JP6018149B2 - 窒化ケイ素膜被着方法 - Google Patents
窒化ケイ素膜被着方法 Download PDFInfo
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- JP6018149B2 JP6018149B2 JP2014204854A JP2014204854A JP6018149B2 JP 6018149 B2 JP6018149 B2 JP 6018149B2 JP 2014204854 A JP2014204854 A JP 2014204854A JP 2014204854 A JP2014204854 A JP 2014204854A JP 6018149 B2 JP6018149 B2 JP 6018149B2
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Description
この出願は、2013年10月3日に出願され、参照によりここに完全に記載されているかの如く組み入れられる、米国仮特許出願第61/886406号の利益を主張するものである。
a.反応器内に基材を供給する工程、
b.次の式I、II及びIIIにより表され、基材表面の少なくとも一部分で反応して化学吸着された層を提供する少なくとも1種のオルガノアミノシランを反応器へ導入する工程、
c.反応器をパージガスでパージする工程、
d.窒素と不活性ガスとを含むプラズマを反応器へ導入して上記の化学吸着された層の少なくとも一部分と反応させ、そして少なくとも1つの反応性部位を提供し、当該プラズマは約0.01〜約1.5W/cm2の範囲のパワー密度で発生させる工程、及び、
e.反応器を不活性ガスで任意選択的にパージする工程、
を含み、そして工程b〜eを窒化ケイ素膜の所望の厚さが得られるまで繰り返す、窒化ケイ素膜を形成する方法が提供される。一部の態様では、R1とR2は同一である。別の態様では、R1とR2は異なる。前述の又はその他の態様において、R1とR2は結合して環を形成してもよい。更なる態様では、R1とR2は環を形成するために結合はしない。
a.反応器内に基材を供給する工程、
b.ジイソプロピルアミノシラン、ジ−sec−ブチルアミノシラン、フェニルメチルアミノシラン、2,6−ジメチルピペリジノシラン、N−メチルシクロヘキシルアミノシラン、N−エチルシクロヘキシルアミノシラン、2−メチルピペリジノシラン、N−シリルデカヒドロキノリン、2,2,6,6−テトラメチルピペリジノシラン、2−(N−シリルメチルアミノ)ピリジン、N−t−ブチルジシラザン、N−t−ペンチルジシラザン、N−(3−メチル−2−ピリジル)ジシラザン、N−(2−メチルフェニル)ジシラザン、N−(2−エチルフェニル)ジシラザン、N−(2,4,6−トリメチルフェニル)ジシラザン、N−(2,6−ジイソプリピルフェニル)ジシラザン、ジイソブチルアミノジシラン、ジ−sec−ブチルアミノジシラン、2,6−ジメチルピペリジノシラン、ジイソプロピルアミノジシラン、N−メチルシクロヘキシルアミノジシラン、N−エチルシクロヘキシルアミノジシラン、フェニルメチルアミノジシラン、2−(N−ジシリルメチルアミノ)ピリジン、N−フェニルエチルジシラン、N−イソプロピルシクロヘキシルアミノジシラン、1,1−(N,N’−ジ−tert−ブチルエチレンジアミノ)ジシランからなる群より選ばれる少なくとも1種のオルガノアミノシラン前駆物質を反応器へ導入し、当該少なくとも1種のオルガノアミノシランが基材の表面の少なくとも一部分で反応して化学吸着された層を提供する工程、
c.窒素、希ガス及びそれらの組み合わせから選ばれる少なくとも1つを含むパージガスで反応器をパージする工程、
