JP2017533589A - ケイ素含有膜の堆積のための組成物及びそれを使用した方法 - Google Patents
ケイ素含有膜の堆積のための組成物及びそれを使用した方法 Download PDFInfo
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- JP2017533589A JP2017533589A JP2017522023A JP2017522023A JP2017533589A JP 2017533589 A JP2017533589 A JP 2017533589A JP 2017522023 A JP2017522023 A JP 2017522023A JP 2017522023 A JP2017522023 A JP 2017522023A JP 2017533589 A JP2017533589 A JP 2017533589A
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- 0 [*+]N([*+])[Si]N(*)[*+]=C Chemical compound [*+]N([*+])[Si]N(*)[*+]=C 0.000 description 3
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Abstract
Description
(a)以下、
(b)ある沸点を有する溶媒であって、溶媒の沸点と少なくとも1つの前駆体化合物の沸点の間の差が40℃以下である、溶媒とを含む、ケイ素含有材料を形成するための組成物であって、組成物が実質的にハライドイオンを含まない、組成物が提供される。本明細書で説明される組成物の幾つかの実施形態において、1つ又は複数の例示の溶媒としては、限定されないが、エーテル、3級アミン、アルキル炭化水素、芳香族炭化水素、3級アミノエーテル、及びそれらの組み合わせを挙げることができる。
a.反応器中に1つ又は複数の基材を設置する工程と、
b.以下、
c.パージガスで反応器をパージする工程と、
d.反応器中に窒素を含むプラズマ源を導入して、化学吸着層の少なくとも一部と反応させる工程であって、プラズマが約0.01〜約1.5W/cm2の範囲の電力密度で生成される、工程と、
e.任意選択で、不活性ガスで反応器をパージする工程、
を含み、工程b〜eが、窒化ケイ素膜の所望の厚さが得られるまで繰り返される方法、が提供される。
a.反応器中に基材を提供する工程と、
b.以下、
c.パージガスで反応器をパージする工程と、
d.反応器中に窒素を含むプラズマを導入して、化学吸着層の少なくとも一部と反応させ、少なくとも1つの反応部位を提供する工程と、
e.任意選択で、不活性ガスで反応器をパージする工程、
を含み、工程b〜eが、窒化ケイ素膜の所望の厚さが得られるまで繰り返される方法が提供される。
窒素保護の下、ドデカン中の2.5グラムのB(C6F5)3の溶液(0.2重量%(wt%)、9.8×10-6モル(mol))を、トリシリルアミン(500g、4.66モル(mol))を含有する1リットル(L)の丸底フラスコに加えた。シランガスが、ガスバブルとして急放出し始めた。反応溶液を、20℃の内部温度に保持しながらおよそ1時間撹拌した。反応溶液の質量が30%減少した後、4,4−ビピリジンを触媒毒として追加し(1.25g、8.00×10-3モル)、バブリングがすぐに止まった。冷却した反応混合物を2時間撹拌した後、揮発性物質を、−78℃に冷却した第2の1Lフラスコ中に真空供給した(25〜35℃/1Torr)。収集した粗液を、ガスクロマトグラフィー(GC)及びガスクロマトグラフィー−質量分析(GC−MS)で決定して、トリシリルアミンとN,N’−ジシリルトリシラザンとの約1:1の混合物になった。分別真空蒸留による浄化(58℃/50Torr)により、99%超の純度、沸点(b.p.)=135℃を持つ無色の液体として、164gのN,N’−ジシリルトリシラザンを得た。GC−MSは、以下の質量ピーク:181(M−1)、149、119、104、91、72を示した。
シリコンウエハを、13.56MHzの直接プラズマを持つシャワーヘッド設計を備えたCN−1反応器中に設置し、2torrのチャンバー圧力で300℃に加熱した。ビス(ジシリルアミノ)シランをケイ素前駆体として使用し、プラズマ源として窒素プラズマを使用した。ALDサイクルを、以下のプロセスパラメータを使用して行った。
a.反応器の準備とウエハの設置
チャンバー圧力:2torr
b.反応器へのケイ素前駆体の導入
窒素の全流量:1000標準立方センチメートル(sccm)
ケイ素前駆体パルス:1秒間
c.パージ
窒素の全流量:1000sccm
パージ時間:10秒間
d.プラズマの導入
窒素の全流量:1000sccm
プラズマ電力:125W
プラズマパルス:10秒間
e.パージ
窒素の全流量:1000sccm
パージ時間:10秒間
