JP2017078223A - Ｐｅａｌｄによりトレンチに誘電体膜を堆積する方法 - Google Patents

Ｐｅａｌｄによりトレンチに誘電体膜を堆積する方法 Download PDF

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JP2017078223A
JP2017078223A JP2016200539A JP2016200539A JP2017078223A JP 2017078223 A JP2017078223 A JP 2017078223A JP 2016200539 A JP2016200539 A JP 2016200539A JP 2016200539 A JP2016200539 A JP 2016200539A JP 2017078223 A JP2017078223 A JP 2017078223A
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秀美 末盛
Hidemi Suemori
秀美 末盛
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Abstract

【課題】プラズマエンハンスト原子層堆積（ＰＥＡＬＤ）によりトレンチに誘電体膜を堆積する方法を提供する。【解決手段】プラズマエンハンスト原子層堆積（ＰＥＡＬＤ）によりトレンチに誘電体膜を堆積する方法は、基板の上面に堆積する膜のウェットエッチング速度が、実質的にトレンチの側壁に堆積する膜のウェットエッチング速度以上である条件下で、ＰＥＡＬＤにより基板のトレンチに誘電体膜を堆積するステップを含み、反応空間に供給される前駆体は、官能基として−Ｎ（ＣＨ３）２を有する。【選択図】図１Ａ

Description

本発明は、概してプラズマエンハンスト原子層堆積（ｐｌａｓｍａ−ｅｎｈａｎｃｅｄ ａｔｏｍｉｃ ｌａｙｅｒ ｄｅｐｏｓｉｔｉｏｎ（ＰＥＡＬＤ））により基板のトレンチに誘電体膜を堆積する方法に関するものである。
ＰＥＡＬＤでは、基板のトレンチの側壁は、基板の上面よりもイオン衝突が少ないため、側壁での表面反応は、上面での表面反応よりも少なくなり、側壁での膜のウェットエッチング速度が上面での膜のウェットエッチング速度とは異なる（より速い）という問題を生じる。
従来、処理温度等を増加させることにより、側壁に堆積される誘電体膜の品質（例えば、密度、硬さ）は、側壁でのエッチング速度が低減されるように改善されている。しかし、改善は部分的であり、側壁と上面との異なるエッチング速度の課題は、十分に解決されていない。
関連する分野に含まれる課題及び解決手段の説明は、単に本発明の文脈を提供する目的で本開示に含まれているものであり、説明のいずれか又は全てが、本発明がなされたときに既知であることを認めるものとして受け取られるべきではない。
本発明の一部の実施形態では、基板のトレンチの側壁での誘電体膜の品質を改善することに代えて、基板の上面での誘電体膜の品質を劣化させることによって、側壁及び上面での膜のエッチング速度を実質的に一致させる。
一部の実施形態は、官能基として−Ｎ（ＣＨ３）２を有する前駆体を用いるＰＥＡＬＤにより、トレンチを有する基板上の誘電体膜の堆積プロセスにおいて、ＲＦパワー等のようなプロセスパラメータを制御することによって、基板のトレンチの側壁での膜の量と、基板の上面での膜の量とを実質的に等しくする方法を提供する。一部の実施形態では、上面での膜のエッチング速度は、ＲＦパワーの増加により増加され、上面上に堆積される膜の品質が低下され、それにより、側壁と上面とのエッチング速度の差を低減する。一部の実施形態では、上面での膜における不純物（例えば、窒素）の量は、堆積プロセスを制御することによって増加される。膜のエッチング速度は、膜の不純物の量に関連し、不純物の量を増加させることにより、エッチング速度を増加させることができる。不純物の量は、例えば、ＲＦパワーを調整することにより制御されることができる。堆積プロセスを制御することによって、側壁での膜における不純物の量と、上面での膜における不純物の量とを実質的に等しくすることにより、側壁と上面とのエッチング速度の差を低減する。
