JP7026997B2 - シリカ層の製造方法 - Google Patents
シリカ層の製造方法 Download PDFInfo
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Description
RnSiO(4-n)/2
SiO3/2L1/2
SiR1(4-n)(OR2)n
スチールウール抵抗度は、下記形成されたシリカ層を25℃の温度および50%の相対湿度に維持した状態でスチールウールを擦って評価した。前記評価過程で肉眼でスクラッチなどの欠陥が観察される時まで荷重を段階的に増加させながら評価を進行させ、その荷重を評価結果で記載した。前記でスチールウールとしてはヨーロッパのBriwax社で販売する等級#0000のスチールウールを利用した。
反射率は形成されたシリカ層をPET(ポリ(エチレンテレフタレート);poly(ethylene terephthalate))フィルム上に合紙した後に25℃の温度および50%の相対湿度で測定装備(分光光度計;spectrophotometer、コニカ-ミノルタ社、CM-2600D)を使って550nm波長の光を基準として評価した。
TEOS(テトラエトキシシラン;tetraethoxy silane)を溶媒であるエタノール(EtOH)と混合し、10分程度撹はんした。引き続き前記混合物に蒸溜水(H2O)および塩酸(HCl)を混合した触媒溶液を略5分にかけてゆっくり滴下して撹はんした。前記滴下後に別途の冷却や恒温維持なしに略18時間の間さらに撹はんした。撹はん後にpHは略2~5の水準であった。前記で混合された成分の比率は略36.14:92.14:104.17:3.65(重量比率:蒸溜水:TEOS:エタノール:塩酸)程度であった。
下記の表1のように界面活性剤の種類および比率を制御したことを除いては実施例1と同様にしてシリカ層を製造したし、その結果も下記の表1に整理した。
下記の表1のように界面活性剤の種類および比率とシリカ層の厚さおよび界面活性剤の洗浄条件を制御したことを除いては実施例1と同様にしてシリカ層を製造し、その結果も下記の表2に整理した。
Claims (13)
- シリカ前駆体、酸触媒および界面活性剤を含む前駆体組成物で形成された前駆体層をゲル化させる段階を含み、
前記ゲル化は前記前駆体層をpKaが8以下であるアミン化合物と接触させて遂行するか、又は、
前記前駆体組成物は潜在性塩基発生剤をさらに含み、前記ゲル化は前記潜在性塩基発生剤から塩基を発生させて遂行する、シリカ層の製造方法。 - 前記シリカ前駆体は下記の化学式DまたはEのシラン化合物、前記シラン化合物の加水分解物または前記シラン化合物の縮合反応物である、請求項1に記載のシリカ層の製造方法:
[化学式D]
SiR1(4-n)(OR2)n
前記化学式DでR1は、水素、アルキル基、アルケニル基、アリール基、アリールアルキル基、エポキシ基または(メタ)アクリロイルオキシアルキル基であり、R2は炭素数1~4のアルキル基、炭素数6~12のアリール基または水素原子であり、nは3または4である:
- 前記前駆体組成物はシリカ前駆体を5~60重量%の範囲内の割合で含む、請求項1又は2に記載のシリカ層の製造方法。
- 前記前駆体組成物は溶媒をさらに含む、請求項1~3のいずれか一項に記載のシリカ層の製造方法。
- 前記溶媒は水性溶媒と有機溶媒の混合溶媒である、請求項4に記載のシリカ層の製造方法。
- 前記界面活性剤は前記前駆体層または前記前駆体組成物内でミセルを形成している、請求項1~5のいずれか一項に記載のシリカ層の製造方法。
- 前記前駆体組成物は溶媒をさらに含み、前記界面活性剤の濃度は前記溶媒に対する臨界ミセル濃度の1倍~5倍の範囲となるように調節されている、請求項1~3のいずれか一項に記載のシリカ層の製造方法。
- 前記界面活性剤は陽イオン性界面活性剤、陰イオン性界面活性剤または非イオン性界面活性剤である、請求項1~7のいずれか一項に記載のシリカ層の製造方法。
- 前記潜在性塩基発生剤は、下記の化学式11で表示される化合物;下記の化学式13~15のうちいずれか一つで表示される陽イオン化合物を有するイオン化合物または下記の化学式18の化合物に含まれているか、それから由来したものである、請求項1~8のいずれか一項に記載のシリカ層の製造方法:
- 前記ゲル化工程後に前記界面活性剤を除去する工程を追加で遂行する、請求項1~9のいずれか一項に記載のシリカ層の製造方法。
- 前記界面活性剤の除去はアルコール溶媒、ケトン溶媒またはアセテート溶媒を使って遂行する、請求項10に記載のシリカ層の製造方法。
- 前記前駆体層のゲル化は基材上で進行される、請求項1~11のいずれか一項に記載のシリカ層の製造方法。
- 前記基材は、高屈折層、ハードコーティング層および反射防止層からなる群から選択されたいずれか一つの機能性層;偏光フィルム、偏光フィルムの保護フィルム、輝度向上フィルム、位相差フィルム、ディスプレイパネルまたはタッチパネルである、請求項12に記載のシリカ層の製造方法。
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KR1020170178519A KR102267504B1 (ko) | 2017-12-22 | 2017-12-22 | 메조포러스 실리카 코팅층을 포함하는 광학 부재의 제조방법 및 이를 이용하여 제조된 광학 부재 |
PCT/KR2018/016447 WO2019125040A1 (ko) | 2017-12-22 | 2018-12-21 | 실리카층의 제조 방법 |
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JP2006093657A (ja) | 2004-07-09 | 2006-04-06 | Jsr Corp | 有機シリカ系膜およびその形成方法、半導体装置の絶縁膜形成用組成物、ならびに配線構造体および半導体装置 |
JP2008509800A (ja) | 2004-08-03 | 2008-04-03 | エシロール アテルナジオナール カンパニー ジェネラーレ デ オプティック | メソポーラス層を被覆した基材の生産方法およびその眼科用光学部品への利用 |
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CN1219700C (zh) * | 1998-12-23 | 2005-09-21 | 贝特勒纪念学院 | 由含表面活性剂的溶液制备的中孔二氧化硅膜及其制备方法 |
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EP3730223A1 (en) | 2020-10-28 |
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