JP7240513B2 - 透明導電性フィルム - Google Patents
透明導電性フィルム Download PDFInfo
- Publication number
- JP7240513B2 JP7240513B2 JP2021545484A JP2021545484A JP7240513B2 JP 7240513 B2 JP7240513 B2 JP 7240513B2 JP 2021545484 A JP2021545484 A JP 2021545484A JP 2021545484 A JP2021545484 A JP 2021545484A JP 7240513 B2 JP7240513 B2 JP 7240513B2
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- Prior art keywords
- light
- conductive layer
- film
- layer
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Images
Classifications
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- 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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- 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
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- 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
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- 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
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C—CHEMISTRY; METALLURGY
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- 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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
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- G—PHYSICS
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- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
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- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1343—Electrodes
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
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Description
透明な樹脂フィルム(基材)としての長尺のシクロオレフィンポリマー(COP)フィルム(商品名「ゼオノア」,厚さ40μm,ゼオン社製)の一方の面に、アクリル樹脂を含有する紫外線硬化性樹脂組成物を塗布して塗膜を形成した。次に、紫外線照射によって当該塗膜を硬化させてハードコート層(厚さ1μm)を形成した。次に、ハードコート層上に、屈折率調整層形成用の紫外線硬化性樹脂組成物(ジルコニア粒子含有の複合樹脂組成物)を塗布して塗膜を形成した。次に、紫外線照射によって当該塗膜を硬化させて、ハードコート層上に屈折率調整層(厚さ90nm,屈折率1.62)を形成した。このようにして、樹脂フィルムと、ハードコート層と、屈折率調整層とをこの順で備える透明基材を作製した(透明基材作製工程)。
以下のこと以外は、実施例1の透明導電性フィルムと同様にして、実施例2および比較例1の各透明導電性フィルムを作製した。
成膜工程において、形成される光透過性導電層の厚さを43nmに代えて41nm(実施例2)としたこと以外は、実施例1の透明導電性フィルムと同様にして、実施例3の透明導電性フィルムを作製した。実施例3の透明導電性フィルムの光透過性導電層(非晶質)は、単一のKr含有ITO層からなる。
以下のこと以外は、実施例1の透明導電性フィルムと同様にして、比較例2~4の各透明導電性フィルムを作製した。
以下のこと以外は、実施例1の透明導電性フィルムと同様にして、比較例5の透明導電性フィルムを作製した。
実施例1~3および比較例1~5の各透明導電性フィルムにおける光透過性導電層の厚さを、FE-TEM観察により測定した。具体的には、まず、FIBマイクロサンプリング法により、実施例1~3および比較例1~5における各光透過性導電層の断面観察用サンプルを作製した。FIBマイクロサンプリング法では、FIB装置(商品名「FB2200」,Hitachi製)を使用し、加速電圧を10kVとした。次に、断面観察用サンプルにおける光透過性導電層の厚さを、FE-TEM観察によって測定した。FE-TEM観察では、FE-TEM装置(商品名「JEM-2800」,JEOL製)を使用し、加速電圧を200kVとした。
