JP5025038B1 - 透光性硬質薄膜 - Google Patents
透光性硬質薄膜 Download PDFInfo
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Abstract
【選択図】図1
Description
その方法は、単一の真空容器内で反応プロセス領域と複数の成膜プロセス領域とがそれぞれ空間的に分離して配置され、各領域での処理が独立して制御可能に構成された成膜装置(ラジカルアシストスパッタリング装置)を用い、移動している基体に向けた薄膜の成膜方法であって、不活性ガスの雰囲気の下、各成膜プロセス領域のそれぞれで、材質が異なる複数のターゲットのうちのいずれかをスパッタリングし、珪素と炭素を含む中間薄膜を形成した後、前記反応プロセス領域で、前記中間薄膜に対して、不活性ガスと水素の混合ガスの雰囲気下で発生させたプラズマを曝露し(または接触させ)、超薄膜に膜変換させ、その後、該超薄膜に対して、前記中間薄膜の形成と前記超薄膜への膜変換を繰り返す方法である。
1…成膜装置(スパッタ装置)、11…真空容器、13…基板ホルダ、12,14,16…仕切壁、
20,40…成膜プロセス領域、スパッタ源(21a,21b,41a,41b…マグネトロンスパッタ電極、23,43…交流電源、24,44…トランス、29a,29b,49a,49b…ターゲット)、スパッタ用ガス供給手段(26,46…スパッタ用ガスボンベ、25,45…マスフローコントローラ)、
60…反応プロセス領域、80…プラズマ源(81…ケース体、83…誘電体板、85a,85b…アンテナ、87…マッチングボックス、89…高周波電源)、反応処理用ガス供給手段(68…反応処理用ガスボンベ、67…マスフローコントローラ)。
なお、本例において「超格子構造(Super lattice構造)」とは、異なる材料をナノ単位の膜厚で制御し、積層した構成をいう。
なお、反応処理用ガス供給手段は、上記構成(つまり、1つのボンベと1つのマスフローコントローラを含む構成)に限らず、複数のボンベとマスフローコントローラを含む構成(後述する本例を例に取ると、不活性ガスと酸素と水素を別々に貯蔵する3つのガスボンベと、各ボンベから供給される各ガスの流量を調整する3つのマスフローコントローラを含む構成)とすることもできる。
(1)まず、成膜の前準備をする。具体的には、まず電極21a,21b(又は41a,41b)の上にターゲット29a,29b(又は49a,49b)をセットする。これとともに、真空容器11の外で基板ホルダ13に成膜対象としての基板Sをセットし、真空容器11のロードロック室内に収容する。
真空容器11内の圧力の安定を確認した後、領域20内の圧力を例えば0.05〜0.2Paに調整し、その後、マスフローコントローラ25を介してガスボンベ26から所定流量のスパッタ用ガスを領域20に導入する。
SiO2層104の成膜と同様に、真空容器11内の圧力の安定を確認した後、領域20内の圧力を例えば0.05〜0.2Paに調整し、その後、マスフローコントローラ25を介してガスボンベ26から所定流量のスパッタ用ガスを領域20に導入する。
図2及び図3に示すスパッタ装置1を用い、基板Sとしてガラス性基板であるBK7(ただし実験例1−1ではサファイア基板)を基板ホルダ13に複数枚セットし、下記の条件で、SiO2層104の成膜と、SiC層106の成膜を交互に繰り返し、超格子構造を有する積層膜102を基板S上に成膜した各実験例サンプルを得た。なお、いずれのサンプルも、積層膜102の一層目と最終層にSiO2層104を成膜した。
・成膜レート:0.4nm/sec、
・基板温度:室温。
・スパッタ用ガス:Ar、
・スパッタ用ガス圧:0.1Pa、
・スパッタ用ガスの導入流量:500sccm、
・ターゲット29a,29b:珪素(Si)、
・スパッタリングパワー密度:8.5W/cm2、
・電極21a,21bに印加する交流電圧の周波数:40kHz。
・反応処理用ガス:O2、
・反応処理用ガスの導入流量:200sccm、
・高周波電源89からアンテナ85a,85bに供給される電力(プラズマ処理電力):2kW、
・アンテナ85a,85bに印加する交流電圧の周波数:13.56MHz。
・一層あたりの膜厚:4nm〜35nm(表1参照)、
・積層数:100層〜1120層(表1参照)。
・成膜レート:0.09nm/sec、
・基板温度:室温。
・スパッタ用ガス:Ar、
・スパッタ用ガス圧:0.1Pa、
・スパッタ用ガスの導入流量:150sccm、
・ターゲット29a,29b:珪素(Si)、
・スパッタリングパワー密度:1.5W/cm2、
・電極21a,21bに印加する交流電圧の周波数:40kHz。
・スパッタ用ガス:Ar、
・スパッタ用ガス圧:0.1Pa、
・スパッタ用ガスの導入流量:150sccm、
・ターゲット49a,49b:炭素(C)、
・スパッタリングパワー密度:4.3W/cm2、
(珪素(Si)で構成されるターゲット29a,29bをスパッタリングするパワー密度の約2.9倍に相当)
