JP2018527615A - 低屈折層及びこれを含む反射防止フィルム - Google Patents
低屈折層及びこれを含む反射防止フィルム Download PDFInfo
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- JP2018527615A JP2018527615A JP2018508677A JP2018508677A JP2018527615A JP 2018527615 A JP2018527615 A JP 2018527615A JP 2018508677 A JP2018508677 A JP 2018508677A JP 2018508677 A JP2018508677 A JP 2018508677A JP 2018527615 A JP2018527615 A JP 2018527615A
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- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 1
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
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- 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
- 238000001953 recrystallisation Methods 0.000 description 1
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- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
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- 239000004408 titanium dioxide 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
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Abstract
Description
本出願は、2015年8月18日付韓国特許出願第10−2015−0116260号及び2016年8月17日付韓国特許出願第10−2016−0104409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。
0.5≧△b*=|b* 1−b* 0|
b* 0は、前記低屈折層の国際照明委員会が定めたL*a*b*色座標系のb*値であり、
b* 1は、前記低屈折層を30℃で加熱された10重量%の水酸化ナトリウム水溶液に2分間浸漬させた後、水で洗浄して水気をふいた後、55℃で加熱された10重量%の水酸化ナトリウム水溶液に30秒間浸漬させた後、水で洗浄して水気をふいて準備したフィルムに対してb* 0を測定した方法と同様に測定したL*a*b*色座標系のb*値である。
30%≧△S=[(S0−S1/S0]X100
S0は、#0000等級のスチールウールに荷重をかけて24rpmの速度で10回往復しながら低屈折層の表面を擦った時にスクラッチが発生しない最大荷重であり、S1は、前記低屈折層を30℃で加熱された10重量%の水酸化ナトリウム水溶液に2分間浸漬させた後、水で洗浄して水気をふいた後、55℃で加熱された10重量%の水酸化ナトリウム水溶液に30秒間浸漬させた後、水で洗浄して水気をふいて準備した前記フィルムに対してS0を測定した方法と同様に測定したスクラッチが発生しない最大荷重である。
製造例1:ハードコーティングフィルム1(HD1)の製造
KYOEISHA社製の塩型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#10 mayer barでコートして90℃で1分間乾燥した後、150mJ/cm2の紫外線を照射して5μmの厚さを有するハードコーティングフィルム(HD1)を製造した。
ペンタエリスリトールトリアクリレート30g、高分子量共重合体(BEAMSET 371、Arakawa社製、Epoxy Acrylate、分子量40,000)2.5g、メチルエチルケトン20g及びレベリング剤(Tego wet 270)0.5gを均一に混合した後に屈折率が1.525の微粒子としてアクリル−スチレン共重合体(体積平均粒径:2μm、製造社:Sekisui Plastic)2gを添加してハードコーティング組成物を製造した。このように得られたハードコーティング組成物をトリアセチルセルロースフィルムに#10 mayer barでコートして90℃で1分間乾燥した。前記乾燥物に150mJ/cm2の紫外線を照射して5μmの厚さを有するハードコーティングフィルム(HD2)を製造した。
窒素ガス導入管、コンデンサ(condenser)及び撹拌機を備えた1L反応器に、イソオクチルトリメトキシシラン(isooctyltrimethoxy silane)36.57g(0.156mol)、3−メタクリルオキシプロピルトリメトキシシラン(3−methacyloxypropyl trimethoxysilane)23.34g(0.094mol)及びメタノール(methanol)500mLを投入して室温で10分間撹拌した。その後、テトラメチルアンモニウムヒドロキシド(tetramethylammonium hydroxide)280g(0.77mol、25wt% in methanol)を投入して、窒素雰囲気下で反応器温度を60℃に上げて8時間反応を行った。反応完了後、カラムクロマトグラフィーと再結晶によりイソオクチル基とメタクリロキシプロピル基に置換されたpolyhedral oligomeric silsesquioxane(POSS)15gを得た。GPクロマトグラフィーで確認した結果、ポリシルセスキオキサンのシリコーンに置換されたイソオクチル基に対するメタクリロキシプロピル基のモル比(メタクリロキシプロピル基のモル数/イソオクチル基のモル数)は、約0.6〜1.67であることが確認された。
2.0Lの電子撹拌機付着ステンレス製オートクレーブを窒素ガスで十分に置換し後、酢酸エチル400g、ペルフルオロ(プロピルビニルエーテル)53.2g、エチルビニルエーテル36.1g、ヒドロキシエチルビニルエーテル44.0g、過酸化ラウロイル1.00g、下記化学式1で表示されるアゾ基含有ポリジメチルシロキサン(VPS1001(商品名)、Wako Pure Chemical Industries,Ltd.製)6.0g及び非イオン性反応性乳化剤(NE−30(商品名)、旭電化工業(株)製)20.0gを添加して、ドライアイスメタノールで−50℃まで冷却した後、再度窒素ガスで系内の酸素を除去した。
