JP7373636B2 - 選択的パッシベーションおよび選択的堆積 - Google Patents
選択的パッシベーションおよび選択的堆積 Download PDFInfo
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- JP7373636B2 JP7373636B2 JP2022172419A JP2022172419A JP7373636B2 JP 7373636 B2 JP7373636 B2 JP 7373636B2 JP 2022172419 A JP2022172419 A JP 2022172419A JP 2022172419 A JP2022172419 A JP 2022172419A JP 7373636 B2 JP7373636 B2 JP 7373636B2
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Images
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Description
本出願は、2017年2月14日出願の米国仮特許出願第62/458,952号、2017年4月4日出願の第62/481,524号および2017年11月28日出願の第62/591,724号の優先権を主張するものである。
外国または国内での優先権を主張するすべての出願は、本出願と共に提出する出願データシートに特定され、それらを37 CFR 1.57の下、参照により本明細書に援用する。
半導体製造におけるデバイス寸法の縮小により、新しい革新的な加工方法が求められている。従来、半導体加工におけるパターニングは、ブランケット層を堆積させ、フォトリソグラフィー技術によってマスクし、マスクの中の開口部を通ってエッチングする、サブトラクティブ法を伴う。リフトオフ技術またはダマシンプロセスを使用するパターニングなど、マスキングステップが対象の材料の堆積に先行する、さらなるパターニングも知られている。ほとんどの場合、パターニングには高価な複数ステップのリソグラフィー技術が採用される。
本開示の一部態様により、選択的堆積を、第1表面に対して優先的に対象の膜を第2表面上に堆積させるように使用し得る。二つの表面は、第2表面に対する第1表面上へのポリマー層の選択的堆積など、それらの表面上に有機材料を選択的に形成することを可能にする、異なる材料特性を有することができ、それによって、それに続く対象の層の、有機パッシベーションされた第1層に対する第2表面上への選択的堆積を可能にする。
当業者は、選択的堆積が完全に選択的、または一部選択的であり得ることを理解するであろう。一部選択的なプロセスは、表面A全体から堆積した材料のすべてを除去することなく、表面B全体から堆積した材料のすべてを除去する、堆積後のエッチングによって、完全に選択的な層をもたらし得る。単純なエッチバックプロセスによって、高価なマスキングプロセスを必要とすることなく、完全に選択的な構造を残したままにし得るため、選択的堆積は、所望の利点を得るために、完全に選択的である必要はない。
図1A~1Dは、第2表面に対して第1表面を選択的にパッシベーションし、その後、パッシベーションされた第1表面に対する、第2表面上への選択的堆積が続く第1実施形態について、概略的に説明する。説明する実施形態では、第1表面は金属製材料を備え、第2表面は無機誘電材料を備え、第2表面上に堆積される対象の材料は、誘電材料を備える。
図2A~2Eは、第2表面に対して第1表面を選択的にパッシベーションし、その後、パッシベーションされた第1表面に対する、第2表面上への選択的堆積が続く第2実施形態について、概略的に説明する。説明する実施形態では、第1表面は無機誘電材料を備え、第2表面は金属製表面を備え、第2表面上に堆積する対象の材料は、誘電材料または金属を備える。
援用した2016年6月1日出願の米国特許出願第15/170,769号に開示されている通り、気相堆積技術は、有機パッシベーション層、ならびに例を挙げると、ポリイミド層、ポリアミド層、多尿症、ポリウレタン層、ポリチオフェン層およびその他などのポリマーに適用され得る。ポリマー層のCVDは、液体前駆体の適用と比較して、より優れた厚み制御、機械的柔軟性、共形カバレッジ(conformal coverage)および生体適合性を生み出し得る。ポリマーの逐次堆積加工によって、小さい研究規模の反応器において、高い成長率を生み出し得る。CVDと同様に、逐次堆積プロセスによって、より優れた厚み制御、機械的柔軟性および共形性を生み出し得る。用語「逐次堆積」および「周期的堆積」は、反応機構がALD、CVD、MLDまたはそれらの混成物に似ているかにかかわらず、基板が交互にまたは順次、異なる前駆体に曝露するプロセスに適用されるように、本明細書で用いられる。