d.窒素含有プラズマを反応器へ導入して上記の化学吸着された層の少なくとも一部分と反応させ、そして少なくとも1つの反応性部位を提供し、当該プラズマは約0.01〜約1.5W/cm2の範囲のパワー密度で発生させる工程、及び、
e.反応器を不活性ガスで任意選択的にパージする工程、
を含み、そして工程b〜eを窒化ケイ素膜の所望の厚さが得られるまで繰り返す、窒化ケイ素膜を形成する方法が提供される。一部の態様では、R1とR2は同一である。別の態様では、R1とR2は異なる。前述の又はその他の態様において、R1とR2は結合して環を形成してもよい。更なる態様では、R1とR2は環を形成するために結合はしない。
a.反応器内に基材を供給する工程、
b.ジイソプロピルアミノシラン、ジ−sec−ブチルアミノシラン、フェニルメチルアミノシラン、2,6−ジメチルピペリジノシラン、N−メチルシクロヘキシルアミノシラン、N−エチルシクロヘキシルアミノシラン、N−イソプロピルシクロヘキシルアミノシラン、2−メチルピペリジノシラン、N−シリルデカヒドロキノリン、2,2,6,6−テトラメチルピペリジノシラン、2−(N−シリルメチルアミノ)ピリジン、N−t−ブチルジシラザン、N−t−ペンチルジシラザン、N−(3−メチル−2−ピリジル)ジシラザン、N−(2−メチルフェニル)ジシラザン、N−(2−エチルフェニル)ジシラザン、N−(2,4,6−トリメチルフェニル)ジシラザン、N−(2,6−ジイソプリピルフェニル)ジシラザン、ジイソプロピルアミノジシラン、ジイソブチルアミノジシラン、ジ−sec−ブチルアミノジシラン、2,6−ジメチルピペリジノシラン、N−メチルシクロヘキシルアミノジシラン、N−エチルシクロヘキシルアミノジシラン、フェニルメチルアミノジシラン、2−(N−ジシリルメチルアミノ)ピリジン、N−フェニルエチルジシラン、N−イソプロピルシクロヘキシルアミノジシラン、1,1−(N,N’−ジ−tert−ブチルエチレンジアミノ)ジシランからなる群より選ばれる少なくとも1種のオルガノアミノシラン前駆物質を反応器へ導入し、当該少なくとも1種のオルガノアミノシランが基材の表面の少なくとも一部分で反応して化学吸着された層を提供する工程、
c.窒素、希ガス及びそれらの組み合わせから選ばれる少なくとも1つを含むパージガスで反応器をパージする工程、
d.希ガスプラズマを反応器へ導入して上記の化学吸着された層の少なくとも一部分と反応させ、そして少なくとも1つの反応性部位を提供し、当該プラズマは約0.01〜約1.5W/cm2の範囲のパワー密度で発生させる工程、及び、
e.反応器を不活性ガスで任意選択的にパージする工程、
を含み、そして工程b〜eを窒化ケイ素膜の所望の厚さが得られるまで繰り返す、窒化ケイ素膜を形成する方法が提供される。
a.反応器内に基材を供給する工程、
b.次の式I、II及びIIIにより表される、基材の表面の少なくとも一部分で反応して化学吸着された層を提供する少なくとも1種のオルガノアミノシランを反応器へ導入する工程、
c.反応器をパージガスでパージする工程、
d.窒素と不活性ガスとを含むプラズマを反応器へ導入して上記の化学吸着された層の少なくとも一部分と反応させ、そして少なくとも1つの反応性部位を提供し、当該プラズマは約0.01〜約1.5W/cm2の範囲のパワー密度で発生させる工程、及び、
e.反応器を不活性ガスで任意選択的にパージする工程、
を含み、そして工程b〜eを窒化ケイ素膜の所望の厚さが得られるまで繰り返す、窒化ケイ素膜を形成する方法が提供される。一部の態様では、R1とR2は同一である。別の態様では、R1とR2は異なる。前述の又はその他の態様において、R1とR2は結合して環を形成してもよい。更なる態様では、R1とR2は環を形成するために結合はしない。所望により、水素を含むプラズマを工程dの前に入れて、オルガノアミノシランと表面との反応から発生する炭化水素を除去するのを促進することができる。水素を含むプラズマは、水素プラズマ、水素/ヘリウム、水素/アルゴンプラズマ、水素/ネオンプラズマ、及びそれらの混合物からなる群より選ばれる。
