JP2024009207A - 周期的堆積プロセスによって基材上に遷移金属含有膜を形成する方法、遷移金属ハロゲン化物化合物を反応チャンバーに供給する方法、及び関連蒸着装置 - Google Patents

周期的堆積プロセスによって基材上に遷移金属含有膜を形成する方法、遷移金属ハロゲン化物化合物を反応チャンバーに供給する方法、及び関連蒸着装置 Download PDF

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JP2024009207A
JP2024009207A JP2023198228A JP2023198228A JP2024009207A JP 2024009207 A JP2024009207 A JP 2024009207A JP 2023198228 A JP2023198228 A JP 2023198228A JP 2023198228 A JP2023198228 A JP 2023198228A JP 2024009207 A JP2024009207 A JP 2024009207A
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transition metal
precursor
substrate
halide compound
gas phase
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ティモ・ハタンパ
Hatanpaa Timo
カチャ・ヴァイネン
Vayrnen Katja
ミッコ・リタラ
Mikko Ritala
マルック・レスケラ
Leskelae Markku
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ASM IP Holding BV
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Abstract

【課題】周期的堆積プロセスにより基材上に遷移金属含有膜を形成する方法が開示されている。【解決手段】方法は、基材を、二座窒素含有付加配位子を含む遷移金属ハロゲン化物化合物を含む第一の気相反応物質と接触させることと、基材を第二の気相反応物質と接触させることとを含むことができる。二座窒素含有配位子を含む遷移金属ハロゲン化物化合物を反応チャンバーに供給する方法が、関連する蒸着装置と共に開示されている。【選択図】図１

Description

関連出願の相互参照
本開示は、２０１８年２月１５日に出願され、「Ａ ＭＥＴＨＯＤ ＯＦ ＦＯＲＭＩＮＧ Ａ ＴＲＡＮＳＩＴＩＯＮ ＭＥＴＡＬ ＣＯＮＴＡＩＮＩＮＧ ＦＩＬＭ ＯＮ Ａ ＳＵＢＳＴＲＡＴＥ ＢＹ Ａ ＣＹＣＬＩＣＡＬ ＤＥＰＯＳＩＴＩＯＮ ＰＲＯＣＥＳＳ， Ａ ＭＥＴＨＯＤ ＦＯＲ ＳＵＰＰＬＹＩＮＧ Ａ ＴＲＡＮＳＩＴＩＯＮ ＭＥＴＡＬ ＨＡＬＩＤＥ ＣＯＭＰＯＵＮＤ ＴＯ Ａ ＲＥＡＣＴＩＯＮ ＣＨＡＭＢＥＲ， ＡＮＤ ＲＥＬＡＴＥＤ ＶＡＰＯＲ ＤＥＰＯＳＩＴＩＯＮ ＡＰＰＡＲＡＴＵＳ」と題された米国特許出願第１５／８９７，５７８号の利益を主張し、これを参照によって本明細書に組み込む。
共同研究協約の当事者
本願で特許請求される発明は、ヘルシンキ大学（ｔｈｅ Ｕｎｉｖｅｒｓｉｔｙ ｏｆ Ｈｅｌｓｉｎｋｉ）とＡＳＭ Ｍｉｃｒｏｃｈｅｍｉｓｔｒｙ Ｏｙとの間の共同研究協約によって、又は共同研究協約のために、及び／又は共同研究協約に関連してなされた。当協約は、特許請求される発明がなされた日及びその日以前に発効しており、特許請求される発明は、当協約の範囲内で取り組まれた活動の結果としてなされたものである。
本開示は、概ね、周期的堆積プロセスにより、基材上に遷移金属含有膜を形成する方法、特にコバルト、銅、及びニッケル含有膜を形成するための方法に関する。本開示はまた、概ね、遷移金属ハロゲン化物化合物を蒸着ツール及び関連する蒸着装置に供給するための方法に関する。
先端技術ノードにおける半導体デバイス製造プロセスは一般に、例えば、元素遷移金属、遷移金属酸化物、遷移金属窒化物、遷移金属ケイ化物、遷移金属リン化物、遷移金属セレン化物、又は遷移金属ホウ化物などの遷移金属含有膜を形成するための最先端の堆積法を必要とする。
遷移金属含有膜の堆積に対する共通要件は、堆積プロセスが極めて共形であることである。例えば、高アスペクト比特徴を含む三次元構造上に遷移金属含有膜を均一に堆積させるために、共形堆積が必要とされることが多い。遷移金属含有膜の堆積に対する別の共通の要件は、堆積プロセスが、大きな基材領域の上に連続する超薄膜を堆積することができることである。遷移金属含有膜が導電性である特定の場合において、堆積プロセスは、低電気耐性の膜を生成するように最適化される必要があり得る。
例えば、原子層堆積（ＡＬＤ）及び周期的化学気相堆積（ＣＣＶＤ）などの周期的堆積プロセスは、一つまた複数の前駆体（反応物質）を反応チャンバーに逐次的に導入し、そこで前駆体は逐次的、自己制御的に一度に一つずつ基材の表面と反応する。原子レベルの厚さ制御による優れた共形性を有する金属含有膜を生成する周期的堆積プロセスが実証されてきた。
周期的堆積プロセスは、例えば、銅含有膜、ニッケル含有膜、及び特にコバルト含有膜等の遷移金属含有膜の堆積に利用されてもよい。しかしながら、遷移金属含有膜の周期的堆積に適した化学的前駆体、及び特にコバルト含有膜は一般的ではなく、法外な費用がかかる。例えば、コバルト含有膜の周期的堆積に利用される既存の化学前駆体は、望ましくない高温堆積プロセス及び／又はプラズマ増強堆積プロセスの使用を必要とし得る。加えて、既存のコバルト化学前駆体を利用する周期的堆積プロセスは、下層基材の材料への堆積プロセスの感度によって望ましくない場合がある。従って、周期的堆積方法、周期的堆積プロセスでの使用に適した化学前駆体、及び関連する蒸着装置は、遷移金属含有膜、特にコバルト、銅、及びニッケル含有膜の形成に望ましい。
この発明の概要は、概念の選択を簡略化した形で紹介するように提供する。これらの概念について、以下の本開示の例示的な実施形態の「発明を実施するための形態」において、更に詳細に説明される。この発明の概要は、特許請求される主題の主要な特徴又は本質的な特徴を特定することを意図していない、又は特許請求される主題の範囲を限定するために使用することも意図していない。
本開示のいくつかの実施形態では、周期的堆積プロセスによる基材上に金属含有膜を形成する方法が提供される。方法は、基材を、二座窒素含有付加配位子を含む遷移金属ハロゲン化物化合物を含む第一の気相反応物質と接触させることと、基材を第二の気相反応物質と接触させることとを含むことができる。
本開示のいくつかの実施形態では、周期的堆積プロセスによる基材上に金属含有膜を形成する追加的方法が提供される。方法は、基材を、付加体形成配位子を含む遷移金属化合物を含む第一の気相反応物質と接触させることと、基材を第二の気相反応物質と接触させることとを含み得、遷移金属は、銅（Ｃｕ）、ニッケル（Ｎｉ）、及びコバルト（Ｃｏ）からなる群から選択される。
本開示のいくつかの実施形態では、反応チャンバーへの二座窒素含有付加配位子を含む遷移金属ハロゲン化物化合物を供給するための方法が提供される。方法は、遷移金属ハロゲン化物化合物を含むように構成された前駆体供給源容器を提供することと、前駆体供給源容器を反応チャンバーに流体接続することと、前駆体供給源容器内に含まれる遷移金属ハロゲン化物化合物を１５０℃を超える温度に加熱することと、少なくとも０．００１ミリバールの遷移金属ハロゲン化物化合物の蒸気圧を生成することと、遷移金属ハロゲン化物化合物を反応チャンバーへ供給することと、を含み得る。
本開示のいくつかの実施形態では、反応性揮発性化学物質を利用する蒸着装置を提供する。装置は、反応チャンバー、反応チャンバー内に配置された基材、反応チャンバーと流体連通する前駆体供給源容器、及び前駆体供給源容器内に配置された二座窒素含有付加配位子を含む遷移金属ハロゲン化物化合物を含み得る。
本発明と先行技術を超えて達成された利点とを要約する目的で、本発明の特定の目的及び利点が本明細書において上記に説明されている。当然のことながら、必ずしもこうした目的又は利点のすべてが本発明の任意の特定の実施形態によって達成されなくてもよいことが理解されるべきである。それ故に、例えば本明細書に教示又は示唆する通り、一つの利点又は一群の利点を達成又は最適化する様態で、本明細書で教示又は示唆されうる通りの他の目的又は利点を必ずしも達成することなく、本発明が具体化又は実行されてもよいことを当業者は認識するであろう。
これらの実施形態のすべては、本明細書に開示する本発明の範囲内であることが意図されている。当業者には、これらの及び他の実施形態は、添付の図面を参照して、以下のある特定の実施形態の詳細な説明から容易に明らかとなり、本発明は、開示されるいかなる特定の実施形態にも限定されない。
本明細書は、本発明の実施形態とみなされるものを具体的に指摘し、明確に特許請求する特許請求の範囲で結論付ける一方で、本開示の実施形態の利点は、添付の図面と併せて読むと、本開示の実施形態のある特定の実施例の説明から、より容易に確認することができる。
図１は、本開示の実施形態による例示的な周期的堆積方法のプロセスフローを示す。 図２は、本開示の実施形態による、堆積させた遷移金属含有膜を含む例示的なデバイス構造の概略図を示す。 図３は、本開示の周期的堆積プロセスで利用される遷移金属ハロゲン化物化合物の例を示す。 図４は、本開示の実施形態による例示的な蒸着装置の概略図を示す。
ある特定の実施形態及び実施例を以下に開示するが、それらは、本発明が具体的に開示する本発明の実施形態及び／又は用途、ならびにその明白な変更及び均等物を超えて拡大することは、当業者により理解されるであろう。それ故に、開示される本発明の範囲は、以下に説明される特定の開示された実施形態によって限定されるべきではないことが意図される。
本明細書に示される図は、任意の特定の材料、構造又はデバイスの実際の図であることを意味せず、本開示の実施形態を説明するために使用される、単に理想化された表現にすぎない。
本明細書で使用される「周期的堆積」という用語は、基材上に膜を堆積させるために反応チャンバーに前駆体（反応物質）を連続的に導入することを指し、原子層堆積及び周期的化学気相堆積などの堆積技術を含む。
本明細書で使用される「周期的化学気相堆積」という用語は、基材を二つ以上の揮発性前駆体に逐次曝し、その前駆体が基材上で反応及び／又は分解して所望の堆積物を生成する、任意のプロセスを指すことができる。
本明細書で使用する通り、「基材」という用語は、使用される場合がある、又はその上にデバイス、回路もしくは膜が形成される場合がある、あらゆる下層材料又は複数の下層材料を指してもよい。
本明細書で使用する用語「原子層堆積」（ＡＬＤ）は、堆積サイクル、好ましくは複数の連続堆積サイクルがプロセスチャンバー内で行われる蒸着プロセスを指すことができる。典型的には、各サイクルの間、前駆体は、堆積表面（例えば、基材の表面又は以前に堆積させた下地の表面、例えば、以前のＡＬＤサイクルを用いて堆積させた材料など）に化学吸着し、追加の前駆体と容易に反応しない単分子層又はサブ単分子層を形成する（すなわち、自己制御反応）。その後、必要に応じて、化学吸着した前駆体を堆積表面上で所望の材料に変換するのに使用するために、反応物（例えば、別の前駆体または反応ガス）をその後プロセスチャンバー内に導入することができる。典型的には、この反応物質は前駆体と更に反応することができる。更に、各サイクル中にパージ工程を利用して、化学吸着された前駆体の変換後に、過剰な前駆体をプロセスチャンバーから除去する、ならびに／または過剰の反応物質及び／もしくは反応副生成物をプロセスチャンバーから除去することができる。更に、本明細書で使用される「原子層堆積」という用語は、関連する用語、例えば、「化学蒸着原子層堆積」、「原子層エピタキシー」（ＡＬＥ）、分子線エピタキシー（ＭＢＥ）、ガス源ＭＢＥ、又は有機金属ＭＢＥ、並びに前駆体組成物、反応性ガス、及びパージ（例えば、不活性キャリア）ガスの交互パルスで実施される場合の化学ビームエピタキシー等、により示されるプロセスを含むことも意味する。
