JP5660804B2 - カーボンナノチューブの形成方法及びカーボンナノチューブ成膜装置 - Google Patents
カーボンナノチューブの形成方法及びカーボンナノチューブ成膜装置 Download PDFInfo
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Description
前記触媒金属層に酸素プラズマ処理を施す工程と、
前記酸素プラズマ処理を施した後の前記触媒金属層に水素プラズマ処理を施して、前記触媒金属層の表面を活性化する工程と、
成膜装置の処理容器内で、被処理体の上方に多数の貫通開口を有する電極部材を配置し、該電極部材に直流電圧を印加しながら、該電極部材の上方空間で生成させたプラズマ中の活性種を、前記貫通開口を通過させて下方の被処理体へ向けて拡散させ、前記活性化された触媒金属層の上にプラズマCVD法によりカーボンナノチューブを成長させることにより被処理体の開口部内にカーボンナノチューブを埋め込む工程と、
を備えている。
前記処理容器内で被処理体を載置する載置台と、
前記処理容器内にプラズマ生成ガスを導入する第1のガス導入部と、
前記処理容器内に、カーボンナノチューブの原料ガスを導入する第2のガス導入部と、
前記処理容器内で、前記載置台の上方に配置された多数の貫通開口を有する電極部材と、
前記電極部材に直流電圧を印加する電源と、
前記処理容器内を減圧排気する排気装置と、
を備え、
前記電極部材に直流電圧を印加しながら該電極部材よりも上方の空間で生成させたプラズマ中の活性種を、前記貫通開口を通過させて下方の被処理体へ向けて拡散させることにより、被処理体上にプラズマCVD法によってカーボンナノチューブを成長させるようにした。
前記電極部材は、前記プラズマ中に前記カーボンナノチューブの原料ガスを混合する部位と、前記載置台との間に介在配置されていてもよい。
前記誘電体部材の上方に設けられ、該誘電体部材を介して前記処理空間にマイクロ波を導入する平面アンテナと、
をさらに備えており、
前記第1のガス導入部は、前記誘電体部材の直下の空間にガスを導入するように配置されており、
前記第2のガス導入部は、前記第1のガス導入部より、前記載置台に近い位置で前記誘電体部材と前記載置台との間に介在して配置されており、
前記電極部材は、前記第2のガス導入部と前記載置台との間に介在して配置されていてもよい。
前記第2のガス導入部は、前記プラズマCVD法によりカーボンナノチューブの成長を行う前の前処理として、被処理体に対して水素プラズマ処理を行うための水素含有ガス供給源に接続されていてもよい。
実施例1:
図9に示すように、Si基板301上に積層形成されたSiO2層303A,303Bの上側のSiO2層303Bに、開口部として約200nm径の凹部305を形成したウエハWを使用した。SiO2層303A,303Bの間には、TiNからなる下地層307が70nmの厚さで形成してあり、凹部305の底面には、下地層307の上にNi触媒層309が2nmの厚さで形成してある。また、SiO2層303Bの表面には、SiCN層311が形成されている。このウエハWを図1の成膜装置100と同様構成を有する成膜装置の処理容器内に搬入し、下記の条件で、酸素プラズマ処理、水素プラズマ処理を順次行った後、処理容器内をパージし、その後、凹部305内にカーボンナノチューブを成長させた。なお、実験に使用したグリッド電極は、ステンレスの材質で、貫通開口の径が2mm、貫通開口の高さ(グリッド電極の厚み)が0.1mmのものを使用した。
処理温度:400℃
処理圧力:267Pa(2Torr)
処理ガス:
O2ガス 100mL/min(sccm)
Arガス 450mL/min(sccm)
マイクロ波パワー:1kW
グリッド電極への印加電圧:0V
処理時間:10分間
処理温度:400℃
処理圧力:66.7Pa(0.5Torr)
処理ガス:
H2ガス 462mL/min(sccm)
Arガス 450mL/min(sccm)
マイクロ波パワー:1kW
グリッド電極への印加電圧:0V
処理時間:30秒間
処理温度:400℃
処理圧力:400Pa(3Torr)
処理ガス:
N2ガス 200mL/min(sccm)
Arガス 450mL/min(sccm)
グリッド電極への印加電圧:0V
処理時間:2分間
処理温度:380℃、400℃、420℃、440℃
処理圧力:400Pa(3Torr)
処理ガス:
C2H4ガス 6.3mL/min(sccm)
H2ガス 370mL/min(sccm)
Arガス 450mL/min(sccm)
マイクロ波パワー:0.5kW
グリッド電極への印加電圧:−100V
処理時間:30分間
次に、グリッド電極に印加する電圧の影響について検討した。実施例1と同様の装置及び方法を用い、グリッド電極に印加する電圧を変化させてカーボンナノチューブを成長させた。本実施例では処理温度を470℃とし、グリッド電極に−100V又は−300Vの電圧を印加した。その他の条件は実施例1に示した条件と同じである。図11Aはグリッド電極に印加した電圧が−100Vのとき、図11Bは−300Vのときのカーボンナノチューブの断面を走査型電子顕微鏡(SEM)で撮影した写真である。これらの結果より、グリッド電極の負電圧を高くすることでカーボンナノチューブの充填密度を高められることが分かる。