a.反応器内に基材を供給する工程、
b.ジイソプロピルアミノシラン、ジ−sec−ブチルアミノシラン、フェニルメチルアミノシラン、2,6−ジメチルピペリジノシラン、N−メチルシクロヘキシルアミノシラン、N−エチルシクロヘキシルアミノシラン、N−イソプロピルシクロヘキシルアミノシラン、2−メチルピペリジノシラン、N−シリルデカヒドロキノリン、2,2,6,6−テトラメチルピペリジノシラン、2−(N−シリルメチルアミノ)ピリジン、N−t−ブチルジシラザン、N−t−ペンチルジシラザン、N−(3−メチル−2−ピリジル)ジシラザン、N−(2−メチルフェニル)ジシラザン、N−(2−エチルフェニル)ジシラザン、N−(2,4,6−トリメチルフェニル)ジシラザン、N−(2,6−ジイソプリピルフェニル)ジシラザン、ジイソプロピルアミノジシラン、ジイソブチルアミノジシラン、ジ−sec−ブチルアミノジシラン、2,6−ジメチルピペリジノシラン、N−メチルシクロヘキシルアミノジシラン、N−エチルシクロヘキシルアミノジシラン、フェニルメチルアミノジシラン、2−(N−ジシリルメチルアミノ)ピリジン、N−フェニルエチルジシラン、N−イソプロピルシクロヘキシルアミノジシラン、1,1−(N,N’−ジ−tert−ブチルエチレンジアミノ)ジシランからなる群より選ばれる少なくとも1種の、基材の表面の少なくとも一部分で反応して化学吸着された層を提供するオルガノアミノシラン前駆物質を反応器へ導入する工程、
c.窒素、希ガス及びそれらの組み合わせから選ばれる少なくとも1種を含むパージガスで反応器をパージする工程、
d.窒素含有プラズマを反応器へ導入して上記の化学吸着された層の少なくとも一部分と反応させ、そして少なくとも1つの反応性部位を提供し、当該プラズマは約0.01〜約1.5W/cm2の範囲のパワー密度で発生させる工程、及び、
e.反応器を不活性ガスで任意選択的にパージする工程、
を含み、そして工程b〜eを窒化ケイ素膜の所望の厚さが得られるまで繰り返す、窒化ケイ素膜を形成する方法が提供される。
シリコンウエハをStellar 3000 PEALD反応器に入れ、約2Torrのチャンバー圧力で300℃の温度に加熱した。被着プロセスは表2に記載したとおりであり、下記の処理条件下で1000回繰り返した。
送給方法: 抽気
アルゴン流量: 300sccm
BTBASパルス: 1秒
アルゴン流量: 300sccm
パージ時間: 2秒
アルゴン流量: 300sccm
窒素流量: 400sccm
プラズマパワー: 500W(0.7W/cm2)
プラズマ時間: 5秒
アルゴン流量: 300sccm
パージ時間: 2秒
シリコンウエハをStellar 3000 PEALD反応器に入れ、約2Torrのチャンバー圧力で300℃の温度に加熱した。被着プロセスは比較例1で説明したのと同じであった。
シリコンウエハをStellar 3000 PEALD反応器に入れ、約2Torrのチャンバー圧力で300℃に加熱した。被着プロセスを表2に記載したとおりに行い、下記の処理条件下で1000回繰り返した。
送給方法: 抽気
アルゴン流量: 300sccm
BTBASパルス: 1秒
アルゴン流量: 300sccm
パージ時間: 2秒
アルゴン流量: 300sccm
アンモニア流量: 400sccm
プラズマパワー: 500W(0.7W/cm2)
プラズマ時間: 5秒
アルゴン流量: 300sccm
パージ時間: 2秒
シリコンウエハをStellar 3000 PEALD反応器に入れ、約2Torrのチャンバー圧力で300℃に加熱した。表2に記載した工程を使って被着プロセスを行い、1000回繰り返した。使用した処理条件は比較例1で説明したのと同じであるが、前駆物質パルスは0.5〜5秒で可変であった。被着速度と屈折率をまとめて下記の表3に示す。