実施例1~3および比較例1~5の各透明導電性フィルムについて、光透過性導電層のホール移動度およびキャリア密度を測定した。本測定には、ホール効果測定システム(商品名「HL5500PC」,バイオラッド社製)を使用した。本測定により得られたホール移動度(cm2/V・s)およびキャリア密度(cm-3)の値を表1に示す。
実施例1~3および比較例1~5の各透明導電性フィルムについて、加熱処理後の光透過性導電層の比抵抗を調べた。加熱処理では、加熱手段として熱風オーブンを使用し、加熱温度を130℃とし、加熱時間を90分とした。JIS K 7194(1994年)に準拠した四端子法により、光透過性導電層の表面抵抗を測定した後、表面抵抗値と光透過性導電層の厚さとを乗じることにより、光透過性導電層の比抵抗(Ω・cm)を求めた(比較例1における光透過性導電層は、上記加熱処理によっては結晶化しなかったので、同層の比抵抗は測定できなかった)。その結果を表1に示す。
実施例1~3および比較例1~5の各透明導電性フィルムについて、光透過性導電層の結晶化速度を調べた。具体的には、まず、各透明導電性フィルムについて、2種類のサンプル(第1サンプル,第2サンプル)を用意した。第1サンプルは、透明導電性フィルムを、140℃で30分間、加熱処理することによって用意した。第2サンプルは、透明導電性フィルムを、140℃で60分間、加熱処理することによって用意した。次に、サンプルを、濃度5質量%の塩酸に、35℃で15分間、浸漬した。次に、サンプルを、水洗した後、乾燥した。次に、サンプルの光透過性導電層の露出平面において、離隔距離15mmの一対の端子の間の抵抗(端子間抵抗)を測定した。この測定において、端子間抵抗が10kΩ以下である場合、光透過性導電層の結晶化が完了していると判断した。
実施例1~3および比較例1~5の各透明導電性フィルムについて、非晶質の光透過性導電層の保存性(保存時における結晶化抑制の程度)を調べた。具体的には、まず、各透明導電性フィルムについて、2種類のサンプル(第3サンプル,第4サンプル)を用意した。第3サンプルは、透明導電性フィルムを、50℃で15時間、静置することによって用意した。第4サンプルは、透明導電性フィルムを、80℃で6時間、静置することによって用意した。次に、熱風オーブン内でサンプルを加熱処理した(光透過性導電層の結晶化)。加熱温度は130℃とし、加熱時間は90分間とした。次に、サンプルにおける光透過性導電層の表面を光学顕微鏡で観察し、クラックの有無を確認した(倍率100倍,観察範囲は2cm×2cm)。
実施例1~3および比較例1における各光透過性導電層がKr原子を含有することは、次のようにして確認した。まず、走査型蛍光X線分析装置(商品名「ZSX PrimusIV」,リガク社製)を使用して、下記の測定条件にて蛍光X線分析測定を5回繰り返し、各走査角度の平均値を算出し、X線スペクトルを作成した。作成されたX線スペクトルにおいて、走査角度28.2°近傍にピークが出ていることを確認することにより、光透過性導電層にKr原子が含有されることを確認した。
スペクトル;Kr-KA
測定径:30mm
雰囲気:真空
ターゲット:Rh
管電圧:50kV
管電流:60mA
1次フィルタ:Ni40
走査角度(deg):27.0~29.5
ステップ(deg):0.020
速度(deg/分):0.75
アッテネータ:1/1
スリット:S2
分光結晶:LiF(200)
検出器:SC
PHA:100-300
実施例1~3の各透明導電性フィルムでは、光透過性導電層がKrを含有し、且つ、当該光透過性導電層におけるキャリア密度が40×1019cm-3以上である。このような実施例1~3の各透明導電性フィルムでは、光透過性導電層において、高い結晶化速度が実現され、且つ良好な保存性が確保された。これに対し、比較例1の透明導電性フィルム(光透過性導電層のキャリア密度が40×1019cm-3未満である)、比較例2,3の各透明導電性フィルム(光透過性導電層がKrを含有せず、且つ同層のキャリア密度が40×1019cm-3以上である)、および、比較例4,5の各透明導電性フィルム(光透過性導電層がKrを含有せず、且つ同層のキャリア密度が40×1019cm-3未満である)では、高い結晶化速度と良好な保存性とを両立できなかった。
D 厚さ方向
10 透明基材
11 樹脂フィルム
12 機能層
20 光透過性導電層
Claims (4)
- 透明基材と非晶質の光透過性導電層とを厚さ方向にこの順で備え、
前記光透過性導電層が、クリプトンを含有し、40×1019cm-3以上100×10 19 cm -3 以下のキャリア密度を有し、且つ18cm 2 /V・s以下のホール移動度を有する、透明導電性フィルム。 - 前記光透過性導電層が、インジウム含有導電性酸化物を含む、請求項1に記載の透明導電性フィルム。
- 前記光透過性導電層が、30nm以上の厚さを有する、請求項1または2に記載の透明導電性フィルム。
- 前記光透過性導電層が、130℃で1.5時間の加熱処理後に2.2×10-4Ω・cm以下の比抵抗を有する、請求項1から3のいずれか一つに記載の透明導電性フィルム。
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