続いて、実施例1と同様の装置及び方法を用い、被処理体の開口部がストレートライン(横長の溝)を形成している場合について検討した。本実施例では、開口部の幅が100nmの溝を形成している基板を用いて、処理温度を420℃としたこと以外は実施例1に示した条件と同一の条件で、グリッド電極に印加する電圧を−100Vとしてカーボンナノチューブを成長させた。その結果、図12に示したように、高い充填率で溝内にカーボンナノチューブを埋め込むことができた。このように、ビアホール用の開口部だけではなく、トレンチ溝用の開口部にもカーボンナノチューブを充填させることが可能である。
Claims (14)
- 表面に1又は複数の開口部を有し、当該開口部の底に触媒金属層が形成された被処理体を準備する工程と、
前記触媒金属層に酸素プラズマ処理を施す工程と、
前記酸素プラズマ処理を施した後の前記触媒金属層に水素プラズマ処理を施して、前記触媒金属層の表面を活性化する工程と、
成膜装置の処理容器内で、被処理体の上方に多数の貫通開口を有する電極部材を配置し、該電極部材に直流電圧を印加しながら、該電極部材の上方空間で生成させたプラズマ中の活性種を、前記貫通開口を通過させて下方の被処理体へ向けて拡散させ、前記活性化された触媒金属層の上にプラズマCVD法によりカーボンナノチューブを成長させることにより被処理体の開口部内にカーボンナノチューブを埋め込む工程と、
を備えているカーボンナノチューブの形成方法。 - 前記電極部材に−300V以上0V以下の範囲内の直流電圧を印加する請求項1に記載のカーボンナノチューブの形成方法。
- 前記電極部材の前記貫通開口の径が0.5mm以上2mm以下の範囲内である請求項1又は2に記載のカーボンナノチューブの形成方法。
- 前記カーボンナノチューブの成長を行う際に、被処理体を350℃以上530℃以下に加熱する請求項1から3のいずれか1項に記載のカーボンナノチューブの形成方法。
- 前記成膜装置は、前記処理容器内にプラズマ生成ガスを導入する第1のガス導入部と、前記処理容器内に前記カーボンナノチューブの原料ガスを導入する第2のガス導入部とが別々に設けられ、前記プラズマ生成ガスにより生成したプラズマ中に、前記第2のガス導入部から導入される前記カーボンナノチューブの原料ガスが混合された後で、該プラズマ中の活性種が、前記電極部材の貫通開口を通過するように構成されている請求項1から4のいずれか1項に記載のカーボンナノチューブの形成方法。
- 前記酸素プラズマ処理、前記水素プラズマ処理及び前記カーボンナノチューブを成長させる処理に利用するプラズマは、マイクロ波プラズマである請求項1から5のいずれか1項に記載のカーボンナノチューブの形成方法。
- 前記マイクロ波プラズマが、多数のマイクロ波放射孔を有する平面アンテナにより前記処理容器内に導入されたマイクロ波により励起されるものである請求項6に記載のカーボンナノチューブの形成方法。
- 被処理体の開口部が、ビアホール又は配線用溝である請求項1から7のいずれか1項に記載のカーボンナノチューブの形成方法。
- 前記開口部の幅が、10nm以上300nm以下である請求項1から8のいずれか1項に記載のカーボンナノチューブの形成方法。
- 前記酸素プラズマ処理、前記水素プラズマ処理及び前記カーボンナノチューブの成長を行う処理を、同一処理容器内で連続して行う請求項1から9のいずれか1項に記載のカーボンナノチューブの形成方法。
- 被処理体に対してプラズマ処理を行う処理空間を形成する処理容器と、
前記処理容器内で被処理体を載置する載置台と、
前記処理容器内にプラズマ生成ガスを導入する第1のガス導入部と、
前記処理容器内に、カーボンナノチューブの原料ガスを導入する第2のガス導入部と、
前記処理容器内で、前記載置台の上方に配置された多数の貫通開口を有する電極部材と、
前記電極部材に直流電圧を印加する電源と、
前記処理容器内を減圧排気する排気装置と、
を備え、
前記電極部材に直流電圧を印加しながら該電極部材よりも上方の空間で生成させたプラズマ中の活性種を、前記貫通開口を通過させて下方の被処理体へ向けて拡散させることにより、被処理体上にプラズマCVD法によってカーボンナノチューブを成長させるとともに、
前記第1のガス導入部は、前記プラズマCVD法によりカーボンナノチューブの成長を行う前の前処理として、被処理体に対して酸素プラズマ処理を行うための酸素含有ガス供給源に接続されており、
前記第2のガス導入部は、前記プラズマCVD法によりカーボンナノチューブの成長を行う前の前処理として、被処理体に対して水素プラズマ処理を行うための水素含有ガス供給源に接続されているカーボンナノチューブ成膜装置。 - 前記プラズマ生成ガスにより生成したプラズマ中に、前記カーボンナノチューブの原料ガスを混合するように、前記第1のガス導入部と前記第2のガス導入部が配置されており、
前記電極部材は、前記プラズマ中に前記カーボンナノチューブの原料ガスを混合する部位と、前記載置台との間に介在配置されている請求項11に記載のカーボンナノチューブ成膜装置。 - 前記処理容器の上部に配置されて前記処理空間を塞ぐ誘電体部材と、
前記誘電体部材の上方に設けられ、該誘電体部材を介して前記処理空間にマイクロ波を導入する平面アンテナと、
をさらに備えており、
前記第1のガス導入部は、前記誘電体部材の直下の空間にガスを導入するように配置されており、
前記第2のガス導入部は、前記第1のガス導入部より、前記載置台に近い位置で前記誘電体部材と前記載置台との間に介在して配置されており、
前記電極部材は、前記第2のガス導入部と前記載置台との間に介在して配置されている請求項11又は12に記載のカーボンナノチューブ成膜装置。 - 前記電極部材の前記貫通開口の径が0.5mm以上2mm以下の範囲内である請求項11から13のいずれか1項に記載のカーボンナノチューブ成膜装置。
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