・電極41a,41bに印加する交流電圧の周波数:40kHz。
・反応処理用ガス:Ar+H2、
・反応処理用ガス中の水素濃度:表1を参照、
・反応処理得用ガス圧:0.3Pa、
・反応処理用ガスの導入流量:500sccm、
・プラズマ処理電力:2kW、
・アンテナ85a,85bに印加する交流電圧の周波数:13.56MHz。
・一層あたりの膜厚:1.25nm〜21nm(表1参照)、
・積層数:100層〜1120層(表1参照)。
・膜厚:2000nm〜7000nm(表1参照)。
得られた各サンプルについて、下記の方法で物性の評価をし、その結果を下記表に示した。
微小硬さ試験機(MMT−X7、マツザワ社製)を用い、下記の測定条件で、実験例サンプルの積層膜表面の硬さを測定した。
・圧子形状:ビッカース圧子(a=136°)、
・測定環境:温度20℃・相対湿度60%、
・試験荷重:25gf、
・荷重速度:10μ/s、
・最大荷重クリープ時間:15秒。
分光光度計(商品名:U−4000、日立社製)を用いて波長650nm〜700nmにおける透過率を測定した。
水平直線往復摺動方式による自動摩擦摩耗解析装置(Triboster TS501:協和界面科学社製)を用い、荷重:50g、速度:60mm/分、測定回数:10往復の条件で、サンプルの積層膜側の動摩擦係数(μk)を測定した。
積層膜102全体とSiO2層104の膜厚を固定した上でSiC層106の膜厚を変動させたとき、一層あたりのSiC層106の膜厚がSiO2層104の30〜60%の範囲外となるサンプル(実験例6,9,11,14,15,18)と比較して、その範囲内となるサンプル(実験例7,8,12,13,16,17)の有用性が確認できた。
積層膜102全体の膜厚を大きくし、かつ一層あたりのSiC層106の膜厚をSiO2層104の30〜60%の範囲内としても、一層あたりのSiO2層の膜厚が5〜30nmの範囲外となるサンプル(実験例10,19)は、その範囲内となるサンプル(実験例8,17など)と比較した有用性が得られないことが確認された。
Claims (4)
- 基体の表面に形成された透光性硬質薄膜であって、
SiO2層とSiC層とを交互に複数積層した超格子構造を有する積層膜で構成されており、
一層あたりの膜厚が、SiO2層:5nm以上30nm以下、SiC層:SiO2層の30%以上60%以下であり、
全体膜厚が3000nm以上である透光性硬質薄膜。 - 請求項1記載の透光性硬質薄膜において、前記SiC層を以下の方法によって、前記基体又は既に形成されたSiO2層の表面に形成した透光性硬質薄膜。
単一の真空容器内で反応プロセス領域と複数の成膜プロセス領域とがそれぞれ空間的に分離して配置され、各領域での処理が独立して制御可能に構成された成膜装置を用い、移動している基体に向けた薄膜の成膜方法であり、不活性ガスの雰囲気の下、各成膜プロセス領域のそれぞれで、材質が異なる複数のターゲットのうちのいずれかをスパッタリングし、珪素と炭素を含む中間薄膜を形成した後、前記反応プロセス領域で、前記中間薄膜に対して、不活性ガスと水素の混合ガスの雰囲気下で発生させたプラズマを曝露し、超薄膜に膜変換させ、その後、該超薄膜に対して、前記中間薄膜の形成と前記超薄膜への膜変換を繰り返す方法。 - ガラス製の前記基体上に請求項1又は2記載の透光性硬質薄膜を形成した光学基板。
- 請求項3記載の光学基板において、波長650nm〜700nmでの透過率が70%以上、前記薄膜側のビッカーズ硬度が1500以上、動摩擦係数が0.5以下である光学基板。
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US (1) | US9422620B2 (ja) |
EP (1) | EP2816136B1 (ja) |
JP (1) | JP5025038B1 (ja) |
KR (1) | KR101287694B1 (ja) |
CN (1) | CN103370437B (ja) |
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JP6392912B2 (ja) * | 2017-01-31 | 2018-09-19 | 学校法人東海大学 | 成膜方法 |
CN107841712B (zh) * | 2017-11-01 | 2018-10-30 | 浙江水晶光电科技股份有限公司 | 高折射率氢化硅薄膜的制备方法、高折射率氢化硅薄膜、滤光叠层和滤光片 |
CN108191258B (zh) * | 2018-01-30 | 2020-05-05 | 武汉理工大学 | 一种dlc薄膜增硬玻璃及其制备方法 |
CN114907020A (zh) * | 2021-02-08 | 2022-08-16 | 深圳南玻应用技术有限公司 | 夹胶镀膜玻璃 |
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JPS61237492A (ja) * | 1985-04-13 | 1986-10-22 | ロ−ム株式会社 | サ−マルプリントヘツドの保護膜形成方法 |