本発明の態様及び関連分野に対して達成された利点を要約する目的のために、本発明の特定の目的及び利点が本開示に記載されている。もちろん、全てのこのような目的又は利点は本発明の任意の特定の実施形態に従って達成され得ることを必ずしも必要としないことは理解される。したがって、例えば、当業者は、本明細書に教示又は示唆され得るような他の目的又は利点を必ずしも達成しなくても、本明細書に教示されている１つの利点又は１群の利点を達成又は最適化するように本発明が具現化され得るか又は実施され得ることを認識するであろう。
本発明のさらなる態様、特徴及び利点は以下の詳細な説明から明らかになるであろう。
本発明のこれら及び他の特徴を好ましい実施形態の図面を参照して記載するが、それらは本発明を例示するためであり、本発明を限定するものではない。図面は、説明の都合上、非常に簡略化されており、必ずしも縮尺通りではない。
図１Ａは、本発明の一実施形態で使用可能な誘電体膜を堆積するＰＥＡＬＤ（ｐｌａｓｍａ−ｅｎｈａｎｃｅｄ ａｔｏｍｉｃ ｌａｙｅｒ ｄｅｐｏｓｉｔｉｏｎ）装置の概略図である。 図１Ｂは、本発明の一実施形態で使用可能なフロー・パスシステム（ｆｌｏｗ−ｐａｓｓ ｓｙｓｔｅｍ（ＦＰＳ））を用いた前駆体供給システムの概略図である。 図２は、本発明の一実施形態に係るＰＥＡＬＤ処理シーケンスを示す。 図３Ａは、本発明の一実施形態に係る膜の堆積に用いられる、膜のＮ濃度と、ＲＦパワーとの関係を示すグラフである。 図３Ｂは、本発明の一実施形態に係る膜の堆積に用いられる、酸化膜のウェットエッチング速度に対する堆積された膜のウェットエッチング速度と、ＲＦパワーとの関係を示すグラフである。 図４は、本発明の一実施形態に係る膜の堆積に用いられる、熱酸化膜のウェットエッチング速度に対する側壁及び上面での堆積された膜のウェットエッチング速度（任意の単位）と、ＲＦパワーとの関係を示すグラフである。 図５は、比較例に基づいて形成されたコンフォーマルな誘電体膜の断面図の走査型透過電子顕微鏡（Ｓｃａｎｎｉｎｇ ｔｒａｎｓｍｉｓｓｉｏｎ ｅｌｅｃｔｒｏｎ ｍｉｃｒｏｓｃｏｐｙ（ＳＴＥＭ））写真を示し、ここで、（ａ）は堆積された膜を示し、（ｂ）はウェットエッチング後の膜を示す。 図６は、本発明の実施形態に基づいて形成されたコンフォーマルな誘電体膜の断面図の走査型透過電子顕微鏡（Ｓｃａｎｎｉｎｇ ｔｒａｎｓｍｉｓｓｉｏｎ ｅｌｅｃｔｒｏｎ ｍｉｃｒｏｓｃｏｐｙ（ＳＴＥＭ））写真を示し、ここで、（ａ）は堆積された膜を示し、（ｂ）はウェットエッチング後の膜を示す。
本開示において、「ガス」は、蒸発した固体及び／又は液体を含んでもよく、単一のガス又はガスの混合物により構成されてもよい。同様に、「一つ」の物品は、一つの種類又は複数の種類を含む属性を指す。本開示では、シャワーヘッドを通じて反応チャンバへ導入されるプロセスガスは、前駆体及び反応ガスを含むか、実質的に前駆体及び反応ガスからなるか、又は前駆体及び反応ガスからなってもよい。反応ガスは、ＲＦパワーが反応ガスに印加されたときに前駆体を酸化するガスを含む。反応ガスは、ＲＦパワーなしでは前駆体と反応しない場合、反応空間に連続的に導入されうる。前駆体は、例えば希ガスのようなキャリアガスと共に導入されうる。プロセスガス以外のガス、すなわち、シャワーヘッドを通過せずに導入されるガスは、例えば反応空間をシールするために用いられてもよく、例えば希ガスのようなシールガスを含む。一部の実施形態では、「膜」は、ターゲットとなる表面もしくは対象となる表面全体を覆うためにピンホールを有さずに実質的に厚さ方向に垂直な方向に連続して延びる層、又はターゲットとなる表面もしくは対象となる表面を単に覆う層を指す。膜は、特定の性質を有する別個の単一の膜もしくは層又は複数の膜もしくは層により構成されてもよく、隣接する膜又は層の間の境界は明確であってもよく、又は明確でなくてもよく、物理的、化学的及び／もしくは任意の他の特性、形成プロセスもしくは順序、ならびに／又は隣接する膜もしくは層の機能もしくは目的に基づいて規定されてもよい。更に、本開示において、任意の２つの数の変数は、その変数の実行可能な範囲を構成でき、実行可能な範囲は通常作業に基づいて決定でき、示された任意の範囲はエンドポイントを含んでいてもよく、又は除外していてもよい。更に、示された変数の任意の値（それらが「約」と共に示されているか否かに関わらず）は、正確な値又はおおよその値を指し、同値を含んでもよく、一部の実施形態において、平均値、中央値、代表値、多数値などを指してもよい。用語「構成される」及び「有する」は、独立して、一部の実施形態における「典型的に又は広義に備える」、「備える」、「実質的に〜からなる」、又は「からなる」を指す。