シリコンウエハを、13.56MHzの直接プラズマを持つシャワーヘッド設計を備えたCN−1反応器中に設置し、2torrのチャンバー圧力で300℃に加熱した。ビス(ジシリルアミノ)シランをケイ素前駆体として使用し、プラズマ源としてアンモニアプラズマを使用した。ALDサイクルを、以下のプロセスパラメータを使用して行った。
a.反応器の準備とウエハの設置
チャンバー圧力:2torr
b.反応器へのケイ素前駆体の導入
アルゴンの全流量:1000sccm
ケイ素前駆体パルス:0.2秒間
c.パージ
アルゴンの全流量:1000sccm
パージ時間:10秒間
d.プラズマの導入
アルゴンの全流量:1000sccm
アンモニアの全流量:500sccm
プラズマ電力:125W
プラズマパルス:10秒間
e.パージ
窒素の全流量:1000sccm
パージ時間:10秒間
シリコンウエハを、13.56MHzの直接プラズマを持つシャワーヘッド設計を備えたCN−1反応器中に設置し、2torrのチャンバー圧力で350℃に加熱した。ビス(ジシリルアミノ)シランをケイ素前駆体として使用した。ALDサイクルを、以下のプロセスパラメータを使用して行った。
a.反応器の準備とウエハの設置
チャンバー圧力:2torr
b.反応器へのケイ素前駆体の導入
アルゴンの全流量:1000sccm
ケイ素前駆体パルス:0.2秒間
c.パージ
アルゴンの全流量:1000sccm
パージ時間:10秒間
d.アンモニアの導入
アルゴンの全流量:1000sccm
アンモニアの全流量:500sccm
プラズマパルス:10秒間
e.パージ
アルゴンの全流量:1000sccm
パージ時間:10秒間
シリコンウエハを、13.56MHzの直接プラズマを持つシャワーヘッド設計を備えたCN−1反応器中に設置し、2torrのチャンバー圧力で300℃に加熱した。ビス(ジシリルアミノ)シランをケイ素前駆体として使用し、プラズマ源として窒素プラズマを使用した。ALDサイクルを、以下のプロセスパラメータを使用して行った。
a.反応器の準備とウエハの設置
チャンバー圧力:2torr
b.反応器へのケイ素前駆体の導入
窒素の全流量:1000sccm
ケイ素前駆体パルス:0.2秒間
c.パージ
窒素の全流量:1000sccm
パージ時間:10秒間
d.プラズマの導入
窒素の全流量:1000sccm
水素の全流量:500sccm
プラズマ電力:125W
プラズマパルス:10秒間
e.パージ
窒素の全流量:1000sccm
パージ時間:10秒間
シリコンウエハを、13.56MHzの直接プラズマを持つシャワーヘッド設計を備えたCN−1反応器中に設置し、2torrのチャンバー圧力で300℃に加熱した。ビス(ジシリルアミノ)シランをケイ素前駆体として使用し、プラズマ源として窒素プラズマを使用した。ALDサイクルを、以下のプロセスパラメータを使用して行った。
a.反応器の準備とウエハの設置
チャンバー圧力:2torr
b.反応器へのケイ素前駆体の導入
窒素の全流量:500sccm
水素の全流量:500sccm
ケイ素前駆体パルス:0.2秒間
c.パージ
窒素の全流量:500sccm
水素の全流量:500sccm
パージ時間:10秒間
d.プラズマの導入
窒素の全流量:500sccm
水素の全流量:500sccm
プラズマ電力:125W
プラズマパルス:10秒間
e.パージ
窒素の全流量:1000sccm
パージ時間:10秒間
Claims (10)
- 前記化合物が、ビス(ジシリルアミノ)シラン及びトリ(エチルシリル)アミンからなる群より選択される少なくとも1つを含む、請求項2に記載の組成物。
- 前記化合物がビス(ジシリルアミノ)シランを含む、請求項3に記載の組成物。
- エーテル、3級アミン、アルキル炭化水素、芳香族炭化水素、及び3級アミノエーテルからなる群より選択される少なくとも1つを含む、請求項2に記載の組成物。
- 前記溶媒が、オクタン、エチルシクロヘキサン、シクロオクタン、及びトルエンからなる群より選択される少なくとも1つを含む、請求項2に記載の組成物。
- 基材の表面の少なくとも一部に窒化ケイ素の膜を堆積するための方法であって、
反応器中に前記基材を設置する工程と、
以下の式IIA〜IID:
c.パージガスで前記反応器をパージする工程と、
d.前記反応器中に窒素を含むプラズマ源を導入して、前記化学吸着層の少なくとも一部と反応させる工程と、
e.任意選択で、不活性ガスで前記反応器をパージする工程と
を含み、工程b〜eが、前記窒化ケイ素の膜の所望の厚さが得られるまで繰り返される、方法。 - 前記プラズマ源が、窒素プラズマ、窒素/ヘリウムプラズマ、窒素/アルゴンプラズマ、アンモニアプラズマ、アンモニア/ヘリウムプラズマ、アンモニア/アルゴンプラズマ、ヘリウムプラズマ、アルゴンプラズマ、水素プラズマ、水素/ヘリウムプラズマ、水素/アルゴンプラズマ、有機アミンプラズマ、及びそれらの混合物からなる群より選択される、請求項7に記載の方法。
- 前記少なくとも1つのケイ素前駆体化合物がビス(ジシリルアミノ)シランを含む、請求項7に記載の方法。
- 工程dでのプラズマが、約0.01〜約1.5W/cm2の範囲の電力密度で生成される、請求項7に記載の方法。
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