JP2014157816A - 透明導電フィルムの製造方法 - Google Patents
透明導電フィルムの製造方法 Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
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- 229910000449 hafnium oxide Inorganic materials 0.000 description 1
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- 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
- C23C14/34—Sputtering
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- C23C14/354—Introduction of auxiliary energy into the plasma
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- H01J37/32—Gas-filled discharge tubes
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Abstract
【解決手段】有機高分子フィルム基材1の少なくとも一方の面に、ロール‐トゥ‐ロールの装置により、{4価金属元素の酸化物/(4価金属元素の酸化物+酸化インジウム)}×100(%)で表される4価金属元素の酸化物の割合が7〜15重量%であるインジウム系複合酸化物のターゲットを用いて、当該ターゲット表面での水平磁場が85〜200mTの高磁場で、不活性ガスの存在下に、RF重畳DCスパッタ成膜法により、透明導電膜2を形成する工程(A)を有し、かつ、前記透明導電膜は、前記インジウム系複合酸化物の結晶質膜であり、前記透明導電膜は、膜厚が10nm〜40nmの範囲であり、前記透明導電膜は、比抵抗値が1.3×10−4〜2.8×10−4Ω・cmである。
【選択図】図1
Description
有機高分子フィルム基材の少なくとも一方の面に、
ロール‐トゥ‐ロールの装置により、
{4価金属元素の酸化物/(4価金属元素の酸化物+酸化インジウム)}×100(%)で表される4価金属元素の酸化物の割合が7〜15重量%であるインジウム系複合酸化物のターゲットを用いて、当該ターゲット表面での水平磁場が85〜200mTの高磁場で、不活性ガスの存在下に、RF重畳DCスパッタ成膜法により、透明導電膜を形成する工程(A)を有し、
かつ、前記透明導電膜は、前記インジウム系複合酸化物の結晶質膜であり、
前記透明導電膜は、膜厚が10nm〜40nmの範囲であり、
前記透明導電膜は、比抵抗値が1.3×10−4〜2.8×10−4Ω・cmであることを特徴とする透明導電性フィルムの製造方法、に関する。
(有機高分子フィルム基材)
有機高分子フィルム基材として、三菱樹脂(株)製のO300E(厚み125μm)のポリエチレンテレフタレート(PET)フィルムを用いた。
上記PETフィルムの易滑処理面でない、平滑面上へ、ITO薄膜を成膜できるように、上記PETフィルムを、R−to―Rのスパッタ成膜装置へ装着した。120℃に加熱したロール電極を使用し、巻取りながら、クライオコイルとターボポンプの排気系で脱ガス処理を行い、成膜なしでの走行中の真空度が3×10−5Paの雰囲気を得た。その後、スパッタ成膜装置にアルゴンガスを導入し、上記PETフィルムを、RF電源(13.56MHz)によるプラズマ放電中を通して、PET表面の前処理を行った。
上記PETフィルムのプラズマ処理面へ、Al金属ターゲットから反応性デュアルマグネトロンスパッタ法にて、厚み20nmのAl2O3薄膜を成膜した。
その後、真空を維持して、高磁場RF重畳DCスパッタ成膜装置の電極上に、予めセットしてあった、ITO酸化物ターゲット(住友金属鉱山社製,スズ酸化物の割合が10重量%)を1.1W/cm2のDC電力密度、RF電力(13.56MHz)/DC電力の電力比が0.6の条件でプリスパッタを行った。ターゲット表面の水平磁場は100mTとした。フィルム基材は低速で巻取りながら、インラインのモニターで表面抵抗値および透過率を測定しながら行った。その他の条件は、フィルム基材の温度は150℃、導入ガスはアルゴンガスのみを用いた。プリスタッタの気圧は0.32Paで行った。インラインの抵抗値が安定状態になるまで行った。