条件及び／又は構造が特定されていない本開示において、当業者は、通常の実験として、本開示を考慮してそのような条件及び／又は構造を容易に得ることができる。
開示された実施形態の全てにおいて、一実施形態において使用されている任意の要素は、意図される目的のために本明細書に明確、必然的又は本質的に開示されている要素を含む、要素と等価の任意の要素と置き換えられてもよい。更に、本発明は装置及び方法に同様に適用されてもよい。
本開示において、任意の定義された意味は、一部の実施形態において、通常及び慣例の意味を必ずしも除外しているわけではない。
一部の実施形態では、用語「前駆体」は、一般的に、別の化合物を生成する化学反応に関与する化合物を指し、特に、膜のマトリクス又は膜の主要骨格を構成する化合物を指す。一方で、用語「反応物質」は、前駆体を活性化する、前駆体を改質する、又は前駆体の反応に触媒作用を及ぼす化合物を指す。
誘電体膜は、約１０から約１００、典型的には約５０から約６０の誘電定数を有する、酸化チタニウム又は多元素材料等で構成される金属酸化膜を含むが、これに限定されない。一部の実施形態では、誘電体膜は、プラズマエンハンストＡＬＤ又は他のプラズマアシストされた周期的な堆積方法によって、トレンチ、ビア又は側壁及び底面を含む他の凹部（まとめて「トレンチ」と呼ぶ）に形成される。トレンチは、約１０ｎｍから約１，０００ｎｍ、典型的には約１００ｎｍから約５００ｎｍの深さを有し、約１から約１０、典型的には約２から約３のアスペクト比を有する。堆積された誘電体膜の厚さは、約２ｎｍから約５００ｎｍ、典型的には約１０ｎｍから約１００ｎｍ、より典型的には約１５ｎｍから約３０ｎｍの範囲内にあってもよい（所望の膜厚は、膜の用途及び目的等に応じて適切とみなされるように選択されることができる）。
実施形態は、好ましい実施形態に対して説明される。しかし、本発明は、好ましい実施形態に限定されない。
一実施形態では、プラズマエンハンスト原子層堆積（ＰＥＡＬＤ）によりトレンチに誘電体膜を堆積する方法は、（ｉ）ＰＥＡＬＤにより誘電体膜が基板のトレンチに堆積される反応空間に印加されるＲＦパワーと、前記トレンチの側壁に堆積される膜の一部のウェットエッチング速度との第１の関係、及び前記ＲＦパワーと、前記基板の上面に堆積される膜の一部のウェットエッチング速度との第２の関係を決定するステップであって、前記反応空間に供給される前駆体は、官能基として−Ｎ（ＣＨ３）２を有する、ステップと、（ｉｉ）前記トレンチの前記側壁に堆積される膜の一部の第１のウェットエッチング速度及び前記基板の前記上面に堆積される膜の一部の第２のウェットエッチング速度に対応するＲＦパワーを決定するステップであって、前記第２のウェットエッチング速度は、ステップ（ｉ）での前記第１の関係及び前記第２の関係に基づいて実質的に前記第１のウェットエッチング速度以上である、ステップと、（ｉｉｉ）前記ＲＦパワーがステップ（ｉｉ）で決定された前記第１の関係及び前記第２の関係で用いられた条件と等しい条件下でＰＥＡＬＤにより基板のトレンチに誘電体膜を堆積するステップと、を備える。
本開示では、「実質的に同一」、「実質的に等しい」等は、重要でない差、又は例えば、１０％未満、５％未満、１％未満又は一部の実施形態におけるその任意の範囲（典型的には差が±５％）等の差のような当業者によって認識される差を指す。また、本開示では、「実質的に高い」、「実質的に異なる」等は、材料の差、又は例えば、少なくとも５％、１０％、２０％、３０％、４０％、５０％、６０％、７０％、８０％又は一部の実施形態におけるその任意の範囲の差のような当業者によって認識される差を指す。