本明細書で使用される場合、「膜」、「薄膜」、「層」及び「薄層」という用語は、本明細書に開示される方法により堆積させた任意の連続的又は非連続的な構造及び材料を意味することを意図する。「膜」、「薄膜」、「層」及び「薄層」としては、例えば、２Ｄ材料、ナノロッド、ナノチューブ、又はナノ粒子、又は部分的なもしくは完全な分子層、又は部分的なもしくは完全な原子層、又は原子及び／もしくは分子のクラスター、を挙げることができる。「膜」「薄膜」、「層」及び「薄層」は、ピンホールを有する材料又は層を含み得るが、それでも少なくとも部分的に連続している。
本明細書で使用される場合、「遷移金属含有膜」という用語は、元素遷移金属、遷移金属酸化物、遷移金属窒化物、遷移金属ケイ化物、遷移金属セレン化物、遷移金属リン化物、遷移金属ホウ化物、及びこれらの混合物を含むが、これらに限定されない遷移金属種を含有する膜を指し得る。更に、「遷移金属含有膜」という用語は、遷移金属種含有膜ならびに炭素及び／又は水素含有膜を指し得る。
本開示の実施形態を通じて多くの例示的な材料が与えられており、例示的な材料のそれぞれに与えられる化学式は限定的であると解釈されるべきではなく、与えられる非限定的な例示的な材料はある例示的な化学量論によって限定されるべきではないことに留意されたい。
本開示は、基材上に遷移金属含有膜を形成するための方法、及び基材上に遷移金属含有膜の周期的堆積のための特定の方法を含む。本開示の実施形態は、例えば、銅含有膜、ニッケル含有膜、及び特にコバルト含有膜などの遷移金属含有膜の周期的堆積の方法を含み得る。
本開示の特定の実施形態では、周期的堆積方法を利用して、例えば、元素コバルト、酸化コバルト、窒化コバルト、ケイ化コバルト、リン化コバルト、セレン化コバルト、又はホウ化コバルトなどのコバルト含有膜を堆積させ得る。新たな半導体デバイス製造プロセスでは、コバルト金属膜は、銅相互接続材料の周囲の誘電材料への電気移動を抑制するために、ライナー層およびキャッピング層などの用途で重要であり得る。実際に、先進技術ノードでデバイス機能のサイズが減少すると、コバルト金属膜は、一般に利用されている銅相互接続に取って代わり、相互接続材料として利用され得る。コバルト金属膜はまた、巨大磁気抵抗用途及び磁気メモリ用途で関心対象であり得る。更に、コバルト薄膜を、集積回路のシリコンゲート接点上に堆積させて、アニーリング時にケイ化コバルトを形成することもできる。コバルトの酸化物は、例えば、リチウムイオン電池及び電気化学水酸化などの新たなエネルギー関連技術での用途を有する可能性があり、触媒材料としても利用されている。
元素コバルト及びコバルト含有膜の堆積は、典型的には、スパッタリング技術、ならびに有機金属前駆体を用いるＣＶＤ法を利用して達成されてきた。しかしながら、コバルト含有膜の堆積に関するそのような公知の方法は、それらの固有の非共形性により、先端技術ノードには不適切であり得る。原子層堆積などの周期的堆積方法は、特徴的に共形堆積方法であり、高いアスペクト比の特徴を含む三次元構造上の共形遷移金属含有膜の堆積に極めて適している。従って、遷移金属含有膜の堆積、特にコバルト含有膜の堆積のための周期的堆積方法が非常に望ましい。
更に、コバルト含有膜の周期的堆積方法の開発は、適切な化学前駆体及びコスト効果の高い化学前駆体の欠如によって妨げられてきた。例えば、公知の化学前駆体を利用するコバルト含有膜の周期的堆積は、例えば３００℃を超える望ましくない高温堆積プロセスを必要とする可能性がある。プラズマ増強原子層堆積プロセスは、より低い堆積温度でのコバルト含有膜の堆積に利用されてもよいが、プラズマ系プロセスの利用は、高エネルギープラズマ反応種による下層の半導体デバイス構造の潜在的な損傷のため、いくつかのデバイス用途では望ましくない場合がある。従って、遷移金属含有膜の堆積に適した化学前駆体が望ましく、周期的堆積プロセスによるコバルト含有膜の堆積には特定の化学前駆体が望ましい。更に、例えば、原子層堆積装置などの適切な蒸着システムに化学前駆体を供給するための方法及び関連装置が必要である。
従って、本開示の実施形態は、周期的堆積プロセスによる基材上に遷移金属含有膜を形成する方法を含み得る。方法は、基材を、二座窒素含有付加配位子を含む遷移金属ハロゲン化物化合物を含む第一の気相反応物質と接触させることと、基材を第二の気相反応物質と接触させることとを含むことができる。
本開示のいくつかの実施形態では、遷移金属含有層（又は膜）は、遷移金属ハロゲン化物化合物を金属前駆体として利用する周期的堆積プロセスによって堆積させることができる。周期的堆積プロセスの非限定的な例示の実施形態は原子層堆積（ＡＬＤ）を含み、ＡＬＤは典型的な自己制御反応に基づいており、それにより反応物質の逐次及び交互パルスを用いて、堆積サイクル当たり材料の約一原子（又は分子）単層を堆積する。堆積条件及び前駆体は、典型的には、一つの反応物質の吸着層が同じ反応物質の気相の反応物質と非反応性の表面終端を残すように、自己飽和反応を提供するように選択される。その後、基材を、前の終端と反応する異なる反応物質と接触させ、連続的な堆積を可能にする。従って、交互パルスの各サイクルは、典型的には、所望の材料の約一単層以下の単層を残す。しかし、上記のように、一つ又は複数のＡＬＤサイクルにおいて、例えば、交互するプロセスの性質にもかかわらずいくつかの気相反応が起こる場合、材料の一つより多い単層を堆積させることができることを、当業者は認識するであろう。
遷移金属含有膜を堆積させるＡＬＤタイプのプロセスでは、一回の堆積サイクルは、基材を第一の反応物質に接触させることと、任意の未反応の第一の反応物質及び反応副生成物を反応空間から除去することと、基材を第二の反応物質に接触させることと、を含むことができ、第二の除去する工程に続く。第一の反応物質は、遷移金属ハロゲン化物化合物（「金属前駆体」）を含んでもよく、第二の反応物質は、酸素前駆体、窒素前駆体、シリコン前駆体、硫黄前駆体、セレン前駆体、リン前駆体、ホウ素前駆体、又は還元剤のうちの少なくとも一つを含んでもよい。
前駆体は、反応物質間の気相反応を防止し、自己飽和表面反応を可能にするように、不活性ガス、例えばアルゴン（Ａｒ）又は窒素（Ｎ２）によって分離されることができる。しかし、いくつかの実施形態では、基材を移動させて、第一の気相反応物質と第二の気相反応物質とを、別々に接触させることができる。反応が自己飽和するので、基材の厳密な温度制御及び前駆体の正確な投与量制御は必要でない場合もある。しかし、基材温度は、入射ガス種が単層に凝縮しないように、及び表面で分解しないようにすることが好ましい。基材を次の反応性化学物質と接触させる前に、余分な化学物質および反応副生成物がある場合には、それらを、例えば反応空間をパージすることによりまたは基材を移動させることにより、基材の表面から除去する。望ましくない気体の分子を、不活性パージガスを用いて反応空間から効果的に排出することができる。パージを促進するために、真空ポンプを使用することができる。
遷移金属含有膜を堆積させるために使用できる反応器を、堆積に使用できる。このような反応器としては、前駆体を供給するための適切な装置及び手段を備えたＡＬＤ反応器、並びにＣＶＤ反応器が挙げられる。いくつかの実施形態によれば、シャワーヘッド反応器を使用し得る。いくつかの実施形態によれば、クロスフロー、バッチ、ミニバッチ、又は空間ＡＬＤ反応器が使用され得る。
使用することができる適切な反応器の例としては、アリゾナ州フェニックスのＡＳＭ Ａｍｅｒｉｃａ，Ｉｎｃ．、及びオランダ、アルメアのＡＳＭ Ｅｕｒｏｐｅ Ｂ．Ｖ．から入手可能な、市販の単一基材（又は単一ウエハ）成膜装置、例えば、Ｐｕｌｓａｒ（登録商標）反応器（例えば、Ｐｕｌｓａｒ（登録商標）２０００、Ｐｕｌｓａｒ（登録商標）３０００、及びＰｕｌｓａｒ（登録商標）ＸＰ ＡＬＤ等）、並びにＥｍｅｒＡＬＤ（登録商標）ＸＰ及びＥｍｅｒＡＬＤ（登録商標）反応器等が挙げられる。他の市販の反応器としては、商品名Ｅａｇｌｅ（登録商標）ＸＰ及びＸＰ８、日本エー・エス・エム（株）（日本、東京）製の反応器が挙げられる。いくつかの実施形態では、反応器は処理中に基材が移動又は回転する空間ＡＬＤ反応器である。
本開示のいくつかの実施形態では、バッチ式反応器を使用し得る。適切なバッチ式反応器としては、商品名Ａ４００及びＡ４１２ＰＬＵＳでＡＳＭ Ｅｕｒｏｐｅ Ｂ．Ｖ（オランダ、アルメア）から市販のＡｄｖａｎｃｅ（登録商標）４００シリーズ反応器が挙げられるが、これに限定されない。いくつかの実施形態では、ウエハは処理中に回転する。他の実施形態では、バッチ式反応器は、１０枚以下のウエハ、８枚以下のウエハ、６枚以下のウエハ、４枚以下のウエハ、もしくは２枚以下のウエハを収容するように構成されるミニバッチ式反応器を備える。バッチ式反応器が使用されるいくつかの実施形態では、ウエハ間の不均一性は３％（１シグマ）未満、２％未満、１％未満又は更には０．５％未満である。
本明細書に記載の堆積方法を、クラスタツールに接続される反応器又は反応チャンバーで任意に行うことができる。クラスタツールでは、各反応チャンバーが一つのタイプのプロセス専用であるため、各モジュール内の反応チャンバーの温度を一定に保つことができ、各運転の前に基材をプロセス温度まで加熱する反応器と比較してスループットが向上する。更に、クラスタツールでは、反応チャンバーを基材間で所望のプロセス圧力レベルに排気する時間を短縮することが可能である。本開示のいくつかの実施形態では、堆積プロセスは、複数の反応チャンバーを含むクラスタツール内で実施されてもよく、各個々の反応チャンバーは、基材を個々の前駆体ガスに曝露させるために使用されてもよく、基材を複数の前駆体ガスに曝露されるように異なる反応チャンバー間を搬送してもよく、基材の搬送は基材の酸化／汚染を回避するために制御された周辺環境下で実施される。本開示のいくつかの実施形態では、堆積プロセスは、複数の反応チャンバーを備えるクラスタツール内で実施されてもよく、各個々の反応チャンバーは、基材を異なる堆積温度に加熱するように構成されてもよい。
独立型反応器にはロードロックが装備されている。その場合、各運転と運転との間に反応空間を冷却する必要はない。いくつかの実施形態では、遷移金属含有膜の堆積のための堆積プロセスは、例えばＡＬＤサイクル又は周期的ＣＶＤサイクルなどの複数の堆積サイクルを含み得る。
いくつかの実施形態では、周期的堆積プロセスは、基材上に遷移金属含有膜を形成するのに使用され、周期的堆積プロセスはＡＬＤタイプのプロセスであり得る。いくつかの実施形態では、周期的堆積は、ハイブリッドＡＬＤ／ＣＶＤ又は周期的ＣＶＤプロセスであることができる。例えば、いくつかの実施形態では、ＡＬＤプロセスの成長速度は、ＣＶＤプロセスと比較して低い場合がある。成長速度を増加させる一つのアプローチは、ＡＬＤプロセスにおいて典型的に使用される温度よりも高い基材温度で動作するアプローチであり、結果として化学蒸着プロセスになるが、更に前駆体の逐次導入を利用し、このようなプロセスは周期的ＣＶＤと呼ばれ得る。