プリスパッタと同様のITOターゲットを用いて、上記同様の高磁場RF重畳DCスパッタ成膜装置により、1.1W/cm2のDC電力密度、RF電力(13.56MHz)/DC電力の電力比が1の条件で本スパッタを行って、膜厚28nmのITO膜を成膜した。ターゲット表面の水平磁場は100mTとした。フィルム基材の温度は150℃とし、導入ガスはアルゴンガスのみを用いた。本スパッタの成膜気圧は0.32Paとした。
上記ITO膜を形成したPETフィルムについて、大気中において、150℃で1時間の熱処理を行い、透明導電性フィルムを得た。
実施例1において、表1に示すように、ITOターゲットのスズ酸化物(SnO2)の割合、高磁場RF重畳DCスパッタ成膜における、RF電源の周波数、RF電力/DC電力の電力比、酸素導入量、アニール処理工程の温度を表1に示すように変えたこと以外は実施例1と同様にして透明導電性フィルムを得た。
実施例および比較例で得られた透明導電性フィルムについて下記の評価を行なった。結果を表1に示す。
透明導電性フィルムのITO膜の表面抵抗値を、三菱油化(株)社製ロレスタGP(形式MCP−T600)を用いて測定した。
ITO膜の結晶状態の確認は、透明導電性フィルムから、剥離法によりITO膜のみサンプリングし、透過型電子顕微鏡TEM(日立、HF2000)にて、加速電圧200kVで観察を行った。図12は、本発明の実施例5で得られたITOフィルムの結晶を示すTEM写真である。
ITO膜の膜厚測定は、サンプルを樹脂で固定したものを、Hitachi,FB−2100にて超薄膜切片として切り出し、該記のTEMにて観察し測定した。
斜入射X線回折測定は以下の装置を用いて測定し、(222)面と(440)面からのピーク強度比を求めた。図11は、本発明の実施例1で得られたITOフィルムのX線回折チャートである。
(株)リガク製 粉末X線回折装置RINT−2000
光源 Cu−Kα線(波長:1.541Å)、40KV、40mA
光学系 並行ビーム光学系
発散スリット:0.05mm
受光スリット:0.05mm
単色化・並行化 多層ベーベルミラー使用
1A・・基板ホルダーまたはキャンロール
2・・・透明導電膜
2A・・インジウム系複合酸化物ターゲット
3・・・スパッタ電極
4・・・高磁場発生する磁石
5・・・高周波導入用マッチングボックス
6・・・ローパスフィルター
7・・・高周波電源(RF電源)
8・・・直流電源(DC電源)
Claims (12)
- 有機高分子フィルム基材上の少なくとも一方の面に透明導電膜を有する透明導電性フィルムの製造方法であって、
有機高分子フィルム基材の少なくとも一方の面に、
ロール‐トゥ‐ロールの装置により、
{4価金属元素の酸化物/(4価金属元素の酸化物+酸化インジウム)}×100(%)で表される4価金属元素の酸化物の割合が7〜15重量%であるインジウム系複合酸化物のターゲットを用いて、当該ターゲット表面での水平磁場が85〜200mTの高磁場で、不活性ガスの存在下に、RF重畳DCスパッタ成膜法により、透明導電膜を形成する工程(A)を有し、
かつ、前記透明導電膜は前記透明導電膜は、膜厚が10nm〜40nmの範囲であり、
前記透明導電膜は、比抵抗値が1.3×10−4〜2.8×10−4Ω・cmであることを特徴とする透明導電性フィルムの製造方法。 - 前記透明導電膜は、フィルム基材の側からアンダーコート層を介して設けられていることを特徴とする請求項1記載の透明導電性フィルムの製造方法。
- 前記インジウム系複合酸化物がインジウム・スズ複合酸化物であり、4価金属元素の酸化物がスズ酸化物であることを特徴とする請求項1または2記載の透明導電性フィルムの製造方法。
- 前記形成工程(A)に係る高磁場RF重畳DCスパッタ成膜法は、
RF電源の周波数が10〜20MHzの時、RF電力/DC電力の電力比が0.4〜1.2であることを特徴とする請求項1〜3のいずれかに記載の透明導電性フィルムの製造方法。 - 前記形成工程(A)に係る高磁場RF重畳DCスパッタ成膜法は、
