JP6533374B2 - Dlc皮膜の成膜方法 - Google Patents
Dlc皮膜の成膜方法 Download PDFInfo
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Description
1)チャンバ10内の圧力が2.6×10−3Paに到達した後、ヒーター(図示せず)によって基材3を200℃まで加熱する。
2)ヒーターを切り、約5分程度待つ。
3)Arガスをチャンバ10内に導入し、基材にバイアス電圧300Vを印加し、ガス圧1.3Paで約1分間基材3のクリーニングを行う。
4)基材3の温度が上がり過ぎないように約1分程度バイアス電圧の印加を止める。
5)上記3)、4)の工程を5回繰り返す。
6)Arガスをチャンバ10内に導入し、基材にバイアス電圧400Vを印加し、ガス圧1.3Paで1分間基材3のクリーニングを行う。
7)基材3の温度が上がり過ぎないように約1分程度バイアス電圧の印加を止める。
8)上記6)、7)の工程を10回繰り返す。
1)チャンバ10内にArガスを導入し、圧力を0.4Paにした後、Tiターゲットにスパッタ出力6kW、基材3にバイアス電圧200Vを印加して30分成膜することで0.2μmのTi層を成膜する。
2)バイアス電圧は50Vとし、Arガス中にメタンガス(CH4ガス)を徐々に加えていくことにより、Ti−TiC傾斜層を作成する。最終的なガス組成はArガス:メタンガス=95:5とし、ガス圧は0.4Pa、スパッタ出力は6kW、7.5分成膜することで0.1μmの傾斜層を成膜する。
3)ガス組成Arガス:メタンガス=90:10とし、ガス圧は0.2Pa、スパッタ出力は6kW、バイアス電圧は50Vとして、90分成膜することで0.3μmのTiC層を成膜する。
先ず、実施例1〜3ならびに比較例1、2として成膜ガスを純度99.9995%のメタンガスのみとしてDLC皮膜の成膜を行った。実施例1〜3ならびに比較例1、2の成膜条件(ガス圧力、ガス流量、電源条件、成膜時間、成膜速度、基材温度)は以下の表1に示す通りである。また、表1には、各成膜条件にて成膜されたDLC皮膜の膜特性(膜厚、表面硬度、密着性)についても記載している。また、図2は実施例1〜3のガス圧力とHIT(インデンテーション硬さ)の関係を示すグラフ、図3はガス圧力と成膜速度の関係を示すグラフ、図4はガス圧力と基材(ワーク)温度の関係を示すグラフである。
次に、実施例4〜8ならびに比較例3、4として成膜ガスを純度98%のアセチレンガスのみとしてDLC皮膜の成膜を行った。実施例4〜8ならびに比較例3、4の成膜条件は以下の表2に示す通りである。また、表2には、各成膜条件にて成膜されたDLC皮膜の膜特性についても記載している。また、図5は実施例4〜8のガス圧力とHIT(インデンテーション硬さ)の関係を示すグラフ、図6はガス圧力と成膜速度の関係を示すグラフ、図7はガス圧力と基材(ワーク)温度の関係を示すグラフである。
また、各成膜条件で成膜されたDLC皮膜の耐熱性は成膜後に当該膜を300℃、400℃、450℃まで加熱したところ、実施例5、6では450℃までHITの変化率も小さく、膜の軟化も見られないことがわかった。また、実施例8では、300℃まではHITの変化率も小さく、膜の軟化も見られないことがわかった。DLC皮膜の耐熱性が300℃よりも低いと、高温となる環境への適用ができなくなるため、耐熱性は高い方が好ましい。例えば耐熱性の好適な範囲は300℃以上、より好ましくは400℃以上である。更に好ましくは450℃以上である。
次に、実施例9〜11ならびに比較例5として、成膜ガスを純度98%のアセチレンガスに流量比20%の純度99.9999%のArガスを加えたものとしてDLC皮膜の成膜を行った。実施例9〜11ならびに比較例5の成膜条件は以下の表3に示す通りである。また、表3には、各成膜条件にて成膜されたDLC皮膜の膜特性についても記載している。また、図9は実施例9〜11のガス圧力とHIT(インデンテーション硬さ)の関係を示すグラフ、図10はガス圧力と成膜速度の関係を示すグラフ、図11はガス圧力と基材(ワーク)温度の関係を示すグラフである。
次に、実施例12、13として成膜ガスをアセチレンガスのみとし、ガス圧力を1Paとし、電源の放電電流(ピーク電流)を8Aならびに12AとしてDLC皮膜の成膜を行った。実施例12、13の成膜条件は以下の表4に示す通りである。なお、表4には、各成膜条件にて成膜されたDLC皮膜の膜特性についても記載している。
次に、実施例14〜18として成膜ガスをアセチレンガスのみとし、直流パルス電源の周波数をそれぞれ1kHz、5kHz、10kHz、20kHz、25kHzとしてDLC皮膜の成膜を行った。実施例14〜18の成膜条件は以下の表5に示す通りである。ここで、パルス電源の周波数は、例えば100kHz超になると安定してプラズマが発生せず成膜が不安定となる恐れがあり、また、装置の大型化や、ワーク温度の高温化等が懸念されるため、1kHz以上100kHz以下とすることが好ましい。更には、以下の表5に示すように1kHz以上25kHz以下とすることがより好ましい。なお、表5には、各成膜条件にて成膜されたDLC皮膜の膜特性についても記載している。また、図12は実施例14〜18のパルス周波数とHIT(インデンテーション硬さ)の相関関係を示すグラフである。
次に、実施例19〜21として成膜ガスをアセチレンのみとし、ガス圧力を0.5Pa、1Pa、3Paとし、電源のパルス周波数をいずれの場合も25kHzとしてDLC皮膜の成膜を行った。実施例19〜21の成膜条件は以下の表6に示す通りである。なお、表6には、各成膜条件にて成膜されたDLC皮膜の膜特性についても記載している。また、図13は実施例19〜21の圧力(成膜圧力)とHIT(インデンテーション硬さ)の相関関係を示すグラフである。
Carbon:ダイヤモンドライクカーボン)皮膜の成膜方法に適用できる。
3…基材