本開示のいくつかの実施形態によれば、ＡＬＤプロセスは、部分的に作成された半導体デバイス構造などの基材上に遷移金属含有膜を堆積させるために使用され得る。本開示のいくつかの実施形態では、各ＡＬＤサイクルは、二つの異なる堆積工程又は段階を含む。堆積サイクルの第一段階（「金属段階」）では、堆積が望まれる基材の表面を、基材の表面上に化学吸着する金属前駆体を含み、基材の表面上に反応物質種の約一単層以下の単層を形成する第一の気相反応物質と接触させる。堆積の第二段階では、堆積が望まれる基材表面は、酸素前駆体、窒素前駆体、シリコン前駆体、硫黄前駆体、セレン前駆体、リン前駆体、ホウ素前駆体、又は還元剤のうちの少なくとも一つを含む第二の気相反応物質と接触し、第二の気相反応物質は、基材の表面上の遷移金属種と反応して、例えば、元素遷移金属、遷移金属酸化物、遷移金属窒化物、遷移金属ケイ化物、遷移金属セレン化物、遷移金属リン化物、遷移金属ホウ化物、及びこれらの混合物、ならびに炭素及び／又は水素を更に含む遷移金属含有膜などの基材上に遷移金属含有膜を形成することができる。
本開示のいくつかの実施形態では、第一の気相反応物質は、本明細書で「金属化合物」とも称される、金属含有前駆体を含むことができる。いくつかの実施形態では、第一の気相反応物質は、付加体形成配位子を有する遷移金属化合物を含み得る。いくつかの実施形態では、第一の気相反応物質は、遷移金属化合物を含み得る。いくつかの実施形態では、第一の気相反応物質は、遷移金属ハロゲン化物化合物を含み得る。いくつかの実施形態では、第一の気相反応物質は、単座、二座、又は多座付加体形成配位子などの付加体形成配位子を有する遷移金属化合物を含み得る。いくつかの実施形態では、第一の気相反応物質は、単座、二座、又は多座付加体形成配位子などの付加体形成配位子を有する遷移金属ハロゲン化物化合物を含み得る。いくつかの実施形態では、第一の気相反応物質は、窒素を含む単座、二座、又は多座付加体形成配位子などの窒素を含む付加体形成配位子を有する遷移金属化合物を含み得る。いくつかの実施形態では、第一の気相反応物質は、亜リン酸、酸素、又は硫黄を含む単座、二座、又は多座付加体形成配位子などの亜リン酸、酸素、又は硫黄を含む付加体形成配位子を有する遷移金属化合物を含み得る。例えば、いくつかの実施形態では、遷移金属ハロゲン化物化合物は、遷移金属塩化物、遷移金属ヨウ化物、遷移金属フッ化物、又は遷移金属臭化物を含み得る。本開示のいくつかの実施形態では、遷移金属ハロゲン化物化合物は、コバルト、ニッケル、又は銅のうちの少なくとも一つを含むが、これに限定されない遷移金属種を含むことができる。本開示のいくつかの実施形態では、遷移金属ハロゲン化物化合物は、塩化コバルト、塩化ニッケル、又は塩化銅のうちの少なくとも一つを含むことができる。いくつかの実施形態では、遷移金属ハロゲン化物化合物は、二座窒素含有付加体形成配位子を含んでもよい。いくつかの実施形態では、遷移金属ハロゲン化物化合物は、二つの窒素原子を含む付加体形成配位子を含んでもよく、ここで窒素原子の各々は少なくとも一つの炭素原子に結合される。本開示のいくつかの実施形態では、遷移金属ハロゲン化物化合物は、中心遷移金属原子に結合された一つ又は複数の窒素原子を含み、それによって金属複合体を形成する。
本開示のいくつかの実施形態では、第一の気相反応物質は、以下の式（Ｉ）を有する遷移金属化合物を含み得る。
（付加体）ｎ－Ｍ－Ｘａ （Ｉ）
式中、「付加体」のそれぞれは、付加体形成配位子であり、単座、二座、又は多座付加体形成配位子又はその混合物となるよう独立して選択されることができ、単座形成配位子の場合、ｎは１～４であり、二座又は多座付加体形成配位子の場合、ｎは１～２であり、Ｍは、例えば、コバルト（Ｃｏ）、銅（Ｃｕ）、又はニッケル（Ｎｉ）などの遷移金属であり、Ｘａのそれぞれは別の配位子であり、ハロゲン化物又は他の配位子となるように独立して選択されることができ、ここでａは、１～４であり、一部の例では、ａは２である。
本開示のいくつかの実施形態では、遷移金属ハロゲン化物化合物などの遷移金属化合物における付加体形成配位子は、窒素原子、亜リン酸原子、酸素原子、又は硫黄原子のうちの少なくとも一つを介して、遷移金属化合物の遷移金属原子に配位させる、単座、二座、又は多座付加体形成配位子を含み得る。本開示のいくつかの実施形態では、遷移金属化合物中の付加体形成配位子は、環状付加配位子を含み得る。本開示のいくつかの実施形態では、遷移金属化合物中の付加体形成配位子は、モノアミン、ジアミン、又はポリアミンを含み得る。本開示のいくつかの実施形態では、遷移金属化合物中の付加体形成配位子は、モノエーテル、ジエーテル、又はポリエーテルを含み得る。いくつかの実施形態では、遷移金属化合物中の付加体形成配位子は、モノホスフィン、ジホスフィン、又はポリホスフィンを含み得る。いくつかの実施形態では、遷移金属化合物中の付加体形成配位子は、付加体形成配位子中に、窒素、酸素、亜リン酸、又は硫黄に加えて炭素を含んでもよい。
本開示のいくつかの実施形態では、遷移金属化合物中の付加体形成配位子は、一つの単座付加体形成配位子を含み得る。本開示のいくつかの実施形態では、遷移金属化合物中の付加体形成配位子は、二つの単座付加体形成配位子を含み得る。本開示のいくつかの実施形態では、遷移金属化合物中の付加体形成配位子は、三つの単座付加体形成配位子を含み得る。本開示のいくつかの実施形態では、遷移金属化合物中の付加体形成配位子は、四つの単座付加体形成配位子を含み得る。本開示のいくつかの実施形態では、遷移金属化合物中の付加体形成配位子は、一つの二座付加体形成配位子を含み得る。本開示のいくつかの実施形態では、遷移金属化合物中の付加体形成配位子は、二つの二座付加体形成配位子を含み得る。本開示のいくつかの実施形態では、遷移金属化合物中の付加体形成配位子は、一つの多座付加体形成配位子を含み得る。本開示のいくつかの実施形態では、遷移金属化合物中の付加体形成配位子は、二つの多座付加体形成配位子を含み得る。
本開示のいくつかの実施形態では、付加体形成配位子は、アミン、ジアミン、又はポリアミン付加体形成配位子などの窒素を含む。このような実施形態では、遷移金属化合物は、トリエチルアミン（ＴＥＡ）、Ｎ，Ｎ，Ｎ’，Ｎ’－テトラメチル－１，２－エチレンジアミン（ＣＡＳ：１１０－１８－９）（ＴＭＥＤＡ）、Ｎ，Ｎ，Ｎ’，Ｎ’－テトラエチルエチレンジアミン（ＣＡＳ：１５０－７７－６）（ＴＥＥＤＡ）、Ｎ，Ｎ’－ジエチル－１，２－エチレンジアミン（ＣＡＳ：１１１－７４－０）（ＤＥＥＤＡ）、Ｎ，Ｎ’－ジイソプロピルエチレンジアミン（ＣＡＳ：４０１３－９４－９）、Ｎ，Ｎ，Ｎ’，Ｎ’－テトラメチル－１，３－プロパンジアミン（ＣＡＳ：１１０－９５－２）（ＴＭＰＤＡ）、Ｎ，Ｎ，Ｎ’，Ｎ’－テトラメチルメタンジアミン（ＣＡＳ：５１－８０－９）（ＴＭＭＤＡ）、Ｎ，Ｎ，Ｎ’，Ｎ’’，Ｎ’’－ペンタメチルジエチレントリアミン（ＣＡＳ：３０３０－４７－５）（ＰＭＤＥＴＡ）、ジエチレントリアミン（ＣＡＳ：１１１－４０－０）（ＤＩＥＮ）、トリエチレンテトラミン（ＣＡＳ：１１２－２４－３）（ＴＲＩＥＮ）、トリス（２－アミノエチル）アミン（ＣＡＳ：４０９７－８９－６）（ＴＲＥＮ、ＴＡＥＡ）、１，１，４，７，１０，１０－ヘキサメチルトリエチレンテトラミン（ＣＡＳ：３０８３－１０－１）（ＨＭＴＥＴＡ）、１，４，８，１１－テトラアザシクロテトラデカン（ＣＡＳ：２９５－３７－４）（Ｃｙｃｌａｍ）、１，４，７－トリメチル－１，４，７－トリアザシクロノナン（ＣＡＳ：９６５５６－０５－７）、又は１，４，８，１１－テトラメチル－１，４，８，１１－テトラアザシクロテトラデカン（ＣＡＳ：４１２０３－２２－９）のうちの少なくとも一つを含み得る。
本開示のいくつかの実施形態では、付加体形成配位子は、ホスフィン、ジホスフィン、又はポリホスフィン付加体形成配位子などの亜リン酸を含む。例えば、遷移金属化合物は、トリエチルホスフィン（ＣＡＳ：５５４－７０－１）、トリメチルホスファイト（ＣＡＳ：１２１－４５－）、１，２－ビス（ジエチルホスフィノ）エタン（ＣＡＳ：６４１１－２１－８）（ＢＤＥＰＥ）、又は１，３－ビス（ジエチルホスフィノ）プロパン（ＣＡＳ：２９１４９－９３－７）のうちの少なくとも一つを含んでもよい。
本開示のいくつかの実施形態では、付加体形成配位子は、エーテル、ジエーテル、又はポリエーテル付加体形成配位子などの酸素を含む。例えば、遷移金属化合物は、１，４－ジオキサン（ＣＡＳ：１２３－９１－１）、１，２－ジメトキシエタン（ＣＡＳ：１１０－７１－４）（ＤＭＥ、モノグライム）、ジエチレングリコールジメチルエーテル（ＣＡＳ：１１１－９６－６）（ジグライム）、トリエチレングリコールジメチルエーテル（ＣＡＳ：１１２－４９－２）（トリグライム）、又は１，４，７，１０－テトラオキサシクロドデカン（ＣＡＳ：２９４－９３－９）（１２－クラウン－４）のうちの少なくとも一つを含み得る。
本開示のいくつかの実施形態では、付加体形成配位子は、例えば、１，７－ジアザ－１２－クラウン－４：１，７－ジオキサ－４，１０－ジアザシクロドデカン（ＣＡＳ：２９４－９２－８）、又は１，２－ビス（メチルチオ）エタン（ＣＡＳ：６６２８－１８－８）のうちの少なくとも一つなどのチオエーテル又は混合エーテルアミンを含む場合がある。
いくつかの実施形態では、遷移金属ハロゲン化物化合物は、塩化コバルトＮ，Ｎ，Ｎ’，Ｎ’－テトラメチル－１，２－エチレンジアミン（ＣｏＣｌ２（ＴＭＥＤＡ））を含み得る。いくつかの実施形態では、遷移金属ハロゲン化物化合物は、臭化コバルトテトラメチルエチレンジアミン（ＣｏＢｒ２（ＴＭＥＤＡ））を含み得る。いくつかの実施形態では、遷移金属ハロゲン化物化合物は、ヨウ化コバルトテトラメチルエチレンジアミン（Ｃｏｌ２（ＴＭＥＤＡ））を含み得る。いくつかの実施形態では、遷移金属ハロゲン化物化合物は、塩化コバルトＮ，Ｎ，Ｎ’，Ｎ’－テトラメチル－１，３－プロパンジアミン（ＣｏＣｌ２（ＴＭＰＤＡ））を含み得る。本開示のいくつかの実施形態では、遷移金属ハロゲン化物化合物は、塩化コバルトＮ，Ｎ，Ｎ’，Ｎ’－テトラメチル－１，２－エチレンジアミン（ＣｏＣｌ２（ＴＭＥＤＡ））、塩化ニッケルテトラメチル－１，３－プロパンジアミン（ＮｉＣｌ２（ＴＭＰＤＡ））、又はヨウ化ニッケルテトラメチル－１，３－プロパンジアミン（ＮｉＩ２（ＴＭＰＤＡ））を含み得る。
本開示のいくつかの実施形態では、基材を遷移金属ハロゲン化物化合物を含む第一の気相反応物質、すなわち付加体形成配位子を含む遷移金属ハロゲン化物と接触させることは、基材を遷移金属ハロゲン化物化合物に曝露すること、すなわち約０．０１秒～約６０秒の間、約０．０５秒～約１０秒の間、又は約０．１秒～約５．０秒の間、接触させることを含むことができる。加えて、遷移金属ハロゲン化物化合物をパルス注入する間、遷移金属ハロゲン化物化合物の流量は、２０００ｓｃｃｍ未満、又は５００ｓｃｃｍ未満、又は更には１００ｓｃｃｍであってもよい。加えて、基材上に遷移金属ハロゲン化物化合物をパルス注入する間、遷移金属ハロゲン化物化合物の流量は、約１～２０００ｓｃｃｍ、約５～１０００ｓｃｃｍ、又は約１０～約５００ｓｃｃｍで変動してもよい。
過剰な遷移金属ハロゲン化物化合物及び反応副生成物がある場合には、それらを、例えば不活性ガスでポンピングすることにより、表面から除去し得る。例えば、本開示のいくつかの実施形態では、この方法は、基材の表面を約２．０秒未満の時間パージするパージサイクルを含み得る。過剰な遷移金属ハロゲン化物化合物及び反応副生成物を、反応チャンバーと流体連通するポンプシステムによって生成される真空を用いて除去してもよい。