RF電源の周波数が20MHzより大きく60MHz以下の時、RF電力/DC電力の電力比が0.2〜0.6であることを特徴とする請求項1〜3のいずれかに記載の透明導電フィルムの製造方法。 - 前記形成工程(A)に係る高磁場RF重畳DCスパッタ成膜法は、
有機高分子フィルム基材の温度が、80〜180℃であることを特徴とする請求項1〜5のいずれかに記載の透明導電フィルムの製造方法。 - 前記形成工程(A)に係る高磁場RF重畳DCスパッタ成膜法は、酸素を導入することなく行うことを特徴とする請求項1〜6のいずれかに記載の透明導電フィルムの製造方法。
- 前記形成工程(A)に係る高磁場RF重畳DCスパッタ成膜法は、不活性ガス量に対して、酸素量の割合が0.5%以下になるように、酸素を導入しながら行うことを特徴とする請求項1〜6のいずれかに記載の透明導電フィルムの製造方法。
- 請求項1〜8のいずれかに記載の透明導電フィルムの製造方法であって、
前記高磁場RF重畳DCスパッタ成膜法を施す前に、酸素を導入することなく、不活性ガスの存在下に、RF重畳DCスパッタ成膜法により、RF電源の周波数が10〜20MHzの時、RF電力/DC電力の電力比が0.4〜1.2の範囲にて、得られた抵抗値が安定状態になるまで成膜を行うプリスパッタ工程(a)を有することを特徴とする透明導電フィルムの製造方法。 - 請求項1〜8のいずれかに記載の透明導電フィルムの製造方法であって、
前記高磁場RF重畳DCスパッタ成膜法を施す前に、酸素を導入することなく、不活性ガスの存在下に、RF重畳DCスパッタ成膜法により、RF電源の周波数が20MHzより大きく60MHz以下の時、RF電力/DC電力の電力比が0.2〜0.6の範囲にて、得られた抵抗値が安定状態になるまで成膜を行うプリスパッタ工程(a)を有することを特徴とする透明導電フィルムの製造方法。 - 前記形成工程(A)の後に、アニール処理工程(B)を、施すことを特徴と請求項1〜10のいずれかに記載の透明導電フィルムの製造方法。
- 前記アニール処理工程(B)を、120℃〜180℃の温度で、5分間〜5時間、大気中で行うことを特徴とする請求項11記載の透明導電フィルムの製造方法。
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JPH03249171A (ja) * | 1990-02-27 | 1991-11-07 | Ulvac Japan Ltd | 透明導電膜の製造方法およびその製造装置 |
JPH059724A (ja) * | 1991-07-09 | 1993-01-19 | Shinkuron:Kk | 透明導電膜の形成方法 |
JP2009104842A (ja) * | 2007-10-22 | 2009-05-14 | Nitto Denko Corp | 透明導電性フィルム、その製造方法及びそれを備えたタッチパネル |
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JP2017008380A (ja) * | 2015-06-23 | 2017-01-12 | 株式会社カネカ | 透明電極付き基板およびその製造方法 |
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WO2014112536A1 (ja) | 2014-07-24 |
US20160024644A1 (en) | 2016-01-28 |
TWI621725B (zh) | 2018-04-21 |
TW201435106A (zh) | 2014-09-16 |
KR101982906B1 (ko) | 2019-05-27 |
US9624573B2 (en) | 2017-04-18 |
CN104937678A (zh) | 2015-09-23 |
JP6215062B2 (ja) | 2017-10-18 |
KR20150103710A (ko) | 2015-09-11 |
CN104937678B (zh) | 2017-04-26 |
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