JP7068558B2 - 透明導電性フィルム - Google Patents
透明導電性フィルム Download PDFInfo
- Publication number
- JP7068558B2 JP7068558B2 JP2021545854A JP2021545854A JP7068558B2 JP 7068558 B2 JP7068558 B2 JP 7068558B2 JP 2021545854 A JP2021545854 A JP 2021545854A JP 2021545854 A JP2021545854 A JP 2021545854A JP 7068558 B2 JP7068558 B2 JP 7068558B2
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- JP
- Japan
- Prior art keywords
- light
- conductive layer
- transmitting conductive
- film
- transparent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
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Images
Classifications
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
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- C23C14/20—Metallic material, boron or silicon on organic substrates
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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
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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
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- G—PHYSICS
- G02—OPTICS
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Description
樹脂フィルムとしての長尺のPETフィルム(厚さ50μm,東レ社製)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2μm)を形成した。このようにして、樹脂フィルムと機能層としてのハードコート層とを備える透明樹脂基材を作製した(この透明基材について165℃で1時間の加熱処理を実施した後の、最も収縮する方向における同透明基材の熱収縮率(最大熱収縮率,本実施例ではMD方向の熱収縮率)は、0.63%である)。
成膜工程における成膜条件の一部を変更したこと、および、結晶化工程の加熱条件を変更したこと以外は、実施例1の透明導電性フィルムと同様にして、実施例2の透明導電性フィルムを作製した。本実施例における成膜工程では、成膜室内の気圧を0.4Paとし、形成される光透過性導電層の厚さを160nmとした。本実施例における結晶化工程では、加熱温度を155℃とし、加熱時間を2時間とした。
成膜工程において、透明樹脂基材上に光透過性導電層の第1領域(厚さ50nm)を形成する第1スパッタ成膜と、当該第1領域上に光透過性導電層の第2領域(厚さ80nm)を形成する第2スパッタ成膜とを順次に実施したこと以外は、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。
成膜工程で形成される光透過性導電層について、第1領域の厚さを50nmから66nm(実施例4)、85nm(実施例5)、または87nm(実施例6)としたこと、および、第2領域の厚さを80nmから64nm(実施例4)、45nm(実施例5)、または38nm(実施例6)としたこと以外は、実施例3の透明導電性フィルムと同様にして、実施例4~6の各透明導電性フィルムを作製した。
スパッタ成膜における次のこと以外は、実施例1の透明導電性フィルムと同様にして、実施例7の透明導電性フィルムを作製した。スパッタリングガスとしてクリプトンとアルゴンとの混合ガス(Kr90体積%,Ar10体積%)を用いた。成膜室内の気圧を0.2Paとした。成膜室に導入される混合ガスおよび酸素の合計導入量に対する酸素導入量の割合を約2.7流量%とし、その酸素導入量は、形成される膜の比抵抗の値が5.7×10-4Ω・cmになるように調整した。
成膜工程において、スパッタリングガスとしてKrに代えてArを用いたこと、および、成膜圧力を0.2Paに代えて0.4Pa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、比較例1の透明導電性フィルムを作製した。比較例1の透明導電性フィルムの光透過性導電層(厚さ130nm,結晶質)は、単一のAr含有ITO層からなる。
成膜工程において、スパッタリングガスとしてKrに代えてArを用い、且つ成膜圧力を0.2Paに代えて0.4Paとしたこと、および、結晶化工程において、165℃で1時間の加熱処理に代えて、170℃で5分間の第1加熱処理と、その後の165℃で1時間の第2加熱処理とを実施したこと以外は、実施例2の透明導電性フィルムと同様にして、比較例2の透明導電性フィルムを作製した。比較例2の透明導電性フィルムの光透過性導電層(厚さ160nm,結晶質)は、単一のAr含有ITO層からなる。
実施例1~7および比較例1,2における各透明導電性フィルムの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1~7および比較例1,2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1~7および比較例1,2の各透明導電性フィルムについて、光透過性導電層の比抵抗を調べた。具体的には、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、比抵抗(Ω・cm)を求めた。その結果を表1に掲げる。
実施例1~7および比較例1,2の各透明導電性フィルムの光透過性導電層に含有されるKrおよびAr原子の含有量を、ラザフォード後方散乱分光法(RBS)によって分析した。検出元素である、In+Sn(ラザフォード後方散乱分光法では、InとSnを分離しての測定が困難であるため、2元素の合算として評価した)、O、Ar、Krの5元素に関して、元素比率を求めることにより、光透過性導電層におけるKr原子およびAr原子の存在量(原子%)を求めた。使用装置および測定条件は、下記のとおりである。分析結果として、Kr含有量(原子%)、Ar含有量(原子%)、および希ガス原子含有量(原子%)を表1に掲げる。Kr含有量の分析に関し、実施例1~7では、検出限界値(下限値)以上の確かな測定値が得られなかった(検出限界値は、測定に付される光透過性導電層の厚さによって異なりうる)。そのため、表1では、光透過性導電層のKr含有量について、同層の厚さにおける検出限界値を下回っていることを示すため、「< 測定に付された光透過性導電層の厚さにおける具体的な検出限界値」と表記する(希ガス原子含有量の表記の仕方についても同様である)。
Pelletron 3SDH(National Electrostatics Corporation製)
<測定条件>
入射イオン:4He++
入射エネルギー:2300keV
入射角:0deg
散乱角:160deg
試料電流:6nA
ビーム径:2mmφ
面内回転:無
照射量:75μC
実施例1~7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。そして、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1~7および比較例1,2の各透明導電性フィルムの光透過性導電層(結晶質ITO膜)の圧縮残留応力を、光透過性導電層の結晶格子歪みから間接的に求めた。具体的には、次のとおりである。
実施例1~7および比較例1,2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安定性を調べた。具体的には、まず、JIS K 7194(1994年)に準拠した四端子法により、透明導電性フィルムの光透過性導電層の第1表面抵抗R1(加熱処理前の表面抵抗)を測定した。次に、透明導電性フィルムを加熱処理した。加熱処理において、加熱温度は175℃であり、加熱時間は1時間である。次に、JIS K 7194(1994年)に準拠した四端子法により、透明導電性フィルムの光透過性導電層の第2表面抵抗R2(加熱処理後の表面抵抗)を測定した。そして、第1表面抵抗R1に対する第2表面抵抗R2の比率(R2/R1)を求めた。その値を表1に掲げる。R2/R1の値が1に近いほど、加熱処理による光透過性導電層の抵抗値変化が少ないことを示し、従って、同層の結晶安定性が高いことを示す。
D 厚さ方向
10 透明樹脂基材
11 樹脂フィルム
12 機能層
20 光透過性導電層
21 第1領域
22 第2領域
Claims (5)
- 透明樹脂基材と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結晶質膜であり、
前記光透過性導電層が、前記厚さ方向と直交する面内第1方向において第1圧縮残留応力を有し、且つ、前記厚さ方向および前記面内第1方向のそれぞれと直交する面内第2方向において、前記第1圧縮残留応力より小さな第2圧縮残留応力を有し、
前記第1圧縮残留応力に対する前記第2圧縮残留応力の比率が、0.82以下である、透明導電性フィルム。 - 前記光透過性導電層がクリプトンを含有することを特徴とする、請求項1に記載の透明導電性フィルム。
- 前記透明樹脂基材が、ガラス基材とは隣接しないことを特徴とする、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、2.2×10-4Ω・cm未満の比抵抗を有することを特徴とする、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。
- 前記光透過性導電層が、100nm以上の厚さを有することを特徴とする、請求項1から4のいずれか一つに記載の透明導電性フィルム。
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