JP4725085B2 - 非晶質炭素、非晶質炭素被膜部材および非晶質炭素膜の成膜方法 - Google Patents
非晶質炭素、非晶質炭素被膜部材および非晶質炭素膜の成膜方法Info
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Classifications
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/30—Self-sustaining carbon mass or layer with impregnant or other layer
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Mechanical Engineering (AREA)
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Description
成膜炉内に配置されかつマイナス極に結線された基材保持具に前記基材が互いに対向する状態で複数の該基材を配置すると共に、隣接する2個の該基材の負グローが互いに重なるように、水素含有量が60at%以上である処理ガス圧力およびプラズマ電源を操作して得られ、
炭素を主成分とし、水素を30at%を超え60at%以下含み、該炭素の全体量を100at%とした場合にsp3混成軌道を持つ炭素量が10at%以上85at%以下であり、かつ、弾性率が40〜150GPaでビッカース硬さがHv400〜1500であることを特徴とする。
成膜炉内に配置されかつマイナス極に結線された基材保持具に前記基材が互いに対向する状態で複数の該基材を配置すると共に、隣接する2個の該基材の負グローが互いに重なるように、水素含有量が60at%以上である処理ガス圧力およびプラズマ電源を操作して得られ、
前記被膜は、炭素を主成分とし、水素を30at%を超え60at%以下含み、該炭素の全体量を100at%とした場合にsp3混成軌道を持つ炭素量が10at%以上85at%以下であり、かつ、弾性率が40〜150GPaでビッカース硬さがHv400〜1500である非晶質炭素からなることを特徴とする。
成膜炉内に配置されかつマイナス極に結線された基材保持具に前記基材が互いに対向する状態で複数の該基材を配置すると共に、隣接する2個の該基材の負グローが互いに重なるように、水素含有量が60at%以上である処理ガス圧力およびプラズマ電源を操作して行うことを特徴とする。
本発明の非晶質炭素は、炭素を主成分とし、水素を30at%を超え60at%以下含み、かつ、弾性率が40〜150GPaであることを特徴とする。本発明の非晶質炭素には、一般的な非晶質炭素よりも多くの水素が含まれる。水素量が多い非晶質炭素は、有機成分であるC−H結合を多く含むため、弾性率が40〜150GPaの低い弾性率を示す軟質な非晶質炭素である。水素量が少ないと非晶質炭素の柔軟性が損なわれ、また、水素量が多すぎると非晶質炭素の合成が困難となる。本発明の非晶質炭素の好ましい水素量は、35at%以上50at%以下である。
本発明の非晶質炭素被膜部材は、導電性の基材と、その基材の表面の少なくとも一部に固定した被膜と、からなる。そして、被膜は、炭素を主成分とし、水素を30at%を超え60at%以下含み、かつ、弾性率が40〜150GPaである非晶質炭素からなる。なお、被膜は、前述した本発明の非晶質炭素からなる被膜である。
本発明の非晶質炭素膜の成膜方法は、プラズマCVD法によって導電性の基材の表面の少なくとも一部に非晶質炭素膜を形成する。この際、成膜炉内に配置されかつマイナス極に結線された基材保持具に、基材が互いに対向する状態で複数の基材を配置すると共に、隣接する2個の基材の負グローが互いに重なるように、処理ガス圧力およびプラズマ電源を操作して行う。
図1(および図5)は非晶質炭素膜の成膜装置の概略説明図である。
実施例1の非晶質炭素被膜部材を、図1および図2を用いて説明する。なお、図2は、本実施例における成膜中のグロー放電の様子を模式的に表した図であって、図1のX−X’での断面図である。
平板基材22をステンレス鋼(SUS304)とした他は実施例1と同様に、平板基材22の表面に非晶質炭素膜を成膜した。なお、6時間の成膜(成膜温度300℃)で、平板基材22の表面に膜厚16μmの膜が得られた。
平板基材22をアルミニウム合金2017(22mm×39mm×3mm)とし、成膜温度を500℃とした他は実施例1と同様に、平板基材22表面に非晶質炭素膜を成膜した。なお、2.5時間の成膜で、平板基材22の表面に膜厚22μmの膜が得られた。