一部の実施形態では、基板の上面に堆積される膜のウェットエッチング速度は、膜の堆積のために用いられるＲＦパワーの関数として変化し、官能基として−Ｎ（ＣＨ３）２を有する前駆体が用いられるとき、膜のウェットエッチング速度は、ＲＦパワーが増加すると、一箇所の頂点を有する下向きの放物線に沿って、変化する。つまり、ＲＦパワーが相対的に弱いときには、ＲＦパワーが増加すると、ウェットエッチング速度は減少する、すなわち、堆積する膜の品質が改善される。しかし、ＲＦパワーが更に増加するとき、より多くのプラズマが上面に到達し、不純物濃度も増加し始める。一般的に、ウェットエッチング速度の変化は、不純物濃度の変化と相関する。その結果、ウェットエッチング速度は、最小値（最も低い頂点）に到達後に、増加し始める。最も低い頂点で得られる上面での膜の品質は、最も高くなるように見える。しかし、上面での膜の品質が、最も低い頂点で最も高いとき、側壁での膜の品質は、高くない、すなわち、側壁での膜のウェットエッチング速度は、相対的に高い。プラズマが側壁には容易に到達しないため、側壁での膜の品質は、上面での膜の品質とは対照的に、ＲＦパワーの強度にあまり影響されない。一部の実施形態では、側壁での膜のウェットエッチング速度は、ＲＦパワーが増加すると、徐々に減少する。よって、側壁での膜のウェットエッチング速度は、ＲＦパワーが相対的に低いとき、ＲＦパワーが増加すると、上面での膜のウェットエッチング速度の最も低い頂点の後のある値で、上面での膜のウェットエッチング速度よりも高くなるが、上面での膜のウェットエッチング速度が増加し続ける一方で、側壁での膜のウェットエッチング速度は、徐々に減少するので、上面での膜のウェットエッチング速度及び側壁での膜のウェットエッチング速度は、ほぼ等しくなる（上面での膜のエッチング速度と、ＲＦパワーとの関係を表す線分、及び側壁での膜のウェットエッチング速度と、ＲＦパワーとの関係を表す線分は、交差する。）。
一部の実施形態では、膜を堆積するためのＲＦパワーを調整することのみ（他のプロセスパラメータを変更しない）により、第２のウェットエッチング速度（すなわち、上面に堆積される膜のウェットエッチング速度）は、第１のウェットエッチング速度（すなわち、側壁に堆積される膜のウェットエッチング速度）と実質的に等しい又はそれ以上となり、ウェットエッチング後の膜のコンフォーマリティを改善することができる。一部の実施形態では、ウェットエッチング後の膜のコンフォーマリティは、約９０％から約１１０％、理想的には約９５％から約１００％の範囲内にある。コンフォーマリティは、基板の上面での膜の厚さに対する、基板のトレンチの側壁（又は底面）での膜の厚さの比率として定義される。第１のウェットエッチング速度は、基板に堆積される膜のコンフォーマリティに応じて選択される。コンフォーマリティが約１００％である場合、第１及び第２のウェットエッチング速度は、実質的に等しく、ウェットエッチング後の膜のコンフォーマリティは、約１００％のままである。一部の実施形態では、堆積された膜のコンフォーマリティは、約８０％から約１００％の範囲内にある。従来、ウェットエッチング後のコンフォーマリティは、堆積された膜のコンフォーマリティよりも約５％から約１０％低い。これに対して、本発明の一部の実施形態では、ウェットエッチング後のコンフォーマリティは、堆積された膜のコンフォーマリティよりも約５％から約１５％（典型的には１０％付近）高い。一部の実施形態では、基板のトレンチの側壁での膜の品質の改善に代えて、基板の上面での膜の品質を劣化することにより、上記のことを実現する。
一部の実施形態では、前駆体は、ジメチルアミド金属錯体である。一部の実施形態では、金属錯体における金属は、チタニウムである。例えば、ゲルマニウムのような他の金属も用いられうる。一部の実施形態では、前駆体は、テトラキス（ジメチルアミド）チタニウム、テトラキス（ジメチルアミド）ゲルマニウムからなる群から選択された１以上の化合物である。
一部の実施形態では、ステップ（ｉｉｉ）で用いられるＲＦパワー（すなわち、ＲＦパワー決定ステップ）は、基板の面積当たり、約０．０２Ｗ／ｃｍ３から約１．４Ｗ／ｃｍ３、典型的には約０．０７Ｗ／ｃｍ３から約０．７Ｗ／ｃｍ３、より典型的には約０．３Ｗ／ｃｍ３から約０．４Ｗ／ｃｍ３の範囲内にある。
本開示では、ウェットエッチング速度は、以下の表１に示される条件下で膜をウェットエッチングすることによって評価される。