表2に記載した工程を使って被着プロセスを行い、1000回繰り返した。使用した処理条件は比較例1で説明したのと同じであるが、前駆物質パルスは0.2〜5秒の範囲で可変であった。被着した全ての膜の被着速度と屈折率をまとめて下記の表5に示す。被着速度と屈折率の両方とも例1で示したDIPASと一致している。
シリコンウエハをStellar 3000 PEALD反応器に入れ、約2Torrのチャンバー圧力で300℃に加熱した。室温で200sccmのArキャリアガスを使って1Torrの蒸気圧でDSBASをチャンバーへ送給した。基材温度を300℃に設定した。ガスと前駆物質の配管温度をしかるべく調整して、反応器より前での凝縮を防止した。表2に記載した工程を使用しそして下記のプロセスパラメータを使用して、被着を行った。
アルゴン流量=300sccm
Si前駆物質パルス: 1秒
アルゴン流量: 300sccm
パージ時間: 5秒
アルゴン流量: 325〜425sccm
窒素流量: 75〜200sccm
Arと窒素の合計流量: 500sccm
チャンバー圧力: 2Torr
プラズマパワー: 500W(0.7W/cm2)
プラズマ時間: 5秒
アルゴン流量: 300sccm
チャンバー圧力: 2Torr
パージ時間: 0.5秒
シリコンウエハをStellar 3000 PEALD反応器に入れ、約2Torrのチャンバー圧力で300℃に加熱した。室温で200sccmのArキャリアガスを使用して、PMASを1Torrの蒸気圧でチャンバーへ送給した。基材温度を300℃に設定した。ガスと前駆物質の配管温度をしかるべく調整して、反応器の前での凝縮を防止した。表2に記載した工程を使用して例3で示したのと同様のプロセスパラメーターの下で被着を行った。プラズマ工程又は工程3の間、アルゴンと窒素の流量はそれぞれ300sccm及び200sccmであった。得られた膜のサイクル当たりの成長は0.18Å/サイクル、屈折率は1.95であった。この膜はまた、希HFウェットエッチ速度が0.53Å/secであった。
シリコンウエハをStellar 3000 PEALD反応器に入れ、約2Torrのチャンバー圧力で300℃に加熱した。室温で200sccmのArキャリアガスを使用して、PMADSを1Torrの蒸気圧でチャンバーへ送給した。基材温度を300℃に設定した。ガスと前駆物質の配管温度をしかるべく調整して、反応器の前での凝縮を防止した。表2に記載した工程と例3で示したプロセスパラメーターを使用して被着を行った。プラズマ工程又は工程3の間、アルゴンと窒素の流量はそれぞれ300sccm及び200sccmであった。得られた膜のサイクル当たりの成長は0.22Å/サイクル、屈折率は1.94であった。この膜はまた、希HFウェットエッチ速度が0.77Å/sec、炭素混入物が7.0原子%(at%)であった。
シリコンウエハをStellar 3000 PEALD反応器に入れ、約2Torrのチャンバー圧力で300℃に加熱した。抽気を利用してDIPADSを15Torrでチャンバーへ送給した。基材温度を300℃に設定した。ガスと前駆物質の配管温度をしかるべく調整して、反応器に到達する前の凝縮を防止した。表2に記載した工程を使用するとともに例3で示したプロセスパラメーターを使用して被着を行った。プラズマ工程又は工程3の間、アルゴンと窒素の流量はそれぞれ300sccm及び200sccmであった。得られた膜のサイクル当たりの成長は0.26Å/サイクル、屈折率は1.92であった。この膜はまた、希HFウェットエッチ速度が0.67Å/s、炭素混入物が4.9at%であった。