10…チャンバ
15…排気装置
20…Arガス供給部
21…メタンガス供給部
22…アセチレンガス供給部
28…電源
Claims (6)
- 基材に電圧を印加することのみにより、チャンバ内のガスをプラズマ化し、プラズマCVD法で基材上にDLC皮膜を成膜させる成膜方法であって、
直流パルス電源を用いて基材に印加する電圧をバイアス電圧とし、
チャンバ内に供給する成膜ガスとして、アセチレンガス又はメタンガスを用い、
且つ、チャンバ内のガスの全圧を、
メタンガスを用いた場合は0.5Pa以上3Pa以下とし、
アセチレンガスを用いた場合は0.3Pa以上3Pa以下とし、
前記バイアス電圧は0.9kV以上2.2kV以下とする、DLC皮膜の成膜方法。 - 成膜ガスとしての前記アセチレンガス又はメタンガスにArガスを混合する、請求項1に記載のDLC皮膜の成膜方法。
- 前記パルス電源の周波数は1kHz以上100kHz以下とする、請求項1又は2に記載のDLC皮膜の成膜方法。
- チャンバ内でPVD法により中間層を基材上に形成し、
次いで、同チャンバ内でプラズマCVD法によりDLC皮膜を成膜させる、請求項1〜3のいずれか一項に記載のDLC皮膜の成膜方法。 - 前記中間層の形成において、成膜ガスとしてArガス及びメタンガスを用い、
スパッタ出力及び成膜ガス中のArガスとメタンガスの比を変化させて当該中間層内で連続的に組成を変化させる、請求項4に記載のDLC皮膜の成膜方法。 - 前記中間層の形成において、当該中間層の組成をArガスとメタンガスの比が、基材側が金属リッチ、DLC皮膜側が炭素リッチとなるように構成する、請求項5に記載のDLC皮膜の成膜方法。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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JP2014183701A JP6533374B2 (ja) | 2013-11-06 | 2014-09-09 | Dlc皮膜の成膜方法 |
US15/034,839 US10145007B2 (en) | 2013-11-06 | 2014-10-31 | DLC film film-forming method |
PCT/JP2014/079074 WO2015068655A1 (ja) | 2013-11-06 | 2014-10-31 | Dlc皮膜の成膜方法 |
CN201480060931.9A CN105705678B (zh) | 2013-11-06 | 2014-10-31 | Dlc覆膜的成膜方法 |
MX2016005905A MX2016005905A (es) | 2013-11-06 | 2014-10-31 | Metodo de formacion de pelicula para pelicula dlc. |
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JP2013230539 | 2013-11-06 | ||
JP2013230539 | 2013-11-06 | ||
JP2014037364 | 2014-02-27 | ||
JP2014037364 | 2014-02-27 | ||
JP2014183701A JP6533374B2 (ja) | 2013-11-06 | 2014-09-09 | Dlc皮膜の成膜方法 |
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JP2015178670A JP2015178670A (ja) | 2015-10-08 |
JP6533374B2 true JP6533374B2 (ja) | 2019-06-19 |
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US6002418A (en) * | 1997-04-16 | 1999-12-14 | Fuji Photo Film Co., Ltd. | Thermal head |
US20010044027A1 (en) * | 1999-12-30 | 2001-11-22 | Anderson Jerrel Charles | Diamond-like carbon coating on glass for added hardness and abrasion resistance |
DE10018143C5 (de) * | 2000-04-12 | 2012-09-06 | Oerlikon Trading Ag, Trübbach | DLC-Schichtsystem sowie Verfahren und Vorrichtung zur Herstellung eines derartigen Schichtsystems |
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JP5144562B2 (ja) * | 2008-03-31 | 2013-02-13 | 日本碍子株式会社 | Dlc膜量産方法 |
JP4755262B2 (ja) | 2009-01-28 | 2011-08-24 | 株式会社神戸製鋼所 | ダイヤモンドライクカーボン膜の製造方法 |
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US10145007B2 (en) | 2018-12-04 |
CN105705678B (zh) | 2018-09-28 |
US20160281219A1 (en) | 2016-09-29 |
MX2016005905A (es) | 2016-07-13 |
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