JPS6362867A (ja) * | 1986-09-02 | 1988-03-19 | Seikosha Co Ltd | 有色物品 |
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JP2001234338A (ja) * | 2000-02-25 | 2001-08-31 | Shincron:Kk | 金属化合物薄膜の形成方法およびその形成装置 |
JP2004335325A (ja) * | 2003-05-09 | 2004-11-25 | Ushio Inc | 遠赤外線放射体 |
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US4971851A (en) * | 1984-02-13 | 1990-11-20 | Hewlett-Packard Company | Silicon carbide film for X-ray masks and vacuum windows |
JPS60221562A (ja) * | 1984-04-17 | 1985-11-06 | Matsushita Electric Ind Co Ltd | 耐摩耗膜 |
US5880491A (en) * | 1997-01-31 | 1999-03-09 | The United States Of America As Represented By The Secretary Of The Air Force | SiC/111-V-nitride heterostructures on SiC/SiO2 /Si for optoelectronic devices |
US6252295B1 (en) * | 2000-06-19 | 2001-06-26 | International Business Machines Corporation | Adhesion of silicon carbide films |
US6689479B2 (en) * | 2001-08-28 | 2004-02-10 | Dai Nippon Printing Co., Ltd. | Anti-reflection film, and silica layer |
JP4533815B2 (ja) * | 2005-07-08 | 2010-09-01 | 株式会社東芝 | スパッタリングターゲットとそれを用いた光学薄膜の製造方法 |
CN102213778B (zh) * | 2011-05-27 | 2013-04-24 | 宁波永新光学股份有限公司 | 在光学材料表面形成高硬度低摩擦光学薄膜的方法 |
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JPS61237492A (ja) * | 1985-04-13 | 1986-10-22 | ロ−ム株式会社 | サ−マルプリントヘツドの保護膜形成方法 |
JPS6362867A (ja) * | 1986-09-02 | 1988-03-19 | Seikosha Co Ltd | 有色物品 |
JPS63113507A (ja) * | 1986-10-31 | 1988-05-18 | Hitachi Ltd | 光導波路およびその製造法 |
JP2001234338A (ja) * | 2000-02-25 | 2001-08-31 | Shincron:Kk | 金属化合物薄膜の形成方法およびその形成装置 |
JP2004335325A (ja) * | 2003-05-09 | 2004-11-25 | Ushio Inc | 遠赤外線放射体 |
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KR101287694B1 (ko) | 2013-08-07 |
TW201335393A (zh) | 2013-09-01 |
EP2816136A4 (en) | 2015-10-28 |
WO2013121552A1 (ja) | 2013-08-22 |
CN103370437A (zh) | 2013-10-23 |
EP2816136B1 (en) | 2019-04-10 |
CN103370437B (zh) | 2015-07-15 |
US20140356601A1 (en) | 2014-12-04 |
EP2816136A1 (en) | 2014-12-24 |
TWI429770B (zh) | 2014-03-11 |
US9422620B2 (en) | 2016-08-23 |
HK1185922A1 (zh) | 2014-02-28 |
JPWO2013121552A1 (ja) | 2015-05-11 |
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