上記では、測定ステップは、以下のようになる。（１）膜が堆積された基板を、５×５ｃｍのサイズのピースにカットする、（２）分光エリプソメトリーによって膜の厚さを測定する、（３）基板のピースを、１：１００のフッ化水素酸濃度を有する溶液に５分間浸漬する、（４）純水を用いて基板のピースを完全に洗浄し、基板のピースをブロワーで乾燥する、（５）分光エリプソメトリーによって膜の厚さを測定し、ステップ（２）で測定した厚さとステップ（５）で測定した膜の厚さとの差と、ステップ（２）で測定した膜の厚さとの比として定義されるウェットエッチング速度を算出する。また、熱酸化膜（ｔｈｅｒｍａｌ ｏｘｉｄｅ ｆｉｌｍ（ＴＯＸ））が堆積された基板は、上記と同一のステップにさらされ、ＴＯＸのウェットエッチング速度に対する膜のウェットエッチング速度の比を算出する。
一部の実施形態では、ウェットエッチング速度の程度が膜の不純物濃度に関連するため、本方法は、以下のような不純物濃度に基づいて行われうる。（ａ）第１の条件下で膜を堆積し、上面での膜の不純物濃度（Ｔ１）及び側壁での膜の不純物濃度（Ｓ１）の不純物濃度を測定する、ここで、Ｔ１＜Ｓ１である、（ｂ）例えばＲＦパワー等のようなプロセスパラメータが第１の条件から変更された（例えば、ＲＦパワーが増加している）第２の条件下で膜を堆積し、上面での膜の不純物濃度（Ｔ２）及び側壁での膜の不純物濃度（Ｓ２）の不純物濃度を測定する、ここで、Ｔ１＜Ｔ２かつＳ１＞Ｓ２である、（ｃ）Ｔ２≒Ｓ２となる最適条件が求められるまでステップ（ｂ）を繰り返す（≒は、実質的に同一であることを表す）。
一部の実施形態では、以下の表２で示される条件下でＰＥＡＬＤによって膜を堆積する。
図２は、本発明の一実施形態に係るＰＥＡＬＤ処理シーケンスを示す。本開示では、各横幅は、必ずしも実際の時間の長さを表さず、各縦のラインの上昇したレベルは、ＯＮ状態を表し、各縦のラインの下降したレベルは、ＯＦＦ状態を表す。堆積サイクルは、前駆体を反応ゾーンに供給するステップと、反応ゾーンをパージするステップと、ＲＦパワーを反応ゾーンに印加するステップと、この順序で反応ゾーンをパージするステップと、を含み、パージ／キャリアガスは、堆積サイクルのステップ全体を通じて反応ゾーンに連続的に供給され、堆積用の反応ガスは、堆積サイクルのステップ全体を通じて反応ゾーンに連続的に供給される。堆積サイクルでは、前駆体を供給するステップ、反応ゾーンをパージするステップ、ＲＦパワーを反応ゾーンに印加するステップ、及び反応ゾーンをパージするステップは、目標とする膜厚並びに目標とする膜の組成及び品質に応じてｐ回（ｐは、１５０から３５０、典型的には２５０から３００の整数である）繰り返されることができるが、繰り返すことは必ずしも必要ではない。
本開示では、用語「連続的」は、実施形態に応じて、真空破壊がないこと、大気に曝されないこと、ｉｎ−ｓｉｔｕ処理としてチャンバを開かないこと、シーケンスの１つのステップとして中断をしないこと、及びメインプロセス条件を変更しないことのうちの少なくとも１つを指す。一部の実施形態では、ステップ間の遅延、又は重要でない又は実体のない他のステップ等のような補助的なステップは、ステップとしてカウントせず、よって、用語「連続的」は、介在する補助的なステップを排除するものではない。
図２に示されるシーケンスでは、前駆体は、連続的に供給されるキャリアガスを用いてパルスで供給される。これは、キャリアガスラインには、前駆体リザーバー（ボトル）を有する迂回ラインが設けられ、メインライン及び迂回ラインが切り替えられ、キャリアガスのみが反応チャンバに供給されることが意図されるときに、迂回ラインが閉じられ、一方で、キャリアガス及び前駆体ガスが反応チャンバに供給されることが意図されるときに、メインラインが閉じられ、かつキャリアガスが迂回ラインを通じて流れ、前駆体ガスと共にボトルから流れ出るフロー・パスシステム（ｆｌｏｗ−ｐａｓｓ ｓｙｓｔｅｍ（ＦＰＳ））を用いて実現されうる。このようにして、キャリアガスは、反応チャンバに連続的に流れ込み、メインラインと迂回ラインとを切り替えることによってパルスで前駆体ガスを運ぶことができる。図１Ｂは、本発明の実施形態に係るフロー・パスシステム（ＦＰＳ）を用いた前駆体供給システムを示す（黒いバルブは、バルブが閉じられていることを示す）。図１Ｂの（ａ）に示されるように、初めに、前駆体を反応チャンバ（図示せず）に供給するとき、例えばＡｒ（又はＨｅ）のようなキャリアガスは、バルブｂ及びｃを有するガスラインを通じて流れ、そして、ボトル（リザーバー）２０に侵入する。キャリアガスは、ボトル２０内の蒸気圧に対応する量で前駆体ガスを運びつつ、ボトル２０から流れ出て、バルブｆ及びｅを有するガスラインを通じて流れ、そして、前駆体と共に反応チャンバへ供給される。上記では、バルブａ及びｄは、閉じられている。図１Ｂの（ｂ）に示されるように、キャリアガス（希ガス）のみを反応チャンバへ供給するとき、キャリアガスは、ボトル２０をバイパスする一方で、バルブを有するガスラインを通じて流れる。上記では、バルブｂ、ｃ、ｄ、ｅ及びｆは、閉じられている。
