル−N−(1,3−ジメチルブチリデン)プロピルアミン、N−フェニル−3−アミノプロピルトリメトキシシラン、3−クロロプロピルトリメトキシシラン、3−メルカプトプロピルメチルジメトキシシラン、3−メルカプトプロピルトリメトキシシラン、ビス(トリエトキシシリルプロピル)テトラスルフィド及び3−イソシアネートプロピルトリエトキシシランからなる群より選ばれた1種以上を含む、請求項13に記載の反射防止フィルム。 - 前記低屈折層は、ビニル基及び(メタ)アクリレート基からなる群より選ばれた1種以上の反応性官能基を1以上含むシラン系化合物をさらに含む、請求項1に記載の反射防止フィルム。
- 前記ハードコーティング層は、光硬化性樹脂を含むバインダー樹脂と前記バインダー樹脂に分散された有機または無機微粒子を含む、請求項1に記載の反射防止フィルム。
- 前記有機または無機微粒子は、粒径が1〜10μmである、請求項16に記載の反射防止フィルム。
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CN107360718A (zh) | 2017-11-17 |
US20180231688A1 (en) | 2018-08-16 |
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EP3248776B1 (en) | 2023-06-07 |
JP2019144579A (ja) | 2019-08-29 |
JP2021076849A (ja) | 2021-05-20 |
KR102015050B1 (ko) | 2019-08-27 |
US10627548B2 (en) | 2020-04-21 |
CN107360718B (zh) | 2019-01-29 |
JP2019035991A (ja) | 2019-03-07 |
CN109988331A (zh) | 2019-07-09 |
EP3248776A1 (en) | 2017-11-29 |
US20200217991A1 (en) | 2020-07-09 |
KR101813707B1 (ko) | 2017-12-29 |
KR20170052479A (ko) | 2017-05-12 |
CN109988331B (zh) | 2020-03-27 |
US11415726B2 (en) | 2022-08-16 |
JP2018535440A (ja) | 2018-11-29 |
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