堆積サイクルの第二段階では、基材を、酸素前駆体、窒素前駆体、シリコン前駆体、硫黄前駆体、セレン前駆体、リン前駆体、ホウ素前駆体、又は還元剤のうちの少なくとも一つを含む第二の気相反応物質と接触させることができる。いくつかの実施形態では、第二の気相反応物質は、酸素前駆体を含んでもよく、本明細書に開示される周期的堆積方法によって堆積される遷移金属含有膜は、遷移金属酸化物を含み得る。いくつかの実施形態では、第二の気相反応物質は、以下により詳細に説明される還元剤を含んでもよく、ここに開示される周期的堆積方法によって堆積される遷移金属含有膜は、元素遷移金属を含み得る。いくつかの実施形態では、第二の気相反応物質は、窒素前駆体を含んでもよく、本明細書に開示される周期的堆積方法によって堆積される遷移金属含有膜は、遷移金属窒化物を含み得る。いくつかの実施形態では、第二の気相反応物質は、シリコン前駆体を含んでもよく、本明細書に開示される周期的堆積方法によって堆積される遷移金属含有膜は、遷移金属ケイ化物を含み得る。いくつかの実施形態では、第二の気相反応物質は、硫黄前駆体を含んでもよく、本明細書に開示される周期的堆積方法によって堆積される遷移金属含有膜は、遷移金属硫化物を含み得る。いくつかの実施形態では、第二の気相反応物質は、セレン前駆体を含んでもよく、本明細書に開示される周期的堆積方法によって堆積される遷移金属含有膜は、遷移金属セレン化物を含み得る。いくつかの実施形態では、第二の気相反応物質は、リン前駆体を含んでもよく、本明細書に開示される周期的堆積方法によって堆積される遷移金属含有膜は、遷移金属リン化物を含み得る。いくつかの実施形態では、第二の気相反応物質は、ホウ素前駆体を含んでもよく、本明細書に開示される周期的堆積方法によって堆積される遷移金属含有膜は、遷移金属ホウ化物を含み得る。
本開示の実施形態では、第二の気相反応物質は酸素前駆体を含み、酸素前駆体は、オゾン（Ｏ３）、分子状酸素（Ｏ２）、酸素原子（Ｏ）、酸素プラズマ、酸素ラジカル、酸素励起種、水（Ｈ２Ｏ）、又は過酸化水素（Ｈ２Ｏ２）のうちの少なくとも一つを含んでもよい。本開示の実施形態では、第二の気相反応物質は窒素前駆体を含み、窒素前駆体は、アンモニア（ＮＨ３）、ヒドラジン（Ｎ２Ｈ４）、トリアザン（Ｎ３Ｈ５）、ｔｅｒｔ－ブチルヒドラジン（Ｃ４Ｈ９Ｎ２Ｈ３）、メチルヒドラジン（ＣＨ３ＮＨＮＨ２）、ジメチルヒドラジン（（ＣＨ３）２Ｎ２Ｈ２）、もしくは窒素プラズマのうちの少なくとも一つを含むことでき、又は窒素プラズマは水素を含む。
いくつかの実施形態では、第二の気相反応物質は、炭化水素置換ヒドラジン前駆体を含み得る。堆積サイクルの第二の段階（「置換ヒドラジン段階」）では、基材を、炭化水素置換ヒドラジン前駆体を含む第二の気相反応物質と接触させる。本開示のいくつかの実施形態では、方法は、少なくとも４個の炭素原子を有するアルキル基を含むように置換ヒドラジンを選択することを更に含むことができ、ここで、「アルキル基」は、長さが少なくとも４個の炭素原子の飽和又は不飽和炭化水素鎖を指し、例えば、ブチル、ペンチル、ヘキシル、ヘプチル及びオクチル、並びにそれらの異性体、例えば、それらのｎ－、ｉｓｏ－、ｓｅｃ－及びｔｅｒｔ－異性体など、であるが、これらに限定されない。アルキル基は、直鎖又は分枝鎖であってもよく、アルキル基のすべての構造異性体形態を包含してもよい。いくつかの実施形態では、アルキル鎖は置換されていてもよい。本開示のいくつかの実施形態では、アルキルヒドラジンは、窒素に結合した少なくとも一つの水素を含み得る。本開示のいくつかの実施形態では、アルキルヒドラジンは、窒素に結合した少なくとも二つの水素を含み得る。本開示のいくつかの実施形態では、アルキルヒドラジンは、窒素に結合した少なくとも一つの水素、及び窒素に結合した少なくとも一つのアルキル鎖を含み得る。本開示のいくつかの実施形態では、第二の反応物質は、アルキルヒドラジンを含んでもよく、更に一つ又は複数のｔｅｒｔ－ブチルヒドラジン（Ｃ４Ｈ９Ｎ２Ｈ３）、ジメチルヒドラジン、又はジエチルヒドラジンを含み得る。本開示のいくつかの実施形態では、置換ヒドラジンは、窒素に結合した少なくとも一つの炭化水素基を有する。本開示のいくつかの実施形態では、置換ヒドラジンは、窒素に結合した少なくとも二つの炭化水素基を有する。本開示のいくつかの実施形態では、置換ヒドラジンは、窒素に結合した少なくとも三つの炭化水素基を有する。本開示のいくつかの実施形態では、置換ヒドラジンは、窒素に結合した少なくとも一つのＣ１－Ｃ３炭化水素基を有する。本開示のいくつかの実施形態では、置換ヒドラジンは、窒素に結合した少なくとも一つのＣ４－Ｃ１０炭化水素基を有する。本開示のいくつかの実施形態では、置換ヒドラジンは、窒素に結合した直鎖、分枝鎖、又は環状若しくは芳香族炭化水素基を有する。本開示のいくつかの実施形態では、置換ヒドラジンは、窒素に結合した置換炭化水素基を含む。
本開示のいくつかの実施形態では、置換ヒドラジンは、以下の式ＩＩを有する：
ＲＩＲＩＩ－Ｎ－ＮＲＩＩＩＲＩＶ （ＩＩ）
式中、ＲＩは、炭化水素基、例えば、直鎖、分枝鎖、環状、芳香族又は置換炭化水素基など、から選択されることができ、ＲＩＩ、ＲＩＩＩ、ＲＩＶ基のそれぞれは、水素基又は炭化水素基、例えば、直鎖、分枝鎖、環状、芳香族又は置換炭化水素基など、であるように独立して選択されることができる。
いくつかの実施形態では、式（ＩＩ）のＲＩ、ＲＩＩ、ＲＩＩＩ、ＲＩＶの各々は、直鎖、分枝鎖、環状、芳香族又は置換炭化水素基のようなＣ１－Ｃ１０炭化水素、Ｃ１－Ｃ３炭化水素、Ｃ４－Ｃ１０炭化水素、又は水素とすることができる。いくつかの実施形態では、ＲＩ、ＲＩＩ、ＲＩＩＩ、ＲＩＶ基の少なくとも一つは、フェニル基のような芳香族基を含む。いくつかの実施形態では、ＲＩ、ＲＩＩ、ＲＩＩＩ、ＲＩＶ基の少なくとも一つは、メチル、エチル、ｎ－プロピル、ｉ－プロピル、ｎ－ブチル、ｉ－ブチル、ｓ－ブチル、ｔｅｒｔ－ブチル基又はフェニル基を含む。いくつかの実施形態では、各々のＲＩ、ＲＩＩ、ＲＩＩＩ、ＲＩＶ基の少なくとも二つは、メチル、エチル、ｎ－プロピル、ｉ－プロピル、ｎ－ブチル、ｉ－ブチル、ｓ－ブチル、ｔｅｒｔ－ブチル基又はフェニル基を含むように、独立して選択することができる。いくつかの実施形態では、ＲＩＩ、ＲＩＩＩ及びＲＩＶ基は水素である。いくつかの実施形態では、ＲＩＩ、ＲＩＩＩ及びＲＩＶ基の少なくとも二つ一つは水素である。いくつかの実施形態では、ＲＩＩ、ＲＩＩＩ及びＲＩＶ基の少なくとも一つは水素である。いくつかの実施形態では、ＲＩＩ、ＲＩＩＩ及びＲＩＶ基の全ては水素である。
本開示の実施形態では、第二の気相反応物質は、シリコン前駆体を含み、シリコン前駆体は、シラン（ＳｉＨ４）、ジシラン（Ｓｉ２Ｈ６）、トリシラン（Ｓｉ３Ｈ８）、テトラシラン（Ｓｉ４Ｈ１０）、イソペンタシラン（Ｓｉ５Ｈ１２）、又はネオペンタシラン（Ｓｉ５Ｈ１２）のうちの少なくとも一つを含み得る。本開示の実施形態では、第二の気相反応物質は、シリコン前駆体を含み、シリコン前駆体は、Ｃ１－Ｃ４アルキルシランを含み得る。本開示の実施形態では、第二の気相反応物質は、シリコン前駆体を含み、シリコン前駆体は、シラン族からの前駆体を含み得る。
本開示の実施形態では、第二の気相反応物質は、ホウ素前駆体を含み、ホウ素前駆体は、ボラン（ＢＨ３）、ジボラン（Ｂ２Ｈ６）又はデカボラン（Ｂ１０Ｈ１４）などのその他のボランのうちの少なくとも一つを含み得る。
本開示の実施形態では、第二の気相反応物質は、水素前駆体を含み、水素前駆体は、Ｈ２、Ｈ原子、Ｈ－イオン、Ｈ－プラズマ、又はＨ－ラジカルのうちの少なくとも一つを含み得る。
本開示のいくつかの実施形態では、第二の気相反応物質は、リン前駆体、硫黄前駆体、又はセレン化物前駆体を含む。いくつかの実施形態では、硫黄前駆体は、水素及び硫黄を含む。いくつかの実施形態では、硫黄前駆体はアルキル硫黄化合物である。いくつかの実施形態では、第二の反応物質は、一つ又は複数の硫黄元素、Ｈ２Ｓ、（ＣＨ３）２Ｓ、（ＮＨ４）２Ｓ、（（ＣＨ３）２ＳＯ）、及びＨ２Ｓ２を含む。いくつかの実施形態では、セレン前駆体はアルキルセレン化合物である。いくつかの実施形態では、第二の反応物質は、元素セレン、Ｈ２Ｓｅ、（ＣＨ３）２Ｓｅ、及びＨ２Ｓｅ２のうちの一つ又は複数を含む。いくつかの実施形態では、セレン前駆体は、水素及びセレンを含む。いくつかの実施形態では、第二の反応物質は、Ｔｅ、Ｓｂ、Ｓｅ、例えば、（Ｍｅ３Ｓｉ）２Ｔｅ、（Ｍｅ３Ｓｉ）２Ｓｅ、又は（Ｍｅ３Ｓｉ）３Ｓｂなどのアルキルシリル化合物を含んでもよい。いくつかの実施形態では、リン前駆体はアルキルリン化合物である。いくつかの実施形態では、第二の反応物質は、元素リン、ＰＨ３、又はメチルホスフィンなどのアルキルホスフィンのうちの一つ又は複数を含む。いくつかの実施形態では、リン前駆体は、水素及びリンを含む。
本開示の実施形態では、第二の気相反応物質は、還元剤などの有機前駆体を含み、例えば、アルコール、アルデヒド又はカルボン酸、又は他の有機化合物、例えば、金属又は半金属を有しないが、－ＯＨ基を含む有機化合物を利用してもよい。アルコールは、第一級アルコール、第二級アルコール、第三級アルコール、ポリヒドロキシアルコール、環状アルコール、芳香族アルコール、及びアルコールの他の誘導体とすることができる。
第一級アルコールは、別の炭素原子に結合される炭素原子に取り付けられる－ＯＨ基を有し、特に一般式（ＩＩＩ）による第一級アルコールである。
Ｒ１－ＯＨ （ＩＩＩ）
式中、Ｒ１は、直鎖又は分岐鎖Ｃ１－Ｃ２０アルキル、又はメチル、エチル、プロピル、ブチル、ペンチル又はヘキシルなどのアルケニル基である。第一級アルコールの例には、メタノール、エタノール、プロパノール、ブタノール、２－メチルプロパノール及び２－メチルブタノールが含まれる。
第二級アルコールは、二つの他の炭素原子に結合される炭素原子に取り付けられる－ＯＨ基を有する。特に、第二級アルコールは以下の一般式（ＩＶ）を有する。
式中、各Ｒ１は、メチル、エチル、プロピル、ブチル、ペンチル又はヘキシルなどの直鎖又は分岐鎖Ｃ１－Ｃ２０アルキル及びアルケニル基の群から独立して選択される。第二級アルコールの例には、２－プロパノール及び２－ブタノールが含まれる。
第三級アルコールは、三つの他の炭素原子に結合される炭素原子に取り付けられる－ＯＨ基を有する。特に、第三級アルコールは以下の一般式（Ｖ）を有する。
式中、各Ｒ１は、メチル、エチル、プロピル、ブチル、ペンチル又はヘキシルなどの直鎖又は分岐鎖Ｃ１－Ｃ２０アルキル及びアルケニル基の群から独立して選択される。第三級アルコールの一例はｔｅｒｔ－ブタノールである。
ジオール及びトリオールなどのポリヒドロキシアルコールは、上述の通り、第一級、第二級及び／又は第三級アルコール基を有する。ポリヒドロキシアルコールの例は、エチレングリコール及びグリセロールである。
環状アルコールは、５～６個の炭素原子など、１～１０個の環の一部である少なくとも一つの炭素原子に取り付けられる－ＯＨ基を有する。
芳香族アルコールは、側鎖のベンゼン環又は炭素原子のいずれかに取り付けられた少なくとも一つの－ＯＨ基を有する。
有機前駆体は、一般式（ＶＩ）を有する化合物、一般式（ＶＩＩ）を有するアルカンジアール化合物、ハロゲン化アルデヒド及びアルデヒドの他の誘導体からなる群から選択される、少なくとも一つのアルデヒド基（－ＣＨＯ）を含んでもよい。
従って、一実施形態では、有機前駆体は一般式（ＶＩ）を有するアルデヒドである。
Ｒ３－ＣＨＯ （ＶＩ）
式中、Ｒ３は、水素及びメチル、エチル、プロピル、ブチル、ペンチル又はヘキシルなどの直鎖又は分岐鎖Ｃ１－Ｃ２０アルキル及びアルケニル基からなる群から選択される。いくつかの実施形態では、Ｒ３は、メチル又はエチルからなる群から選択される。例示的な化合物は、限定されないが、式（ＶＩ）によると、ホルムアルデヒド、アセトアルデヒド、及びブチルアルデヒドである。