前駆体は、キャリアガスを用いて提供されてもよい。ＡＬＤが自己制限型吸着反応プロセスであるため、堆積された前駆体分子の数は、反応表面サイトの数によって決定され、飽和後の前駆体露出とは独立しており、前駆体の供給は、反応表面サイトが飽和され、それによって、サイクル毎に行われる。堆積用のプラズマは、例えば、堆積サイクルを通じて連続的に流れるアンモニアガス中に、ｉｎ ｓｉｔｕで生成されてもよい。他の実施形態では、プラズマは、リモート生成され、反応チャンバに提供されてもよい。
上述されたように、各堆積サイクルの各パルス又は各段階は、自己制限型であることが好ましい。影響を受けやすい構造表面を飽和させるために、各段階において過剰な反応物質が供給される。表面飽和は、全ての利用可能な反応サイト（例えば、物理的な大きさ又は「立体障害」の制限を受ける）の反応物質の占有を確実にし、よって、優れたステップカバレッジを確実にする。一部の実施形態では、完全な飽和がなされず、単層未満が基板表面に吸着されるように、反応物質の１以上のパルス時間を低減することができる。
プロセスサイクルは、例えば、図１Ａに示される装置を含む適切な装置を用いて行われうる。図１Ａは、本発明の一部の実施形態で使用可能な、以下に示されるシーケンスを行うようにプログラムされた制御装置と連動することが望ましいＰＥＡＬＤ装置の概略図である。この図では、反応チャンバ３の内部１１（反応ゾーン）で互いに平行かつ対向している一対の導電性平板電極４，２を設け、ＨＲＦパワー（１３．５６ＭＨｚ又は２７ＭＨｚ）２０を一方に印加し、他方を電気的にグランド１２にすることによって、電極間にプラズマを励起する。温度レギュレータが下部ステージ２（下部電極）に設けられ、その上に配置される基板１の温度は、所定の温度で一定に維持される。上部電極４は、同様に、シャワープレートとして機能し、反応ガス（及び希ガス）及び前駆体ガスは、それぞれガスライン２１及びガスライン２２並びにシャワープレート４を通じて、反応チャンバ３へ導入される。また、反応チャンバ３には、排気ライン７を有する円形ダクト１３が設けられ、円形ダクト１３を通じて、反応チャンバ３の内部１１におけるガスを排気する。また、反応チャンバ３の下に配置される搬送チャンバ５には、搬送チャンバ５の内部１６（搬送ゾーン）を介して反応チャンバ３の内部１１にシールガスを導入するためにシールガスライン２４が設けられ、反応ゾーンと搬送ゾーンとを隔てるためのセパレーションプレート１４が設けられる（それを通じてウェーハが搬送チャンバ５へ搬送される又は搬送チャンバ５から搬送されるゲートバルブは、この図から省略されている）。搬送チャンバには、排気ライン６も設けられる。一部の実施形態では、多元素膜の堆積及び表面処理は、同一の反応空間で行われ、全てのステップは、大気又は他の酸素を含む雰囲気へ基板を露出することなく、連続的に行われうる。一部の実施形態では、リモートプラズマユニットは、ガスを励起するために用いられうる。
一部の実施形態では、図１Ａに示される装置では、（前述された）図１Ｂに示される不活性ガスの流れと前駆体ガスの流れとを切り替えるシステムは、反応チャンバの圧力を実質的に変動せずに、パルスで前駆体ガスを導入するために用いられうる。
一部の実施形態では、デュアルチャンバリアクタ（互いに近くに配置されるウェーハを処理するための２つのセクション又はコンパートメント）を用いることができ、反応ガス及び希ガスは、共有ラインを通じて供給される一方で、前駆体ガスは、共有されないラインを通じて供給される。
前記装置は、本明細書の他の箇所に記載される堆積及びリアクタ洗浄処理を行わせるようにプログラムされる又は構成される１以上のコントローラ（図示せず）を含むことを当業者は理解するであろう。コントローラは、当業者によって理解されるように、各種の電源、加熱システム、ポンプ、ロボティクス及びリアクタのガスフローコントローラ又はバルブと接続される。