ASM Stellar PEALDツール内でモノアミノシラン前駆物質すなわちジ−sec−ブチルアミノシラン(DSBAS)と次のビスアミノシラン前駆物質すなわちビス(t−ブチルアミノ)シラン(BTBAS)及びビス(ジエチルアミノ)シラン(BDEAS)を使用して、膜を被着した。室温で200sccmのArキャリアガスを使用して、前駆物質を1Torrの蒸気圧でチャンバーへ送給した。基材温度を300℃に設定した。表2に示した処理工程を使用するとともに例3で説明した処理条件を使用し、そしてプラズマ工程又は工程3の間375sccmのArと125sccmのN2を使用して、被着を行った。
ASM Stellar PEALDツール内で前駆物質ジ−sec−ブチルアミノシラン(DSBAS)とビス(t−ブチルアミノ)シラン(BTBAS)とビス(ジエチルアミノ)シラン(BDEAS)を使用して、膜を被着した。室温で200sccmのArキャリアガスを使用して、前駆物質を1Torrの蒸気圧でチャンバーへそれぞれ送給した。基材温度を200℃に設定した。ガスと前駆物質の配管温度をしかるべく調整して、反応器の前での凝縮を防止した。上記以外は、例7で説明したとおりに被着を行った。被着した各膜の屈折率とサイクル当たりの成長速度を被着直後に測定した。それらを表8に提示する。
シリコンウエハをCN−1 PEALD反応器に入れ、2Torrのチャンバー圧力で300℃に加熱した。バブリング法を使ってDIPASを反応器へ送給した。ALDサイクルは表2に提示した処理工程から構成されるものであり、下記のプロセスパラメーターを使用した。
DIPAS: 50sccmのアルゴンが前駆物質容器を通過
アルゴン流量: 100sccm
Si前駆物質パルス: 1秒
アルゴンと窒素の合計流量500sccm
パージ時間: 10秒
Ar流量: 0〜500sccm
窒素流量: 0〜500sccm
Arと窒素の合計流量: 500sccm
プラズマパワー: 125W(0.7W/cm2)
プラズマ時間: 5秒
アルゴンと窒素の合計流量: 500sccm
パージ時間: 10秒
ジイソプロピルアミノシラン(DIPAS)とHe/N2プラズマからケイ素含有膜を被着させた。プロセスパラメーターとALDの工程は、Arガスの代わりにヘリウムを使用したことを除き、例9で説明したのと同じであった。表10は、He/N2プラズマを使用して被着した膜では希HFウェットエッチ抵抗(WER)が非常に小さいことを示している。試験した全てのHe/N2比において、膜はWER>22.1nm/minであり、屈折率が1.85未満である。
300℃のスクリーニングPEALD反応器と2Torrのチャンバー圧力を使用し、下記の詳細なプロセスパラメーターを用いて、ジイソプロピルアミノシラン(DIPAS)とN2のみのプラズマとからSi含有膜を被着させた。
送給方法: 抽気
Si前駆物質パルス: 1秒
N2流量: 500sccm
N2流量: 500sccm
パージ時間: 10秒
窒素流量: 500sccm
プラズマパワー: 125W(0.7W/cm2)
プラズマ時間: 5秒
4.プラズマをパージ
窒素流量: 500sccm
パージ時間: 10秒
Claims (8)
- 基材の少なくとも一表面上に窒化ケイ素膜を形成する方法であって、
a.反応器内に基材を供給する工程、