別の実施形態では、有機前駆体は一般式（ＶＩＩ）を有するアルデヒドである。
ＯＨＣ－Ｒ４－ＣＨＯ （ＶＩＩ）
式中、Ｒ４は直鎖又は分岐鎖Ｃ１－Ｃ２０飽和又は不飽和炭化水素である。別の方法として、アルデヒド基は相互に直接結合されてもよい（Ｒ４はｎｕｌｌである）。
少なくとも一つの－ＣＯＯＨ基を含有する有機前駆体は、一般式（ＶＩＩＩ）の化合物、ポリカルボン酸、ハロゲン化カルボン酸及びカルボン酸の他の誘導体からなる群から選択されうる。
従って、一実施形態では、有機前駆体は一般式（ＶＩＩＩ）を有するカルボン酸である。
Ｒ５－ＣＯＯＨ （ＶＩＩＩ）
式中、Ｒ５は、水素又はメチル、エチル、プロピル、ブチル、ペンチル又はヘキシル、例えば、メチル又はエチルなどの直鎖もしくは分岐鎖Ｃ１－Ｃ２０アルキル又はアルケニル基である。いくつかの実施形態では、Ｒ５は、直鎖又は分岐鎖Ｃ１－Ｃ３アルキル又はアルケニル基である。式（ＶＩＩ）による化合物の例は、ギ酸、プロパン酸及び酢酸であり、いくつかの実施形態ではギ酸（ＨＣＯＯＨ）である。
本開示のいくつかの実施形態では、基材を第二の気相反応物質に曝露すること、すなわち接触させることは、第二の気相反応物質を基材上で０．１秒～２．０秒、又は約０．０１秒～約１０秒、又は約２０秒未満、約１０秒未満、又は約５秒未満の時間、パルスすることを含む。基材上で第二の気相反応物質をパルスする間、第二の気相反応物質の流量は、５０ｓｃｃｍ未満、又は２５ｓｃｃｍ未満、又は１５ｓｃｃｍ未満、又は更には１０ｓｃｃｍ未満であり得る。
例えば、パージガスのパルス注入及び／又は排気系により生成された真空により、基材の表面から過剰な第二の気相反応物質及び反応副生成物がある場合には、それらを除去してもよい。パージガスは、これらに限定されないが、アルゴン（Ａｒ）、窒素（Ｎ２）、ヘリウム（Ｈｅ）などの任意の不活性ガスであることが好ましく、又は場合によっては、水素（Ｈ２）を使用することもできる。一つの段階は、パージ（すなわち、パージガスパルス）または他の反応物質除去ステップが介在する場合、一般に別の段階の直後に続くと考えられる。
基材を第一の気相反応物質（すなわち、金属ハロゲン化物化合物）及び第二の気相反応物質（例えば、酸素前駆体）と交互に接触させる堆積サイクルは、所望の厚さの遷移金属含有膜が堆積されるまで一回又は複数回繰り返されてもよい。当然のことながら、本開示のいくつかの実施形態では、基材を第一の気相反応物質及び第二の気相反応物質と接触させる順序は、基材を最初に第二の気相反応物質と接触させるのに続いて、第一の気相反応物質と接触させる順序であってもよい。更に、いくつかの実施形態では、周期的堆積プロセスは、基材を第二の気相反応物質と一回又は複数回接触させる前に、基材を第一の気相反応物質と一回又は複数回接触させることを含むことができ、あるいは同様に、基材を第一の気相反応物質と一回又は複数回接触させる前に、基材を第二の気相反応物質と一回又は複数回接触させることを含むことができる。
更に、本開示のいくつかの実施形態は、プラズマ反応物質を含まなくてもよく、例えば第一及び第二の気相反応物質はイオン化された反応種を実質的に含まない。いくつかの実施形態では、第一及び第二の気相反応物質は、イオン化反応種、励起種及びラジカル種を実質的に含まない。例えば、第一の気相反応物質及び第二の気相反応物質の両方は、下地の基材のイオン化損傷及びそれにより生成される関連する欠陥を防止するために、プラズマ反応物質を含まないことができる。非プラズマ反応物質の使用は、高エネルギーのプラズマ種がデバイスの性能特性を損傷及び／又は劣化させる可能性があるので、下層の基材が、壊れやすい製造、又は少なくとも部分的に製造された半導体デバイス構造を含む場合に、特に有用でありうる。
本開示のいくつかの実施形態では、本開示の例示的な周期的堆積方法は、還元剤を含む第三の気相反応物質と基材を接触させることを含む、追加的なプロセス工程を含み得る。いくつかの実施形態では、還元剤は、水素（Ｈ２）、水素（Ｈ２）プラズマ、アンモニア（ＮＨ３）、アンモニア（ＮＨ３）プラズマ、ヒドラジン（Ｎ２Ｈ４）、シラン（ＳｉＨ４）、ジシラン（Ｓｉ２Ｈ６）、トリシラン（Ｓｉ３Ｈ８）、ゲルマン（ＧｅＨ４）、ジゲルマン（Ｇｅ２Ｈ６）、ボラン（ＢＨ３）、ジボラン（Ｂ２Ｈ６）、第三級ブチルヒドラジン（Ｃ４Ｈ１２Ｎ２、セレン前駆体、ホウ素前駆体、亜リン酸前駆体、硫黄前駆体、有機前駆体（例えば、アルコ－ル、アルデヒド、又はカルボン酸類）又は水素前駆体のうちの少なくとも一つを含んでもよい。本開示のいくつかの実施形態では、本開示の例示的な周期的堆積方法は、還元剤である第二の気相反応物質と基材を接触させることを含み得る（任意の追加的な前駆体／反応物質の接触工程なしで）。
還元剤を含む第三の気相反応物質は、反応チャンバーに導入され、例示的な周期的堆積方法のいくつかのプロセス段階で基材に接触してもよい。本開示のいくつかの実施形態では、還元剤は反応チャンバー内に導入され、第一の気相反応物質とは別個に、及び第二の気相反応物質とは別個に、基材と接触させることができる。例えば、基材を第一の気相反応物質と接触させる前に、基材を第一の気相反応物質と接触させた後かつ基材を第二の気相反応物質と接触させる前に、及び／又は基材を第二の気相反応物質と接触させた後に、還元剤を反応チャンバーに導入し、基材と接触させてもよい。本開示のいくつかの実施形態では、還元剤は反応チャンバー内に導入され、第一の気相反応物質と同時に、及／又は第二の気相反応物質と同時に、基材と接触させることができる。例えば、還元剤及び第一の気相反応物質は、反応チャンバー内に同時に流れ込み、同時に基材に接触することができ、及び／又は還元剤及び第二の気相反応物質は、反応チャンバー内に同時に流れ込み、同時に基材に接触することができる。
本開示のいくつかの実施形態では、第一の気相反応物質は、遷移金属ハロゲン化物化合物を含んでもよく、第二の気相反応物質は、酸素前駆体を含んでもよい。このような実施形態では、周期的堆積プロセスは、基材上に遷移金属酸化物を堆積し得る。非限定的な例として、第一の気相の反応物質は、ＣｏＣｌ２（ＴＭＥＤＡ）を含んでもよく、第二の気相反応物質は、水（Ｈ２Ｏ）を含んでもよく、基材上に堆積した膜は、酸化コバルトを含んでもよい。いくつかの実施形態では、遷移金属酸化物は、遷移金属酸化物を還元剤に曝すことによって更に処理されてもよい。いくつかの実施形態では、遷移金属酸化物は、フォーミングガス（Ｈ２＋Ｎ２）、アンモニア（ＮＨ３）、ヒドラジン（Ｎ２Ｈ４）、水素分子（Ｈ２）、水素原子（Ｈ）、水素プラズマ、水素ラジカル、水素励起種、アルコール、アルデヒド、カルボン酸、ボラン、又はアミンを含む、少なくとも一つの還元剤に曝されてもよい。
いくつかの実施形態では、遷移金属酸化物を還元剤に曝すことで、遷移金属酸化物を元素遷移金属に還元することができる。非限定的な例として、本開示の周期的堆積プロセスを利用して、酸化コバルト膜を５０ナノメ－トルの厚さに堆積させ、酸化コバルト膜を１０００ミリバールの圧力及び約２５０℃の温度で１０％のフォーミングガスに曝し、酸化コバルト膜を元素コバルトに還元することができる。本開示のいくつかの実施形態では、遷移金属酸化物は、５００ナノメ－トル未満、又は１００ナノメ－トル未満、又は５０ナノメ－トル未満、又は２５ナノメ－トル未満、又は２０ナノメートル未満、又は１０ナノメートル未満、又は更には５ナノメ－トル未満の厚さを有し得る。いくつかの実施形態では、遷移金属酸化物は、５時間未満、又は１時間未満、又は３０分未満、又は１５分未満、又は１０分未満、又は５分未満、又は更には１分未満、還元剤に曝されてもよい。いくつかの実施形態では、遷移金属酸化物は、５００℃未満、又は４００℃未満、又は３００℃未満、又は２５０℃未満、又は２００℃未満、又は更には１５０℃未満の基材温度で、還元剤に曝されてもよい。いくつかの実施形態では、遷移金属酸化物は、減圧雰囲気中で還元剤に曝されてもよく、圧力は、約０．００１ミリバール～約１０バール、又は約１ミリバール～約１０００ミリバールであってもよい。
遷移金属ハロゲン化物化合物を含む第一の気相反応物質及び遷移金属含有膜を堆積するための第二の気相反応物質を利用する、本明細書に記載される周期的堆積プロセスは、加熱された基材を用いてＡＬＤ又はＣＶＤ堆積システムで実施され得る。例えば、いくつかの実施形態では、方法は、基材を約８０℃～約１５０℃の温度に加熱すること、又は更に基材を約８０℃～約１２０℃の温度に加熱することを含み得る。もちろん、任意の所定の周期的堆積プロセス、例えばＡＬＤ反応等の適切な温度ウィンドウは、表面終端及び含まれる反応物質種に依存するであろう。ここで、温度は、使用される前駆体に応じて変化し、一般に約７００℃以下である。いくつかの実施形態では、蒸着プロセスの場合、堆積温度は一般に約１００℃以上であり、いくつかの実施形態では、堆積温度は約１００℃～約３００℃であり、いくつかの実施形態では、堆積温度は約１２０℃～約２００℃である。いくつかの実施形態では、堆積温度は約５００℃未満、又は約４００℃より低く、又は約３５０℃より低く、又は約３００℃より低い。場合によっては、堆積温度は約３００℃より低く、約２００℃より低く、又は約１００℃より低くてもよい。場合によっては、堆積温度は、約２０℃を超え、約５０℃を超え、及び約７５℃を超えてもよい。本開示のいくつかの実施形態では、堆積温度は、すなわち堆積中の基材の温度は約２７５℃である。
いくつかの実施形態では、遷移金属含有膜の成長速度は、約０．００５Å／サイクル～約５Å／サイクル、約０．０１Å／サイクル～約２．０Å／サイクルである。いくつかの実施形態では、遷移金属含有膜の成長速度は、約０．０５Å／サイクルより大きい、約０．１Å／サイクルより大きい、約０．１５Å／サイクルより大きい、約０．２０Å／サイクルより大きい、約０．２５Å／サイクルより大きい、又は約０．３Å／サイクルより大きい。いくつかの実施形態では、遷移金属含有膜の成長速度は、約２．０Å／サイクル未満、約１．０Å／サイクル未満、約０．７５Å／サイクル未満、約０．５Å／サイクル未満、又は０．２Å／サイクル未満である。本開示のいくつかの実施形態では、遷移金属含有膜の成長速度は約０．４Å／サイクルであり得る。
本開示の実施形態は、図１の例示的な周期的堆積方法１００により詳細に例示されることができる周期的堆積を含むことができる。方法１００は、少なくとも一つの基材を反応チャンバー内に供給すること、及び基材を堆積温度に加熱することを含む、プロセスブロック１１０によって開始することができる。例えば、基材は、一つ又は複数の部分的に製造された半導体デバイス構造を含んでもよく、反応チャンバーは、原子層堆積反応チャンバーを備えてもよく、基材は約２７５℃未満の堆積温度に加熱されてもよい。加えて、反応チャンバー内の圧力を制御して、反応チャンバー内の雰囲気を減少させることができる。例えば、周期的堆積プロセスの間の反応チャンバー内の圧力は、１０００ミリバール未満、又は１００ミリバール未満、又は１０ミリバール未満、又は５ミリバール未満、又は更に、一部の場合、１ミリバール未満であってもよい。
方法１００は、基材を遷移金属ハロゲン化物化合物に接触させることを含む、プロセスブロック１２０を継続してもよく、例えば、基材を遷移金属ハロゲン化物化合物に、約１秒の間、接触させてもよい。本開示のいくつかの実施形態では、遷移金属化合物は、約０．０１秒～約６０秒の間、約０．０５秒～約１０秒の間、又は約０．１秒～約５秒の間、基材に接触することができる。更に、基材上に遷移金属前駆体をパルス注入する間、遷移金属前駆体の流量は、２０００ｓｃｃｍ未満、又は１０００ｓｃｃｍ未満、又は５００ｓｃｃｍ未満、又は２００ｓｃｃｍ未満、又は更に１００ｓｃｃｍ未満であることができる。