本発明は、以下の実施例を参照して更に説明される。しかし、実施例は、本発明を限定するものではない。条件及び／又は構造が特定されていない実施例では、当業者は、通常の実験として、本開示を考慮して、このような条件及び／又は構造を明示的に提供することができる。また、特定の実施例に適用される数値は、一部の実施形態では、少なくとも±５０％の範囲で変更されることができ、数値はおおよそである。
実施例１
図２に示されるシーケンス並びに図１Ａ及び１Ｂに示されるＰＥＡＬＤ装置を用いて、以下の表３に示される条件下で、約２のアスペクト比及び約３２０ｎｍの開口深さを有するパターンニングされた表面を有する３００ｍｍ基板上に酸化チタニウム膜を形成した。
基板の上面に堆積された各膜の一部のウェットエッチング速度を測定した。その結果が図３Ｂに示され、ここで、ウェットエッチング速度は、ＷＥＲＲ／［ＴＯＸ］、すなわち、熱酸化膜のウェットエッチング速度に対する膜のウェットエッチング速度の比として表される。図３Ｂに示されるように、膜のウェットエッチング速度は、ＲＦパワーが増加すると、一箇所の頂点を有する下向きの放物線に沿って、変化した。つまり、ＲＦパワーが相対的に弱いときには、ＲＦパワーが増加すると、ウェットエッチング速度は減少する、すなわち、堆積する膜の品質が改善される。ウェットエッチング速度は、最小値（最も低い頂点）に達した後に、増加し始める。最も低い頂点で得られる上面上の膜の品質は、最も高くなり、その後、ＲＦパワーが増加すると、ウェットエッチング速度が増加し、上面に堆積された膜の品質が劣化する。窒素濃度もまた、膜のいくつかに対して測定され、その結果が図３Ａに示される。ウェットエッチング速度の変化は、概して、不純物濃度の変化に相関していた。
実施例２
膜は、実施例１と同一の条件下で堆積され、各膜のウェットエッチング速度は、上面だけでなく、側壁でも測定された。その結果は、図４に示される。図３Ｂに示されるように、ウェットエッチング速度は、最小値（最も低い頂点）に達した後、増加し始め、図４は、最も低い頂点の後のウェットエッチング速度を示す。最も低い頂点で得られた上面上の膜の品質は最も高かった。上面上の膜の品質が、最も低い頂点において最も高くなるが、側壁での膜の品質は、高くない、すなわち、側壁での膜のウェットエッチング速度は、相対的に高かった。プラズマが側壁に容易に到達しないため、側壁での膜の品質は、上面での膜の品質とは対照的に、ＲＦパワーの強度にあまり影響されない。側壁での膜のウェットエッチング速度は、図４に示されるように、ＲＦパワーが増加すると、徐々に減少した。よって、側壁での膜のウェットエッチング速度は、ＲＦパワーが相対的に低いとき、ＲＦパワーが増加すると、上面での膜のウェットエッチング速度の最も低い頂点の後のある値で、上面での膜のウェットエッチング速度よりも高くなったが、図４に示されるように、上面での膜のウェットエッチング速度が増加し続ける一方で、側壁での膜のウェットエッチング速度は、徐々に減少するので、上面での膜のウェットエッチング速度及び側壁での膜のウェットエッチング速度は、ほぼ等しくなった。つまり、上面での膜のエッチング速度と、ＲＦパワーとの関係を表す線分、及び側壁での膜のウェットエッチング速度と、ＲＦパワーとの関係を表す線分は、約５００Ｗにおいて交差する。
実施例３
ＲＦパワーが２００Ｗのときに、トレンチに堆積された膜は、走査型透過電子顕微鏡（Ｓｃａｎｎｉｎｇ ｔｒａｎｓｍｉｓｓｉｏｎ ｅｌｅｃｔｒｏｎ ｍｉｃｒｏｓｃｏｐｙ（ＳＴＥＭ））によって分析された。図５は、膜の断面のＳＴＥＭ写真を示し、ここで、（ａ）は堆積された時の膜を示し、（ｂ）はウェットエッチング後の膜を示す。図５に示されるように、堆積された膜のコンフォーマリティは、上部側壁では８９％であり、下部側壁では９６％であり、底部では９７％であり、一方で、ウェットエッチング後の膜のコンフォーマリティは、上部側壁では８３％であり、下部側壁では９０％であり、底部では８９％であった、すなわち、膜のコンフォーマリティは、ウェットエッチング後に、約６％から約８％減少した。