(1)低屈折層製造用光硬化性コーティング組成物の製造
下記表1の成分を混合して、MIBK(methyl isobutyl ketone)溶媒に固形分が3重量%になるように希釈した。
下記表2に記載されたハードコーティングフィルム上に、前記表1でそれぞれ得られた光硬化性コーティング組成物を#3 mayer barでコートして、60℃で1分間乾燥した。そして、窒素パージ下で前記乾燥物に180mJ/cm2の紫外線を照射して110nmの厚さを有する低屈折層を形成することによって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、次の項目の実験を行った。
30℃のNaOH水溶液(NaOHを蒸溜水に10重量%に希釈した溶液)に実施例1〜3及び比較例1〜5で得られた反射防止フィルムそれぞれを2分間浸漬してから流れる水で洗浄した後、水気をふいた。次いで、水気をふいた反射防止フィルムを再び55℃のNaOH水溶液(NaOHを蒸溜水に10重量%に希釈した溶液)に30秒間浸漬してから流れる水で洗浄した後、水気をふいた。
前記アルカリ前処理の前後時点でSolidSpec 3700(島津製作所)を用いて実施例及び比較例で製造した反射防止フィルムの平均反射率及び色座標値を測定した。
前記前処理の前後時点で、#0000等級のスチールウールに荷重をかけて24rpmの速度で10回往復して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。LED 50W天井照明下で肉眼で観察されるスクラッチが発生しない最大荷重を測定した。前記荷重は、横2cm、縦2cmの面積(2*2cm2)当たり重量(g)で定義される。
Claims (10)
- 下記式1を満たす低屈折層:
[式1]
0.5≧△b*=|b* 1−b* 0|
上記式1において、
b*0は、前記低屈折層の国際照明委員会が定めたL*a*b*色座標系のb*値であり、
b*1は、前記低屈折層を30℃で加熱された10重量%の水酸化ナトリウム水溶液に2分間浸漬させた後、水で洗浄して水気をふいた後、55℃で加熱された10重量%の水酸化ナトリウム水溶液に30秒間浸漬させた後、水で洗浄して水気をふいて準備したフィルムに対してb* 0を測定した方法と同様に測定したL*a*b*色座標系のb*値である。 - 上記式1のb* 0値が1〜−8である請求項1に記載の低屈折層。
- 上記式1のb*1値が1.5〜−8.5である請求項1に記載の低屈折層。
- 下記式2を満たす請求項1に記載の低屈折層:
[式2]
30%≧△S=[(S0−S1)/S0]X100
上記式2において、
S0は、#0000等級のスチールウールに荷重をかけて24rpmの速度で10回往復しながら低屈折層の表面を擦った時、スクラッチが発生しない最大荷重であり、
S1は、前記低屈折層を30℃で加熱された10重量%の水酸化ナトリウム水溶液に2分間浸漬させた後、水で洗浄して水気をふいた後、55℃で加熱された10重量%の水酸化ナトリウム水溶液に30秒間浸漬させた後、水で洗浄して水気をふいて準備した前記フィルムに対してS0を測定した方法と同様に測定したスクラッチが発生しない最大荷重である。 - 上記式2のS0値が250〜800gである請求項4に記載の低屈折層。
- 上記式2のS1値が200〜800gである請求項4に記載の低屈折層。
- 480〜680nmの波長領域で最小反射率を示す請求項1に記載の低屈折層。
- 380〜780nm波長領域の光に対する平均反射率が0.9〜2.5%である請求項1に記載の低屈折層。
- 光重合性化合物、反応性官能基が1以上置換されたポリシルセスキオキサン、−O−CF2CF2−O−CF3を含むフッ素系化合物、無機粒子及び光重合開始剤を含む光硬化性コーティング組成物を光硬化して得られた光硬化物を含む請求項1に記載の低屈折層。
- 請求項1の低屈折層と、前記低屈折層の一面に形成されたハードコーティング層を含む反射防止フィルム。
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR10-2015-0116260 | 2015-08-18 | ||
KR20150116260 | 2015-08-18 | ||
KR10-2016-0104409 | 2016-08-17 | ||
KR1020160104409A KR101807208B1 (ko) | 2015-08-18 | 2016-08-17 | 저굴절층 및 이를 포함하는 반사 방지 필름 |
PCT/KR2016/009111 WO2017030392A1 (ko) | 2015-08-18 | 2016-08-18 | 저굴절층 및 이를 포함하는 반사 방지 필름 |
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EP3950307A4 (en) * | 2019-03-29 | 2022-04-13 | Lg Chem, Ltd. | OPTICAL LAMINATE |
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JP2020101801A (ja) | 2020-07-02 |
JP6651609B2 (ja) | 2020-02-19 |
CN107110996A (zh) | 2017-08-29 |
KR101807208B1 (ko) | 2017-12-08 |
CN110031919A (zh) | 2019-07-19 |
KR20170137686A (ko) | 2017-12-13 |
CN107110996B (zh) | 2019-05-03 |
US20170343704A1 (en) | 2017-11-30 |
CN110031919B (zh) | 2020-12-22 |
TWI618735B (zh) | 2018-03-21 |
EP3223043A1 (en) | 2017-09-27 |
EP3223043A4 (en) | 2018-04-04 |
US11614567B2 (en) | 2023-03-28 |
KR20170021758A (ko) | 2017-02-28 |
EP3223043B1 (en) | 2020-12-16 |
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US20200333509A1 (en) | 2020-10-22 |
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