基材を遷移金属ハロゲン化物化合物と接触させると、過剰な金属前駆体及びあらゆる反応副生成物は、パージ／排気プロセスによって反応チャンバーから除去されることができる。
方法１００は、例えば、酸素前駆体、窒素前駆体、ケイ素前駆体、リン前駆体、セレン前駆体、ホウ素前駆体、又は還元剤など、第二の気相反応物質と基材を接触させることを含む、プロセスブロック１３０を続けることができる。第二の気相反応物質、例えば、水は、基材におよそ４秒間接触してもよい。本開示のいくつかの実施形態では、第二の気相反応物質は、約０．０１秒～約６０秒の間、又は約０．０５秒～約１０秒の間、又は約０．１秒～約５．０秒の間、基材に接触することができる。更に、基材上で第二の気相反応物質をパルスする間、第二の気相反応物質の流量は、２０００ｓｃｃｍ未満、又は１０００ｓｃｃｍ未満、又は５００ｓｃｃｍ未満、又は２００ｓｃｃｍ未満、又は更には１００ｓｃｃｍ未満であり得る。
基材を第二の気相反応物質前駆体と接触させると、過剰な第二の気相反応物質及び任意の反応副生成物は、パージ／排気プロセスによって反応チャンバーから除去されることができる。
基材が遷移金属ハロゲン化物化合物（プロセスブロック１２０）と交互にかつ連続的に接触し、第二の気相反応物質（プロセスブロック１３０）と接触する、例示的な周期的堆積方法１００は、一つの堆積サイクルを構成してもよい。本開示のいくつかの実施形態では、遷移金属含有膜を堆積させる方法は、堆積サイクルを一回又は複数回繰り返すことを含むことができる。例えば、方法１００は、周期的堆積方法１００がプロセスブロック１５０を介して継続又は終了するかどうかを判断する決定ゲート１４０を継続してもよい。決定ゲート１４０は、堆積した遷移金属含有膜の厚さに基づいて決定され、例えば、遷移金属含有膜の厚さが所望のデバイス構造に対して不十分である場合、方法１００はプロセスブロック１２０に戻り、基材を遷移金属ハロゲン化物化合物と接触させ、そして基材を第二の気相反応物質と接触させるプロセスを一回又は複数回繰り返してもよい。遷移金属含有膜が所望の厚さに堆積すると、方法はプロセスブロック１５０を介して終了し、遷移金属含有膜及び下層の半導体構造は、追加のプロセスを施して、一つ又は複数のデバイス構造を形成することができる。
本明細書に記載のいくつかの実施形態に従って堆積させた遷移金属を含む膜又は層は、連続性薄膜であってもよい。いくつかの実施形態では、本明細書に記載のいくつかの実施形態に従って堆積させた遷移金属を含む薄膜は、約１００ナノメ－トル未満、又は約６０ナノメ－トル未満、又は約５０ナノメ－トル未満、又は約４０ナノメ－トル未満、又は約３０ナノメ－トル未満、又は約２５ナノメ－トル未満、又は約２０ナノメ－トル未満、又は約１５ナノメ－トル未満、又は約１０ナノメ－トル未満、又は約５ナノメ－トル未満、又は更に薄い厚さで連続的であってもよい。本明細書で言及される連続性は、物理的連続性又は電気的連続性であることができる。いくつかの実施形態では、膜が物理的に連続し得る厚さは、膜が電気的に連続する厚さと同じでなくてもよく、膜が電気的に連続し得る厚さは、膜が物理的に連続している厚さと同じでなくてもよい。
いくつかの実施形態では、本明細書に記載のいくつかの実施形態に従って堆積させた遷移金属含有膜は、約２０ナノメートル～約１００ナノメートルの厚さを有することができる。いくつかの実施形態では、本明細書に記載のいくつかの実施形態に従って堆積させた遷移金属含有膜は、約２０ナノメートル～約６０ナノメートルの厚さを有することができる。いくつかの実施形態では、本明細書に記載のいくつかの実施形態に従って堆積させた遷移金属含有膜は、約２０ナノメートルを超える、又は約３０ナノメートルを超える、又は約４０ナノメートルを超える、又は約５０ナノメートルを超える、又は約６０ナノメートルを超える、又は約１００ナノメートルを超える、又は約２５０ナノメートルを超える、又は約５００ナノメートルを超える、又は更に大きい厚さを有することができる。いくつかの実施形態では、本明細書に記載のいくつかの実施形態に従って堆積させた遷移金属含有膜は、約５０ナノメートル未満、約３０ナノメートル未満、約２０ナノメートル未満、約１５ナノメートル未満、約１０ナノメートル未満、約５ナノメートル未満、約３ナノメートル未満、約２ナノメートル未満、又は約１ナノメートル未満の厚さを有することができる。
本開示のいくつかの実施形態では、遷移金属含有膜は、例えば高いアスペクト比特徴を含む非平面の基材などの三次元構造上に堆積し得る。いくつかの実施形態では、遷移金属含有膜のステップカバレージは、アスペクト比（高さ／幅）が約２より大きい、約５より大きい、約１０より大きい、約２５より大きい、約５０より大きい、又は更に約１００より大きい構造において、約５０％以上、又は約８０％以上、又は約９０％以上、又は約９５％以上、又は約９８％以上、又は約９９％以上、もしくはそれより大きくてもよい。
本開示のいくつかの実施形態では、本開示の実施形態に従って堆積させた遷移金属含有膜は、約５０原子％未満の酸素、約２５原子パーセント未満の酸素、約１０原子％未満の酸素、約５原子％未満の酸素、約２原子％未満の酸素、又は更に約１原子％未満の酸素を含み得る。別の実施形態では、遷移金属含有膜は、約５原子％未満の水素、又は約２原子％未満の水素、又は約１原子％未満の水素、又は更に約０．５原子％未満の水素を含むことができる。更に別の実施形態では、遷移金属含有膜は、約５原子％未満の炭素、又は約２原子％未満の炭素、又は約１原子％未満の炭素、又は更に約０．５原子％未満の炭素を含むことができる。更に別の実施形態では、遷移金属含有膜は、約５原子％未満のハロゲン化物種、又は約２原子％未満のハロゲン化物種、又は約１原子％未満のハロゲン化物種、又は更に約０．５原子％未満のハロゲン化物種を含むことができる。いくつかの実施形態では、遷移金属含有材料の原子％は、飛行時間測定弾性反跳粒子検出法（ＴｏＦ－ＥＲＤＡ）を利用して決定され得る。
本開示のいくつかの実施形態では、本開示の周期的堆積プロセスを利用して、例えば、酸化コバルトなどの遷移金属酸化物を堆積することができる。原子層堆積などの周期的堆積プロセスに利用される前のコバルト前駆体は、水（Ｈ２Ｏ）に対して非反応性であることが証明されているため、オゾン（Ｏ３）が酸素前駆体として、一般的に利用されてきた。しかしながら、酸化コバルトの周期的堆積のためのオゾンの使用は、典型的には、酸化コバルト（ＩＩ）（ＣｏＯ）ではなく、酸化コバルト（ＩＩ、ＩＩＩ）（Ｃｏ３Ｏ４）の形成をもたらす。いくつかの実施形態では、Ｃｏ３Ｏ４ではなく、ＣｏＯを堆積させることが有益であり得、例えば、ＣｏＯ形態のより低い酸化状態のコバルトは、より容易にコバルト金属に還元され得る。従って、本開示のいくつかの実施形態では、本開示の周期的堆積プロセスを利用して、実質的に酸化コバルト（ＩＩ）（ＣｏＯ）膜を堆積させることができ、すなわち、コバルト対酸素の比が１：１と実質的に等しい。本開示のいくつかの実施形態では、周期的堆積プロセスの間の堆積温度は、堆積された膜の化学量論に影響を与える可能性があ。例えば、本明細書に開示される周期的堆積プロセスを利用して酸化コバルト膜を堆積させる場合、基材温度は、堆積された膜内のコバルト対酸素（Ｃｏ：Ｏ）の比に影響を与え得る。従って、本開示の非限定的な例示的実施形態として、酸化コバルト膜は、ＣｏＣｌ２（ＴＭＥＤＡ）をコバルト前駆体として利用し、水（Ｈ２Ｏ）を酸素前駆体として利用して堆積され得る。このような周期的堆積プロセスの間、基材温度は約２７５℃に制御され得、コバルト対酸素の比（Ｃｏ：Ｏ）が約１：１の酸化コバルト（ＩＩ）（ＣｏＯ）の堆積を生じ得る。
本明細書に開示される周期的堆積プロセスによって堆積された遷移金属含有膜は、例えば、ライナー層、キャッピング層、ギャップ充填層、トレンチ充填層、シード層、コンタクト層／コンタクト充填層、電気移動改善層、バックエンド（ＢＥＯＬ）用途での導電性相互接続、及び半導体デバイス接点のシリサイド形態などの様々な状況で利用されてもよい。いくつかの実施形態では、本開示の遷移金属含有膜は、一つ又は複数のデバイス構造に電流を供給するように構成された電極、又は電極の少なくとも一部として利用されてもよい。本開示のいくつかの実施形態では、本開示の遷移金属含有膜は、一つ又は複数のＣＭＯＳデバイスへの電極の少なくとも一部として、ＣＭＯＳデバイス用途で利用され得る。
非限定的な例示的実施形態として、図２に示すように、例えば、コバルトなどの遷移金属含有膜は、バックエンド（ＢＥＯＬ）メタライゼーション用途でのバリア材料及び／又はキャッピング層として利用されてもよい。より詳細には、図２は、トランジスタ及びメモリ素子（図示せず）などの部分的に製作及び／又は製作された半導体デバイス構造を備え得る、基材２０２を備える、部分的に製作された半導体デバイス構造２００を示す。部分的に製作された半導体デバイス構造２００は、低誘電率材料、すなわちシリコン含有誘電体又は金属酸化物などの低ｋ誘電体を含み得る、基材２０２上に形成された誘電材料２０４を含み得る。トレンチは、誘電材料２０４内に形成されてもよく、バリア材料２０６は、金属相互接続材料２０８が周囲の誘電材料２０４の中へと拡散するのを防止又は実質的に防止するトレンチの表面上に配置されてもよい。本開示のいくつかの実施形態では、バリア材料２０６は、本明細書に記載の周期的堆積プロセスによって堆積されたコバルトを含み得る。本開示のいくつかの実施形態では、コバルト膜は、３５オングストローム未満、又は２５オングストローム未満、又は更に１５オングストローム未満の厚さを有してもよい。部分的に製作された半導体構造２００はまた、基材２０２内に配置された複数のデバイス構造を電気的に相互接続するための金属相互接続材料２０８を備えてもよい。いくつかの実施形態では、金属相互接続材料２０８は、銅、又はコバルトのうちの一つ又は複数を含んでもよい。バリア材料としてコバルトの使用に加えて、コバルトはキャッピング層としても利用されてもよい。従って、図２を参照すると、部分的に製作された半導体デバイス構造２００は、金属相互接続材料２０８の上面上に直接配置されるキャッピング層２１０も含みうる。キャッピング層２１０は、金属相互接続材料２０８の酸化を防止し、重要なことには、後続の製造プロセスで、すなわち、複数レベルの相互接続構造のために、部分的に製作された半導体構造２００の上に形成される追加的誘電材料への金属相互接続材料２０８の拡散を防止するために利用され得る。本開示のいくつかの実施形態では、キャッピング層２１０はまた、２０オングストローム未満、又は１５オングストローム未満、又は更に１０オングストローム未満の厚さを有するコバルトを含んでもよい。いくつかの実施形態では、金属相互接続材料２０８、バリア材料２０６、及びキャッピング層２１０は、基材２０２内に配置された複数の半導体デバイスの電気相互接続のための電極を集合的に形成してもよい。
本開示の実施形態は、例えば、原子層堆積、化学蒸着、及び周期化学気相堆積などの蒸着プロセスに有用な化学前駆体の合成にも利用され得る。従って、本開示の実施形態は、例えば、二座窒素含有付加配位子を含む、遷移金属ハロゲン化物など、本明細書において前述した通り、付加体形成配位子を含む遷移金属ハロゲン化物化合物を合成する方法を含み得る。いくつかの実施形態では、本開示の方法は、塩化コバルト（ＩＩ）（ＴＭＥＤＡ）、塩化ニッケル（ＩＩ）（ＴＭＥＤＡ）、又は塩化銅（ＩＩ）（ＴＭＥＤＡ）のうちの一つ又は複数を合成するために利用され得る。いくつかの実施形態では、本開示の方法は、ヨウ化コバルト（ＩＩ）（ＴＭＥＤＡ）、ヨウ化ニッケル（ＩＩ）（ＴＭＥＤＡ）、又はヨウ化銅（ＩＩ）（ＴＭＥＤＡ）のうちの一つ又は複数を合成するために利用され得る。いくつかの実施形態では、本開示の方法は、臭化コバルト（ＩＩ）（ＴＭＥＤＡ）、臭化ニッケル（ＩＩ）（ＴＭＥＤＡ）、又は臭化銅（ＩＩ）（ＴＭＥＤＡ）のうちの一つ又は複数を合成するために利用され得る。更に、いくつかの実施形態では、本開示の方法は、塩化コバルト（ＩＩ）（ＴＭＰＤＡ）、塩化ニッケル（ＩＩ）（ＴＭＰＤＡ）、及び塩化銅（ＩＩ）（ＴＭＰＤＡ）を合成するために利用され得る。