また、ＲＦパワーが５００Ｗのときに、トレンチに堆積された膜は、走査型透過電子顕微鏡（ＳＴＥＭ）によって分析された。図６は、膜の断面のＳＴＥＭ写真を示し、ここで、（ａ）は堆積された時の膜を示し、（ｂ）はウェットエッチング後の膜を示す。図６に示されるように、堆積された時の膜のコンフォーマリティは、上部側壁では８３％であり、下部側壁では８９％であり、底部では９０％であり、一方で、ウェットエッチング後の膜のコンフォーマリティは、上部側壁では９３％であり、下部側壁では１００％であり、底部では９９％であった、すなわち、膜のコンフォーマリティは、ウェットエッチング後に、約１０％から約１２％減少した。上述したように、ＲＦパワーを増加させることにより、上面での膜の品質を低下させることにより（ここで、ウェットエッチング後の厚さの低下は、ＲＦパワーが２００ＷのときよりもＲＦパワーが５００Ｗのときに、より大きくなる）、ウェットエッチング後の膜のコンフォーマリティは、良好に改善された。
多数かつ様々な変更が本発明の趣旨から逸脱しない範囲でなされることが当業者によって理解されるであろう。よって、本発明の形態は、例示的なものであり、本発明の範囲を制限することを意図するものではないことが明確に理解されるべきである。

Claims (11)

  1. プラズマエンハンスト原子層堆積（ＰＥＡＬＤ）によりトレンチに誘電体膜を堆積する方法であって、
    （ｉ）ＰＥＡＬＤにより誘電体膜が基板のトレンチに堆積される反応空間に印加されるＲＦパワーと、前記トレンチの側壁に堆積される膜の一部のウェットエッチング速度との第１の関係、及び前記ＲＦパワーと、前記基板の上面に堆積される膜の一部のウェットエッチング速度との第２の関係を決定するステップであって、前記反応空間に供給される前駆体は、官能基として−Ｎ（ＣＨ３）２を有する、ステップと、
    （ｉｉ）前記トレンチの前記側壁に堆積される膜の一部の第１のウェットエッチング速度及び前記基板の前記上面に堆積される膜の一部の第２のウェットエッチング速度に対応するＲＦパワーを決定するステップであって、前記第２のウェットエッチング速度は、ステップ（ｉ）での前記第１の関係及び前記第２の関係に基づいて実質的に前記第１のウェットエッチング速度以上である、ステップと、
    （ｉｉｉ）前記ＲＦパワーがステップ（ｉｉ）で決定された前記第１の関係及び前記第２の関係で用いられた条件と等しい条件下でＰＥＡＬＤにより基板のトレンチに誘電体膜を堆積するステップと、
    を備える方法。
  2. ステップ（ｉｉｉ）で用いられる前記ＲＦパワーは、前記第２のウェットエッチング速度が、ステップ（ｉ）での前記第１の関係及び前記第２の関係に基づいて前記第１のウェットエッチング速度と実質的に等しいように選択される請求項１に記載の方法。
  3. 前記前駆体は、ジメチルアミド金属錯体である請求項１に記載の方法。
  4. 前記金属錯体における金属は、チタニウムである請求項３に記載の方法。
  5. ステップ（ｉｉｉ）で用いられる前記ＲＦパワーは、前記基板の面積当たり約０．０７Ｗ／ｃｍ３から約０．７Ｗ／ｃｍ３の範囲内にある請求項１に記載の方法。
  6. 前記トレンチは、約１００ｎｍから約５００ｎｍの深さ、及び約１から約５のアスペクト比を有する請求項１に記載の方法。
  7. ステップ（ｉｉｉ）で堆積された前記誘電体膜は、約１０ｎｍから約１００ｎｍの厚さを有する請求項１に記載の方法。
  8. （ｉｖ）ステップ（ｉｉｉ）で堆積された前記誘電体膜をエッチングするステップを更に備える請求項１に記載の方法。
  9. ステップ（ｉｉｉ）で堆積された前記誘電体膜は、第１のコンフォーマリティを有し、ステップ（ｉｖ）でエッチングされた前記誘電体膜は、前記第１のコンフォーマリティよりも大きい第２のコンフォーマリティを有する請求項８に記載の方法。
  10. 前記第２のコンフォーマリティは、約９０％から約１１０％である請求項９に記載の方法。
  11. プラズマエンハンスト原子層堆積（ＰＥＡＬＤ）によりトレンチに誘電体膜を堆積する方法であって、
    基板の上面での堆積膜のウェットエッチング速度が、実質的にトレンチの側壁での前記堆積膜のウェットエッチング速度以上である条件下で、ＰＥＡＬＤにより前記基板の前記トレンチに誘電体膜を堆積するステップを備え、反応空間に供給される前駆体は、官能基として−Ｎ（ＣＨ３）２を有する、方法。

JP2016200539A 2015-10-15 2016-10-12 Ｐｅａｌｄによりトレンチに誘電体膜を堆積する方法 Pending JP2017078223A (ja)

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