JP2023010726A - 防汚層付き光学フィルム - Google Patents
防汚層付き光学フィルム Download PDFInfo
- Publication number
- JP2023010726A JP2023010726A JP2022172169A JP2022172169A JP2023010726A JP 2023010726 A JP2023010726 A JP 2023010726A JP 2022172169 A JP2022172169 A JP 2022172169A JP 2022172169 A JP2022172169 A JP 2022172169A JP 2023010726 A JP2023010726 A JP 2023010726A
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- Prior art keywords
- layer
- antifouling layer
- antifouling
- film
- optical film
- Prior art date
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Images
Classifications
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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
- G02B1/18—Coatings for keeping optical surfaces clean, e.g. hydrophobic or photo-catalytic films
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
- B32B7/023—Optical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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Abstract
Description
反応性スパッタリングでは、ターゲットとして金属ターゲットを用い、上述のガスとして、アルゴンなどの不活性ガスと酸素(反応性ガス)との混合ガスを用いる。不活性ガスと酸素との流量比(sccm)の調整により、成膜される無機酸化物に含まれる酸素の割合を調整できる。
まず、透明な樹脂フィルムとしての長尺のトリアセチルセルロース(TAC)フィルム(厚さ80μm)の片面に、ハードコート層を形成した(ハードコート層形成工程)。本工程では、まず、紫外線硬化型のアクリルモノマー(商品名「GRANDIC PC-1070」,DIC社製)100質量部と、ナノシリカ粒子を含有するオルガノシリカゾル(商品名「MEK-ST-L」,ナノシリカ粒子の平均一次粒子径は50nm,固形分濃度30質量%,日産化学社製)25質量部(ナノシリカ粒子換算量)と、チキソトロピー付与剤(商品名「ルーセンタイトSAN」,有機粘土である合成スメクタイト,コープケミカル社製)1.5質量部と、光重合開始剤(商品名「OMNIRAD907」,BASF社製)3質量部と、レベリング剤(商品名「LE303」,共栄社化学社製)0.15質量部とを混合して、固形分濃度55質量%の組成物(ワニス)を調製した。混合には、超音波分散機を使用した。次に、上記TACフィルムの片面に組成物を塗布して塗膜を形成した。次に、この塗膜を、紫外線照射により硬化させた後、加熱により乾燥させた。紫外線照射では、光源として高圧水銀ランプを使用し、波長365nmの紫外線を用い、積算照射光量を200mJ/cm2とした。また、加熱の時間は80℃とし、加熱の温度は3分間とした。これにより、TACフィルム上に厚さ6μmのハードコート(HC)層を形成した。
次のこと以外は、実施例1の光学フィルムと同様にして、実施例2の光学フィルムを作製した。下地層前処理工程を実施しなかった(即ち、下地層前処理としてのプラズマ処理の放電電力は0Wとした)。防汚層形成工程(真空蒸着)において、蒸着源として、信越化学社製の「KY1903-1」(パーフルオロポリエーテル基含有アルコキシシラン化合物)を乾燥して得た固形分を用いた。
下地層前処理工程後であって防汚層形成工程前に、ワークフィルムを一旦 ロール状に巻き取ったこと以外は、実施例1の光学フィルムと同様にして、比較例1の光学フィルムを作製した。
防汚層形成工程以外は、実施例1の光学フィルムと同様にして、比較例2の光学フィルムを作製した。本比較例の防汚層形成工程では、ウェットコーティング法によって防汚層を形成した。具体的には、まず、コーティング剤としての「オプツール UD509」(ダイキン工業社製)を、希釈溶媒(商品名「フロリナート」,3M社製)で希釈して、固形分濃度0.1質量%のコーティング液を調製した。次に、スパッタ成膜工程で形成された反射防止層の上に、コーティング液をグラビアコーティングによって塗布して塗膜を形成した。次に、この塗膜を、60℃で2分間の加熱によって乾燥させた。これにより、反射防止層上に厚さ7nmの防汚層を形成した。
実施例1,2および比較例1,2の各光学フィルムの防汚層表面を、X線光電子分光法(ESCA)によって分析した。分析用の試料は、光学フィルムから10mm×10mm程度のサイズに切り出して用意した。分析には、X線光電子分光装置(商品名「Quantum 2000」,アルバック・ファイ社製)を使用した。本分析では、下記の条件でX線光電子分光測定を行った。
X-ray Settinng:200μmφ(15kV,30W)
光電子取り出し角:試料表面に対して5度、15度、30度、45度
実施例1,2および比較例1,2の各光学フィルムについて、防汚層表面の水接触角を調べた。まず、光学フィルムの防汚層表面に、約1μLの純水の滴下によって水滴を形成した。次に、防汚層表面上の水滴の表面と防汚層表面とがなす角度を測定した。測定には、接触角計(商品名「DMo-501」,協和界面科学社製)を使用した。その測定結果を、初期の水接触角θ0として表1に示す。
実施例1,2および比較例1,2の各光学フィルムについて、消しゴム摺動試験を経ることによる防汚層表面の防汚性低下の程度を調べた。具体的には、まず、光学フィルムの防汚層表面に対して消しゴムを摺動させつつ往復動させる摺動試験を実施した。この試験では、Minoan社製の消しゴム(Φ6mm)を使用し、防汚層表面に対する消しゴムの荷重を1kg/6mmΦとし、防汚層表面上の消しゴムの摺動距離(往復動における片道)を20mmとし、消しゴムの摺動速度を40rpmとし、防汚層表面に対して消しゴムを往復動させる回数は3000往復とした。次に、光学フィルムの防汚層表面における消しゴム摺動箇所の水接触角を、初期の水接触角θ0の測定方法と同様の方法で測定した。その測定結果を、消しゴム摺動試験後の水接触角θ1として、表1に示す。
実施例1,2の光学フィルムでは、比較例1,2の各光学フィルムと比較して、消しゴム摺動試験を経ることによる防汚層表面における水接触角の低下の程度が有意に小さく、従って、防汚性の低下が有意に小さい(防汚層表面では、水接触角の低下が小さいほど、防汚性の低下は小さい)。
10 透明基材
11 樹脂フィルム
12 ハードコート層
20 光学機能層
21 第1高屈折率層
22 第1低屈折率層
23 第2高屈折率層
24 第2低屈折率層
30 防汚層
31 表面
41 密着層
42 無機酸化物下地層
T 厚さ方向
Claims (7)
- 透明基材と防汚層とを厚さ方向に順に備え、
前記防汚層における前記透明基材とは反対の表面側の、X線光電子分光法での元素分析によって検出されるSiに対するFの比率が、分析深さ1nmでは20以上である、防汚層付き光学フィルム。 - 前記防汚層における前記比率が、分析深さ1nmから分析深さ5nmにかけて単調減少する、請求項1に記載の防汚層付き光学フィルム。
- 前記防汚層が、パーフルオロポリエーテル基を有するアルコキシシラン化合物を含有する、請求項1に記載の防汚層付き光学フィルム。
- 前記防汚層がドライコーティング膜である、請求項1に記載の防汚層付き光学フィルム。
- 前記透明基材と前記防汚層との間に無機酸化物下地層を備え、当該無機酸化物下地層上に前記防汚層が配置されている、請求項1に記載の防汚層付き光学フィルム。
- 前記無機酸化物下地層が二酸化ケイ素を含む、請求項5に記載の防汚層付き光学フィルム。
- 前記無機酸化物下地層における前記防汚層側の表面が、0.5nm以上10nm以下の表面粗さRaを有する、請求項5または6に記載の防汚層付き光学フィルム。
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