以下の記載は、ＣｏＣｌ２（ＴＭＥＤＡ）の合成方法を開示し、ＣｏＣｌ２（ＴＭＥＤＡ）の合成のために開示された方法は、本明細書に開示される追加の遷移金属ハロゲン化物化合物の合成方法に等しく適用可能であり、限定として解釈されるべきではないことを理解されたい。
薬剤前駆体合成方法は、標準シュレンクテクニック（Ｓｃｈｌｅｎｋ ｔｅｃｈｎｉｑｕｅｓ）と不活性ガス（例えば、Ｎ２又はＡｒ）グローブボックスを使用して、空気と水分を厳密に排除して行われるすべての取り扱いと操作で実行され得る。無水ＣｏＣｌ２（９９％）及びＮ，Ｎ，Ｎ’，Ｎ’－テトラメチルエチレンジアミン（ＴＭＥＤＡ）（９９％）を反応物質として利用した。加えて、ジクロロメタン（ＣＨ２Ｃｌ２）は、適切な溶媒として利用され、このプロセスは４Å以上の分子ふるいで、ＣＨ２Ｃｌ２を脱酸素化及び乾燥させることを含む。
本開示のいくつかの実施形態では、ある量のＣｏＣｌ２を量り、シュレンク瓶と同じような適切な容器に加えることができる。ある量のＣＨ２Ｃｌ２を、ＣｏＣｌ２に追加できる。その後、化学量論量のＴＭＥＤＡを溶液に滴下してもよい。いくつかの実施形態では、付加体形成配位子、例えば、ＴＭＥＤＡは、例えば、ハロゲン化物化合物の量よりも、２倍、又は５倍、又は更に１０倍多い量など、ハロゲン化物化合物を上回って添加され得る。得られた懸濁液は、室温で約１時間攪拌され得る。非限定的な例として、６．００ｇ（４６．２１１ｍｍｏｌ）のＣｏＣｌ２を計量し、１００ｍｌのＣＨ２Ｃｌ２と共にシュレンク瓶に追加してもよい。５．３７ｇ（４６．２１１ｍｍｏｌ）のＴＭＥＤＡを溶液に加え、室温で１時間攪拌してもよい。得られた青色溶液を蒸発乾燥させ、青色の生成物を生成することができる。得られた生成物は、昇華器に移動され、生成物は、約１５０～２００℃の温度で昇華され、それによっててＣｏＣｌ２（ＴＭＥＤＡ）を生成することができる。本開示のいくつかの実施形態では、得られた揮発性遷移金属ハロゲン化物化合物、例えば、ＣｏＣｌ２（ＴＭＥＤＡ）は、５ａｔ％未満、又は２ａｔ％未満、又は１ａｔ％未満、又は０．１ａｔ％未満、又は更に０．０１ａｔ％未満の割合の不純物濃度を有することができる。本開示のいくつかの実施形態では、揮発性遷移金属ハロゲン化物化合物は、有機遷移金属前駆体と比較して、より高い分解温度を有することができる。例えば、本開示の遷移金属ハロゲン化物化合物は、１５０℃より大きい、又は２００℃よりも更に高い分解温度を有し得る。
従って、本開示のいくつかの実施形態では、遷移金属含有膜の蒸着に利用され得る、遷移金属ハロゲン化物化合物が合成され得る。いくつかの実施形態では、付加体形成配位子を含む金属ハロゲン化物化合物は、遷移金属ハロゲン化物化合物及び付加体形成配位子を、約５０℃未満、又は約３０℃未満、又は更に約１５℃未満の温度で組み合わせることを含む、ワンステップ合成プロセスを利用して合成することができ、合成プロセス全体は、５時間未満、又は２時間未満、又は１時間未満、又は更に３０分未満の時間で完了することができる。
本開示の実施形態はまた、遷移金属ハロゲン化物化合物を収容するように、及び遷移金属ハロゲン化物化合物を反応チャンバーに供給するように構成された一つ又は複数の前駆体供給源容器を含む蒸着装置も含み得る。従って、本開示のいくつかの実施形態では、反応性揮発性化学物質を利用する蒸着装置を提供する。装置は、反応チャンバー、反応チャンバー内に配置された基材、反応チャンバーと流体連通する前駆体供給源容器、及び前駆体供給源容器内に配置された二座窒素含有配位子を含む遷移金属ハロゲン化物化合物を含み得る。
より詳細には、図４は、反応チャンバー４０２を含む、蒸着装置４００を概略的に示す。図４は、蒸着装置４００の簡略化された概略バージョンであり、本開示の蒸着装置４００で利用され得るありとあらゆる要素、すなわち、これらに限定されないが、バルブ、電気接続、マスフローコントローラ、シール、及びガス導管などを含まないことに留意されたい。本開示のいくつかの実施形態では、反応チャンバー４０２は、反応チャンバー内の基材４０６を保持するように構成されたサセプタ４０４を含み得る。また、反応チャンバー内に配置されるのは、基材を様々なガスに選択的に曝すために利用されるシャワーヘッドガス分配器４０８である。
本開示のいくつかの実施形態では、前駆体供給源容器４１０Ａは、導管又は他の適切な手段４１２Ａを介して反応チャンバー４０２に流体連通していてもよく、更に、マニホールド、バルブ制御システム、質量流量制御システム、又は機構に連結されて、前駆体供給源容器４１０Ａに由来する気体前駆体を制御してもよい。前駆体供給源容器４１０Ａは、二座窒素含有配位子を含む遷移金属ハロゲン化物化合物を貯蔵するように構成されてもよい。いくつかの実施形態では、前駆体供給源容器４１０Ａは、前駆体供給源容器４１０Ａ内に貯蔵される遷移金属ハロゲン化物化合物に対して実質的に化学的に不活性であり得る、石英材料を含んでもよい。本開示の代替実施形態では、前駆体供給源容器４１０Ａは、例えば、ハステロイ、モネルまたはそれらの組み合わせなど、耐食性金属または金属合金より製作されてもよい。
本開示のいくつかの実施形態では、前駆体供給源容器４１０Ａは、前駆体供給源容器４１０Ａに貯蔵された遷移金属ハロゲン化物化合物を加熱するように構成された、一つ又は複数の加熱部４１４を更に備えてもよい。いくつかの実施形態では、一つ又は複数の加熱部４００は、約０℃を超える、又は約２０℃を超える、又は約１００℃を超える、又は約１５０℃を超える、又は約２００℃を超える、又は約２００℃を超える、又は約３００℃を超える、又は更に約４００℃を超える温度まで、遷移金属ハロゲン化物化合物を加熱するように利用されてもよい。いくつかの実施形態では、一つ又は複数の加熱部４１４は、前駆体供給源容器４１０Ａに貯蔵された遷移金属ハロゲン化物化合物を、約１７０℃の温度まで加熱するように構成されてもよい。
いくつかの実施形態では、前駆体供給源容器４１０Ａと関連付けられる一つ又は複数の加熱部４１４は、遷移金属ハロゲン化物化合物を固体から液体又は気体のいずれかに変換するように構成される。いくつかの実施形態では、前駆体供給源容器４１０Ａと関連付けられる一つ又は複数の加熱部４１４は、前駆体貯蔵容器４１０Ａ内に貯蔵された遷移金属ハロゲン化物化合物の粘性を制御するために利用されてもよい。いくつかの実施形態では、前駆体供給源容器４１０Ａと関連付けられる一つ又は複数の加熱部４１４は、前駆体供給源容器内に貯蔵された遷移金属ハロゲン化物化合物によって生成された蒸気圧を制御するように構成されてもよい。本開示のいくつかの実施形態では、遷移金属ハロゲン化物化合物は、２５℃よりも高い、又は５０℃よりも高い、又は更に１００℃よりも高い温度で、０．０１ミリバールを超える蒸気圧を有してもよい。本開示のいくつかの実施形態では、遷移金属ハロゲン化物化合物は、３５０℃未満、又は２５０℃未満、又は２００℃未満、又は更に１５０℃未満の温度で、０．０１ミリバールを超える蒸気圧を有してもよい。本開示のいくつかの実施形態では、遷移金属ハロゲン化物化合物は、２５℃よりも高い、又は更に１００℃よりも高い温度で、０．１ミリバールを超える蒸気圧を有してもよい。本開示のいくつかの実施形態では、遷移金属ハロゲン化物化合物は、４００℃未満、又は２００℃未満、又は更に１００℃未満の温度で、０．１ミリバールを超える蒸気圧を有してもよい。本開示のいくつかの実施形態では、２５℃より高い、又は更に１００℃より高い温度で、１ミリバールを超える蒸気圧を有してもよい。例えば、遷移金属ハロゲン化物化合物を、１５０℃より高い温度まで加熱し、０．００１ミリバールを超える蒸気圧を発生させることができる。
いくつかの実施形態では、前駆体供給源容器４１０Ａ内に貯蔵された遷移金属ハロゲン化物４１６は、塩化コバルト（ＴＭＥＤＡ）、又は塩化ニッケル（ＴＭＥＤＡ）のうちの少なくとも一つを含み得る。いくつかの実施形態では、前駆体供給源容器４１０Ａ内に貯蔵された遷移金属ハロゲン化物４１６は、ヨウ化コバルト（ＴＭＥＤＡ）を含み得る。いくつかの実施形態では、前駆体供給源容器４１０Ａ内に貯蔵された遷移金属ハロゲン化物４１６は、含み得る。更に、いくつかの実施形態では、前駆体供給源容器４１０Ａ内に貯蔵された遷移金属ハロゲン化物４１６は、塩化コバルト（ＴＭＰＤＡ）、及び塩化ニッケル（ＴＭＰＤＡ）を含み得る。
本開示のいくつかの実施形態では、蒸気通路４１８は、一つまたは複数のキャリアガスが、キャリアガス貯蔵容器（図示せず）から蒸気通路４１８を介して前駆体供給源容器の中へ移送されてもよいように、前駆体供給源容器４１０Ａに接続されてもよい。いくつかの実施形態では、マスフローコントローラ（図示せず）を蒸気通路４１８上に配置し、前駆体供給源容器４１０Ａに近接して配置してもよい。例えば、マスフローコントローラは、前駆体供給源容器４１０Ａに入るキャリアガスの質量流束を制御するように較正されてもよく、それによって、前駆体供給源容器４１０Ａから反応チャンバー４０２への遷移金属ハロゲン化物化合物蒸気のその後の流れに対するより大きな制御が可能になる。
いくつかの実施形態では、キャリアガス（例えば、水素、窒素、ヘリウム、アルゴン、及びそれらの混合物）は、遷移金属ハロゲン化物化合物４１６の露出した表面上に流れることができ、それによって、蒸気の一部を遷移金属ハロゲン化物化合物４１６から拾い上げ、遷移金属ハロゲン化物化合物を、キャリアガスと共に、反応チャンバー４０２に移送する。本開示の代替的実施形態では、キャリアガスは、例えば、任意の蒸気通路４１８’によって、遷移金属ハロゲン化物化合物４１６を通して、「バブリング」されてもよく、それによって、遷移金属ハロゲン化物化合物４１６の一部を撹拌及び拾い上げ、遷移金属ハロゲン化物化合物を、ガス導管４１２Ａを介して反応チャンバー４０２に移送する。
本開示のいくつかの実施形態では、蒸着装置４００は、追加の前駆体供給源容器及び不活性パージガス用の一つ又は複数の供給源容器を含み得る。例えば、前駆体供給源容器４１０Ｂは、例えば、酸素前駆体、窒素前駆体、硫黄前駆体、セレン前駆体、リン前駆体、ホウ素前駆体、ケイ素前駆体、又は還元剤のうちの一つ又は複数などの第二の気相反応物質を含むように構成されてもよい。前駆体供給源容器４１０Ｂに含まれる第二の気相反応物質は、ガス導管４１２Ｂを介して反応チャンバー４０２へ移送されてもよい。いくつかの実施形態では、前駆体供給源容器４１０Ｂは、更に、前駆体供給源容器４１０Ｂ内に貯蔵された前駆体の温度を制御するための関連付けられたヒーター４１４を有してもよい。更に、供給源容器４１０Ｃは、例えば、限定されないが、アルゴン（Ａｒ）、窒素（Ｎ２）、又はヘリウム（Ｈｅ）などの不活性パージガスを含むように利用されてもよい。蒸着システム４００は三つの供給源容器を含むが、追加的な化学前駆体を含む追加的な供給源容器は、反応チャンバー４０２で使用するように構成され得ることを理解されたい。