b.ジイソプロピルアミノシラン、ジ−sec−ブチルアミノシラン、フェニルメチルアミノシラン、2,6−ジメチルピペリジノシラン、N−メチルシクロヘキシルアミノシラン、N−エチルシクロヘキシルアミノシラン、N−イソプロピルシクロヘキシルアミノシラン、2−メチルピペリジノシラン、N−シリルデカヒドロキノリン、2,2,6,6−テトラメチルピペリジノシラン、2−(N−シリルメチルアミノ)ピリジン、N−t−ブチルジシラザン、N−t−ペンチルジシラザン、N−(3−メチル−2−ピリジル)ジシラザン、N−(2−メチルフェニル)ジシラザン、N−(2−エチルフェニル)ジシラザン、N−(2,4,6−トリメチルフェニル)ジシラザン、N−(2,6−ジイソプリピルフェニル)ジシラザン、ジイソプロピルアミノジシラン、ジイソブチルアミノジシラン、ジ−sec−ブチルアミノジシラン、2,6−ジメチルピペリジノシラン、N−メチルシクロヘキシルアミノジシラン、N−エチルシクロヘキシルアミノジシラン、フェニルメチルアミノジシラン、2−(N−ジシリルメチルアミノ)ピリジン、N−フェニルエチルジシラン、N−イソプロピルシクロヘキシルアミノジシラン、1,1−(N,N’−ジ−tert−ブチルエチレンジアミノ)ジシランからなる群より選ばれる、基材の表面の少なくとも一部分で反応して化学吸着された層を提供する少なくとも1種のオルガノアミノシラン前駆物質を反応器へ導入する工程、
c.窒素、希ガス及びそれらの組み合わせから選ばれる少なくとも1つを含むパージガスで反応器をパージする工程、
d.窒素含有プラズマを反応器へ導入して上記の化学吸着された層の少なくとも一部分と反応させ、そして少なくとも1つの反応性部位を提供し、当該プラズマは約0.01〜約1.5W/cm2の範囲のパワー密度で発生させる工程、及び、
e.反応器を不活性ガスで任意選択的にパージする工程、
を含み、
前記オルガノアミノシランと前記表面との反応から発生した炭化水素を除去するのを促進するため工程dの前に水素を含むプラズマを入れ、
そして工程b〜eを窒化ケイ素膜の所望の厚さが得られるまで繰り返す、窒化ケイ素膜形成方法。 - 前記窒化ケイ素膜が2.4g/cc以上の密度を有する、請求項1記載の方法。
- 当該方法がプラズマ支援化学気相堆積及びプラズマ支援サイクリック化学気相堆積から選ばれる少なくとも1つからなる群より選ばれる気相堆積法である、請求項1記載の方法。
- 当該方法を約400℃以下の温度で実施する、請求項1記載の方法。
- 当該方法を約300℃以下の温度で実施する、請求項1記載の方法。
- 前記窒素含有プラズマを、窒素プラズマ、アルゴン/窒素プラズマ、ネオン/窒素プラズマ、クリプトン/窒素プラズマ、キセノン/窒素プラズマ、及びそれらの組み合わせからなる群より選択する、請求項1記載の方法。
- 工程bが前記反応器へ希ガスを導入することを更に含む、請求項1記載の方法。
- 前記水素を含むプラズマを、水素プラズマ、水素/ヘリウム、水素/アルゴンプラズマ、水素/ネオンプラズマ及びそれらの混合物からなる群より選択する、請求項1記載の方法。
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CN104831254A (zh) | 2015-08-12 |
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KR102478568B1 (ko) | 2022-12-15 |
US9905415B2 (en) | 2018-02-27 |
KR102281913B1 (ko) | 2021-07-23 |
KR20150040234A (ko) | 2015-04-14 |
CN104831254B (zh) | 2019-04-12 |
TWI565822B (zh) | 2017-01-11 |
KR20160132804A (ko) | 2016-11-21 |
TW201514332A (zh) | 2015-04-16 |
US20150099375A1 (en) | 2015-04-09 |
EP2857552A2 (en) | 2015-04-08 |
KR20170018872A (ko) | 2017-02-20 |
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