本比較例では、平板基材22として、アルミニウム合金2017(22mm×39mm×3mm)を4枚用いた。これらの平板基材22は、図4に示すように、厚さ方向に平行かつ並列状態で配置され、この状態で支持台21に固定した。この際、隣接する2個の平板基材22の対向面間の間隔Dは、それぞれ60mmとした。
平板基材22をステンレス鋼(SUS304)とした他は比較例1と同様に、平板基材22表面に非晶質炭素膜を成膜した。なお、2時間の成膜(成膜温度300℃)で、平板基材22の表面に膜厚3μmの膜が得られた。
成膜時間を4時間とした他は比較例1と同様に、平板基材22表面に非晶質炭素膜を成膜した。なお、4時間の成膜(成膜温度300℃)で、平板基材22の表面に膜厚5μmの膜が得られた。
実施例4の非晶質炭素被膜部材を、図5〜図7を用いて説明する。なお、図6は、図5における基材の配置状態を上方から見た平面図である。また、図7は、本実施例における成膜中のグロー放電の様子を模式的に表した図であって、図6のY−Y’での断面図である。
原料ガスとしてメタン、希釈ガスとして水素ガス、を用いた他は、実施例1と同様にして成膜を行った。混合ガスの流量は、メタン:50sccm、水素ガス:60sccm、処理ガス圧を300Paとした他は実施例1と同様に平板基材22表面に非晶質炭素膜を成膜した。なお、6時間の成膜で、平板基材22の表面に膜厚8μmの膜が得られた。
No.1〜No.8の非晶質炭素被膜部材に対して、非晶質炭素膜の水素および珪素の含有量、弾性率、ビッカース硬さ、および、欠陥面積率を測定した。水素の量は弾性反跳粒子検出法(ERDA)、珪素の量はEPMA(electron probe microanalyser)により測定した。弾性率およびビッカース硬さは、ナノインデンターを用いた試験により求めた。欠陥面積率は、電気化学的測定法である、臨界不動態電流密度(CPCD)法により、基材まで貫通する非晶質炭素膜のピンホール型欠陥の面積率を測定した。測定結果を表1に示す。表1では、非晶質炭素膜の組成として、水素および珪素についてだけ示している。残りの組成は炭素である。例えば、NO.1の非晶質炭素膜の組成は、炭素51at%、水素38at%、珪素11at%である。
(比較例4)
実施例1において、処理ガス圧を10Paとして成膜を行った。この際、成膜時間を3時間とした。シース幅および非晶質炭素膜の膜厚を表2に示す。そして、比較例4で得られた非晶質炭素膜を有する非晶質炭素被膜部材を、No.9とした。
実施例1において、処理ガス圧を133,266,400,533Paとして成膜を行った。この際、成膜時間を3時間とした。各処理ガス圧のシース幅および非晶質炭素膜の膜厚を表2に示す。そして、実施例6で得られた非晶質炭素膜を有する非晶質炭素被膜部材を、それぞれNo.10〜13とした。
実施例1において、処理ガス圧を800Paおよび933Paとして成膜を行った。この際、成膜時間を3時間とした。各処理ガス圧のシース幅および非晶質炭素膜の膜厚を表2に示す。そして、比較例5で得られた非晶質炭素膜を有する非晶質炭素被膜部材を、それぞれNo.14,No.15とした。
平板基材22をアルミニウム合金2017(22mm×39mm×3mm)とし、原料ガスとしてヘキサンおよびTMS、希釈ガスとして水素ガスを用い、実施例1と同様にして成膜を行った。本実施例では、混合ガスの流量を、ヘキサン:20sccm、TSM:2sccm、水素ガス:100sccmとし、処理ガス圧を400Pa、成膜温度を300℃とした。
成膜方法および膜組成の異なる二種類の非晶質炭素膜について、C−H結合を評価した。一方は、アルミニウム合金2017製の基材(100mm×50mm×1.5mm)表面に、実施例1と同様にして成膜した非晶質炭素膜である(試料1)。非晶質炭素膜の水素量は約38at%、珪素量は11at%、弾性率は84GPaである。
上述した成膜装置を用い、水素ガス雰囲気で、アルミニウム合金2017製の基材(22mm×39mm×3mm)を種々の配置形態で300℃になるよう放電させ、その際、基材表面に発生したプラズマを測定した。プラズマの測定には、プラズマプロセスモニタ「C7460」(浜松ホトニクス社製)を使用した。測定条件は、測定波長:200〜950nm、測定エリア:φ3mm、露光時間:0.1秒、積算回数:10回とした。そして、波長200〜960nmでの光強度の積分値をプラズマ発光強度と規定した。
16:プラズマ電源
21:支持台(基材保持具)
22:平板基材(基材)
220:メッシュ
222:基板(基材)