本開示のいくつかの実施形態では、蒸着装置４００は、バルブ、マニホールド、ポンプ、及び蒸着装置４００と関連付けられたその他の機器を選択的に動作させるための電子回路及び機械的構成要素を提供する、システム動作及び制御機構４２０を更に備えてもよい。このような回路及び化合物は、それぞれの前駆体供給源容器４１０Ａ、４１０Ｂ、及びパージガス容器４１０Ｃから、前駆体、パージガスを導入するように動作する。システム動作及び制御機構４２０はまた、ガスパルスシーケンスのタイミング、基材及び反応チャンバーの温度、反応チャンバーの圧力、並びに蒸着装置４００に適切な動作を提供するのに必要な様々な他の動作を制御し得る。動作及び制御機構４２０は、反応チャンバー４０２内外への前駆体、反応物質、及びパージガスの流れを制御するための制御ソフトウェア及び電気的又は空気制御バルブを含むことができる。制御システムは、特定のタスクを実行するソフトウェア及び／又はハードウェアコンポーネント、例えばＦＰＧＡ又はＡＳＩＣ等のモジュールを含むことができる。モジュールは、大胆には、制御システムのアドレス指定可能な記憶媒体上に存在するように構成され、一つ又は複数のプロセスを実行するように構成され得る。
関連技術分野の当業者は、異なる数及び種類の前駆体反応物質源及びパージガス源を備える本蒸着装置の他の形態が可能であることを理解する。更に、このような当業者はまた、反応チャンバー４０２の中へ選択的にガスを供給するという目的を達成するために使用され得るバルブ、導管、前駆体原料、パージガス源の多くの配置があることを理解するであろう。更に、蒸着装置の略図として、説明を簡単にするために多くの構成要素を省略する。このような構成要素としては、例えば、様々なバルブ、マニホールド、浄化装置、ヒーター、容器、通気孔、及び／又はバイパス等を挙げることができる。
図４の蒸着装置４００は、蒸着ツールに二座窒素含有付加配位子を含む遷移金属ハロゲン化物化合物を供給するために利用され得る。方法は、遷移金属ハロゲン化物化合物を含むように構成された前駆体供給源容器を提供することと、前駆体供給源容器を反応チャンバーに流体接続することと、前駆体供給源容器内に含まれる遷移金属ハロゲン化物化合物を１５０℃を超える温度に加熱することと、少なくとも０．００１ミリバールの遷移金属ハロゲン化物化合物の蒸気圧を生成することと、遷移金属ハロゲン化物化合物を反応チャンバーへ供給することと、を含み得る。本開示のいくつかの実施形態では、遷移金属ハロゲン化物化合物は、２５℃よりも高い、又は５０℃よりも高い、又は更に１００℃よりも高い温度で、０．０１ミリバールを超える蒸気圧を有してもよい。本開示のいくつかの実施形態では、遷移金属ハロゲン化物化合物は、３５０℃未満、又は２５０℃未満、又は２００℃未満、又は更に１５０℃未満の温度で、０．０１ミリバールを超える蒸気圧を有してもよい。本開示のいくつかの実施形態では、遷移金属ハロゲン化物化合物は、２５℃よりも高い、又は更に１００℃よりも高い温度で、０．１ミリバールを超える蒸気圧を有してもよい。本開示のいくつかの実施形態では、遷移金属ハロゲン化物化合物は、４００℃未満、又は２００℃未満、又は更に１００℃未満の温度で、０．１ミリバールを超える蒸気圧を有してもよい。本開示のいくつかの実施形態では、２５℃より高い、又は更に１００℃より高い温度で、１ミリバールを超える蒸気圧を有してもよい。
いくつかの実施形態では、遷移金属ハロゲン化物化合物は、塩化コバルト（ＴＭＥＤＡ）又は塩化ニッケル（ＴＭＰＤＡ）のうちの少なくとも一つを含むことができる。
上に記載した本開示の例示的実施形態は、添付の特許請求の範囲及びその法的等価物により定義される、本発明の実施形態の単なる例であるため、これらの実施形態によって本発明の範囲は限定されない。いかなる同等の実施形態も、本発明の範囲内にあることを意図している。実際に、記載した要素の代替の有用な組み合わせなど、本明細書に示し記載したものに加えて、本開示の様々な改変が、説明から当業者に明らかとなってもよい。このような改変及び実施形態もまた、添付の特許請求の範囲に入ると意図される。
２００ 半導体デバイス構造
２０２ 基材
２０４ 誘電材料
２０６ バリア材料
２０８ 金属相互接続材料
２１０ キャッピング層
４００ 蒸着装置
４０２ 反応チャンバー
４０４ サセプタ
４０６ 基材
４０８ シャワーヘッドガス分配器
４１０Ａ、４１０Ｂ 前駆体供給源容器
４１０Ｃ パージガス容器
４１２Ａ、４１２Ｂ 導管
４１４ 加熱部
４１６ 遷移金属ハロゲン化物
４１８ 蒸気通路
４２０ システム動作及び制御機構

Claims (28)

  1. 周期的堆積プロセスにより基材上に遷移金属含有膜を形成する方法であって、
    前記基材を、二座窒素含有付加配位子を含む遷移金属ハロゲン化物化合物を含む第一の気相反応物質と接触させることと、
    前記基材を第二の気相反応物質と接触させることとを含む、方法。
  2. 前記付加配位子が二つの窒素原子を含み、各々の窒素原子が少なくとも一つの炭素原子に結合されている、請求項１に記載の方法。
  3. 前記遷移金属ハロゲン化物化合物が遷移金属塩化物を含む、請求項１に記載の方法。
  4. 前記遷移金属塩化物化合物が、塩化コバルト、塩化ニッケル、又は塩化銅のうちの少なくとも一つを含む、請求項３に記載の方法。
  5. 前記遷移金属塩化物化合物が、塩化コバルト（ＴＭＥＤＡ）、又は塩化ニッケル（ＴＭＰＤＡ）のうちの少なくとも一つを含む、請求項４に記載の方法。
  6. 前記第二の気相反応物質が、オゾン（Ｏ３）、分子状酸素（Ｏ２）、酸素原子（Ｏ）、酸素プラズマ、酸素ラジカル、酸素励起種、水（Ｈ２Ｏ）、及び過酸化水素（Ｈ２Ｏ２）からなる群から選択される酸素前駆体を含む、請求項１に記載の方法。
  7. 前記遷移金属含有膜が、遷移金属酸化物を含む、請求項６に記載の方法。
  8. 前記遷移金属酸化物が、酸化コバルト（ＩＩ）（ＣｏＯ）を実質的に含む、請求項７に記載の方法。
  9. 前記遷移金属酸化物を還元剤前駆体と接触させることを更に含み、それによって元素遷移金属を形成する、請求項７に記載の方法。
  10. 前記還元剤前駆体が、フォーミングガス（Ｈ２＋Ｎ２）、アンモニア（ＮＨ３）、ヒドラジン（Ｎ２Ｈ４）、水素分子（Ｈ２）、水素原子（Ｈ）、水素プラズマ、水素ラジカル、水素励起種、アルコール、アルデヒド、カルボン酸、ボラン、又はアミンのうちの少なくとも一つを含む、請求項９に記載の方法。
  11. 第三級ブチルヒドラジン（Ｃ４Ｈ１２Ｎ２）、水素（Ｈ２）、水素（Ｈ２）プラズマ、アンモニア（ＮＨ３）、アンモニア（ＮＨ３）プラズマ、ヒドラジン（Ｎ２Ｈ４）、シラン（ＳｉＨ４）、ジシラン（Ｓｉ２Ｈ６）、トリシラン（Ｓｉ３Ｈ８）、ゲルマン（ＧｅＨ４）、ジゲルマン（Ｇｅ２Ｈ６）、ボラン（ＢＨ３）、及びジボラン（Ｂ２Ｈ６）からなる群から選択される還元剤前駆体を含む、第三の気相反応物質に前記基材を接触させることを更に含む、請求項１に記載の方法。
  12. 前記遷移金属含有膜が、元素コバルト、元素ニッケル、又は元素銅のうちの少なくとも一つを含む、請求項１に記載の方法。
  13. 前記周期的堆積プロセスが、原子層堆積プロセスを含む、請求項１に記載の方法。
  14. 前記周期的堆積プロセスが周期的化学気相堆積プロセスを含む、請求項１に記載の方法。
  15. 前記遷移金属含有膜が、元素遷移金属、遷移金属窒化物、遷移金属ケイ化物、遷移金属硫化物、遷移金属セレン化物、遷移金属リン化物、又は遷移金属ホウ化物のうちの少なくとも一つを含む、請求項１に記載の方法。
  16. 周期的堆積プロセスにより基材上に遷移金属含有膜を形成する方法であって、
    前記基材を付加体形成配位子を含む遷移金属化合物を含む第一の気相反応物質と接触させることと、
    前記基材を第二の気相反応物質と接触させることと、を含み、
    前記遷移金属が、銅（Ｃｕ）、ニッケル（Ｎｉ）、及びコバルト（Ｃｏ）からなる群から選択される、周期的堆積プロセスにより基材上に遷移金属含有膜を形成する方法。
  17. 前記付加体形成配位子が、窒素、リン、酸素、又は硫黄のうちの少なくとも一つを含む、請求項１６に記載の方法。
  18. 前記遷移金属化合物が、遷移金属塩化物、遷移金属ヨウ化物、遷移金属フッ化物、又は遷移金属臭化物からなる群から選択される、遷移金属ハロゲン化物化合物を含む、請求項１６に記載の方法。
  19. 前記遷移金属ハロゲン化物化合物が、二座窒素付加体形成配位子を含む、請求項１８に記載の方法。
  20. 前記遷移金属化合物が、塩化コバルト（ＴＭＥＤＡ）、臭化コバルト（ＴＭＥＤＡ）、ヨウ化コバルト（ＴＭＥＤＡ）、塩化コバルト（ＴＭＰＤＡ）、又は塩化ニッケル（ＴＭＰＤＡ）のうちの少なくとも一つを含む、請求項１６に記載の方法。
  21. 付加体形成配位子を含む前記遷移金属化合物が、遷移金属ハロゲン化物化合物及び付加体形成配位子を５０℃未満の温度で組み合わせることを含む、ワンステップ合成プロセスを利用して合成される、請求項１６に記載の方法。
  22. 前記第二の気相反応物質が、酸素前駆体、窒素前駆体、シリコン前駆体、硫黄前駆体、セレン前駆体、リン前駆体、ホウ素前駆体、又は還元剤のうちの少なくとも一つを含む、請求項１６に記載の方法。
  23. 請求項１に記載の方法に従い形成される、前記遷移金属含有膜を含むデバイス構造。
  24. 二座窒素含有付加配位子を含む遷移金属ハロゲン化物化合物を、反応チャンバーに供給するための方法であって、
    前記遷移金属ハロゲン化物化合物を収容するように構成された前駆体供給源容器を提供することと、
    前記反応チャンバーに前記前駆体供給源容器を流体連結させることと、
    前記前駆体供給源容器内に含まれる前記遷移金属ハロゲン化物化合物を５０℃より高い温度に加熱することと、
    少なくとも０．００１ミリバ－ルの前記遷移金属ハロゲン化物化合物の蒸気圧を生成することと、
    前記遷移金属ハロゲン化物化合物を前記反応チャンバーに供給することと、を含む、二座窒素含有付加配位子を含む遷移金属ハロゲン化物化合物を、反応チャンバーに供給するための方法。
  25. 前記遷移金属ハロゲン化物化合物が、塩化コバルト（ＴＭＥＤＡ）、塩化ニッケル（ＴＭＰＤＡ）のうちの少なくとも一つを含む、請求項２４に記載の方法。
  26. 反応性揮発性化学物質を利用する蒸着装置であって、
    反応チャンバーと、
    前記反応チャンバーに配置された基材と、
    前記反応チャンバーと流体連通する前駆体供給源容器と、
    前記前駆体供給源容器に配置された二座窒素含有付加配位子を含む、遷移金属ハロゲン化物化合物と、を備える、反応性揮発性化学物質を利用する蒸着装置。
  27. 前記遷移金属ハロゲン化物化合物が、塩化コバルト（ＴＭＥＤＡ）、又は塩化ニッケル（ＴＭＰＤＡ）のうちの少なくとも一つを含む、請求項２６に記載の装置。
  28. 前記遷移金属化合物が、１５０℃未満の遷移金属化合物温度で０．００１ミリバールを超える蒸気圧を示す、請求項２６に記載の装置。
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JP7391857B2 (ja) 2023-12-05
US10731249B2 (en) 2020-08-04
CN111684105A (zh) 2020-09-18
TW202244308A (zh) 2022-11-16
WO2019158995A3 (en) 2019-12-19
KR20200121798A (ko) 2020-10-26
US20200340113A1 (en) 2020-10-29
TW201934795A (zh) 2019-09-01
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