24:負グロー
25:シース
26:負グローの重なり
Claims (18)
- プラズマCVD法によって導電性の基材の表面の少なくとも一部に形成される非晶質炭素であって、
成膜炉内に配置されかつマイナス極に結線された基材保持具に前記基材が互いに対向する状態で複数の該基材を配置すると共に、隣接する2個の該基材の負グローが互いに重なるように、水素含有量が60at%以上である処理ガス圧力およびプラズマ電源を操作して得られ、
炭素を主成分とし、水素を30at%を超え60at%以下含み、該炭素の全体量を100at%とした場合にsp3混成軌道を持つ炭素量が10at%以上85at%以下であり、かつ、弾性率が40〜150GPaでビッカース硬さがHv400〜1500であることを特徴とする非晶質炭素。 - 前記炭素の全体量を100at%とした場合に、sp3混成軌道を持つ炭素量が20at%以上50at%以下である請求項1記載の非晶質炭素。
- 全体を100at%とした場合に、珪素を50at%以下含む請求項1記載の非晶質炭素。
- 導電性の基材と、プラズマCVD法によって該基材の表面の少なくとも一部に形成された被膜と、からなり、
成膜炉内に配置されかつマイナス極に結線された基材保持具に前記基材が互いに対向する状態で複数の該基材を配置すると共に、隣接する2個の該基材の負グローが互いに重なるように、水素含有量が60at%以上である処理ガス圧力およびプラズマ電源を操作して得られ、
前記被膜は、炭素を主成分とし、水素を30at%を超え60at%以下含み、該炭素の全体量を100at%とした場合にsp3混成軌道を持つ炭素量が10at%以上85at%以下であり、かつ、弾性率が40〜150GPaでビッカース硬さがHv400〜1500である非晶質炭素からなることを特徴とする非晶質炭素被膜部材。 - 前記炭素の全体量を100at%とした場合に、sp3混成軌道を持つ炭素量が20at%以上50at%以下である請求項4記載の非晶質炭素被膜部材。
- 前記被膜は、膜厚が0.1〜200μmである請求項4記載の非晶質炭素被膜部材。
- 前記非晶質炭素は、全体を100at%とした場合に、珪素を50at%以下含む請求項4記載の非晶質炭素被膜部材。
- プラズマCVD法によって導電性の基材の表面の少なくとも一部に、炭素を主成分とし水素を30at%を超え60at%以下含む非晶質炭素膜を形成する非晶質炭素膜の成膜方法であって、
成膜炉内に配置されかつマイナス極に結線された基材保持具に前記基材が互いに対向する状態で複数の該基材を配置すると共に、隣接する2個の該基材の負グローが互いに重なるように、水素含有量が60at%以上である処理ガス圧力およびプラズマ電源を操作して行うことを特徴とする非晶質炭素膜の成膜方法。 - 前記負グローの重なった部分のプラズマ発光強度は、重ならない部分のプラズマ発光強度の7倍以上である請求項8記載の非晶質炭素膜の成膜方法。
- 前記基材の表面から前記負グローまでのシース幅は、隣接する2個の該基材の対向面間の間隔の4分の1以上で隣接する2個の該基材の対向面間の間隔以下とする請求項8記載の非晶質炭素膜の成膜方法。
- 前記処理ガス圧力の範囲は13〜1330Paとし、隣接する2個の前記基材の対向面間の間隔は2〜60mmである請求項8記載の非晶質炭素膜の成膜方法。
- 隣接する2個の前記基材の一方は、導電性で表裏面を貫通する複数の通孔をもつ部材からなる請求項8記載の非晶質炭素膜の成膜方法。
- 前記複数の通孔をもつ部材は、該通孔の内部で負グローが重なり合う請求項12記載の非晶質炭素膜の成膜方法。
- 前記処理ガスは、炭化水素ガスからなる、または、該炭化水素ガスと、水素ガスおよび希ガスのうちのいずれか一種以上を含む希釈ガスと、の混合ガスからなる請求項8記載の非晶質炭素膜の成膜方法。
- 前記処理ガスは、炭化水素ガスならびに少なくとも珪素を含む有機金属含有ガスおよびハロゲン化合物のうちのいずれか1種以上を含む原料ガスからなる、または、該原料ガスと、水素ガスおよび希ガスのうちのいずれか一種以上を含む希釈ガスと、の混合ガスからなる請求項8記載の非晶質炭素膜の成膜方法。
- 前記有機金属含有ガスは、テトラメチルシランおよびシランである請求項15記載の非晶質炭素膜の成膜方法。
- 前記ハロゲン化合物は、四塩化シリコンである請求項15記載の非晶質炭素膜の成膜方法。
- 前記被膜は、欠陥面積率が10 −4 以下である請求項4〜7のいずれかに記載の非晶質炭素被膜部材。
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