式中、R1は、1~5個の炭素原子、2~5個の炭素原子、2~4個の炭素原子、5個以下の炭素原子、4個以下の炭素原子、3個以下の炭素原子または2個の炭素原子を備える脂肪族炭素鎖であってもよい。一部の実施形態では、反応物質または前駆体における炭素原子間の結合は、単結合、二重結合、三重結合またはそれらのある組み合わせであってもよい。それゆえ、一部の実施形態では、反応物質は2個のアミノ基を備えてもよい。一部の実施形態では、反応物質のアミノ基は、脂肪族炭素鎖上で一方または両方の末端位置を占有してもよい。しかしながら、一部の実施形態では、反応物質のアミノ基は、脂肪族炭素鎖上でどちらの末端位置も専有しなくてよい。一部の実施形態では、反応物質はジアミンを備える。一部の実施形態では、反応物質は、1,2-ジアミノエタン(ジアミノエタネル(diaminoethanel))、1,3-ジアミノプロパン(ジアミノプロパネル(diaminopropanel))、1,4-ジアミノブタン(ジアミノブタネル(diaminobutanel))、1,5-ジアミノペンタン(ジアミノペンタネル(diaminopentanel))、1,2-ジアミノプロパン(ジアミノプロパネル(diaminopropanel))、2,3-ブタンジアミン、2,2-ジメチル-1,3-プロパンジアミン(プロパンジアミネル(propanediaminel))の群より選択される有機前駆体を備えてもよい。
式中、R2は、1~3個の炭素原子、2~3個の炭素原子または3個以下の炭素原子を備える、脂肪族炭素鎖であってもよい。一部の実施形態では、反応物質または前駆体における炭素原子間の結合は、単結合、二重結合、三重結合またはそれらのある組み合わせであってもよい。一部の実施形態では、反応物質は塩化物を備えてもよい。一部の実施形態では、反応物質はジアシルクロリドを備えてもよい。一部の実施形態では、反応物質は、オキサリルクロリド(I)、マロニルクロリドおよびフマリルクロリドの群より選択される、有機前駆体を備えてもよい。
本明細書に記載する選択的堆積プロセスに従って、試料のポリイミド薄層を、いくつかの基板上に堆積させた。タングステン(W)特徴部と酸化シリコン表面とが交互になっている、200mmのシリコンウエハを基板として使用した。タングステン特徴部の幅は250nmで、ピッチはほぼ600nmである。ポリイミド堆積プロセスを、PRIクラスタツールと接続したPulsar 3000(登録商標)クロスフローALD反応器で実施した。
DAHを第1気相反応物質として、PMDAを第2気相反応物質として使用して、本明細書に記載するプロセスに従い、試料のポリイミド層を、タングステン(W)特徴部と酸化シリコン表面とを交互にパターニングした、200mmのシリコンウエハ上に選択的に堆積させた。第1反応物質DAHを、流量450sccmを有するN2キャリアガスによって、45℃で供給した。DAHのパルス時間は5秒、DAHの純時間は4秒であった。第2反応物質PMDAを、流量450sccmを有するN2キャリアガスによって、180℃で反応チャンバに供給した。PMDAのパルス時間は11秒、PMDAのパージ時間は4秒であった。反応温度は190℃であった。試料のポリイミド層を、1000回の堆積サイクルを使用して堆積させた。ポリイミドを約30nmの層厚で、W表面上に堆積させた。約4nmの実質的により少ない量のポリイミドを、酸化シリコン表面上に堆積させた。
援用した2016年5月5日出願の米国仮特許出願第62/332,396号に記載されている通り、本明細書に開示するパッシベーション層などの有機材料に対する、金属製材料、特に、金属酸化物の選択的堆積は、疎水性反応物質を用いて促進し得る。第1表面上にパッシベーション層を選択的に形成した後、一部の実施形態では、金属酸化物の金属を備える第1疎水性反応物質、および酸素を備える第2反応物質と基板を、交互かつ順次接触させることによって、金属酸化物を第2表面上に選択的に堆積させる。一部の実施形態では、第2反応物質は水である。一部の実施形態では、非有機層を第2表面上またはその上方に選択的に堆積させる(例えば、図1A~3Bを参照)以外は、図4Aの順序と同様に、第1および第2反応物質と基板を順次接触させる。
・ C1~C10の炭化水素(単結合、二重結合または三重結合)
o アルキル
・ C1~C5のアルキル
・ Me、Et、Pr、iPr、Bu、tBu
o アルケニル
・ C1~C6のアルケニル
o 環状炭化水素
・ C3~C8
・ シクロペンタジエニル
・ シクロヘプタジエニル
・ シクロヘプタトリエニル
・ シクロヘキシル
・ それらの誘導体
o 芳香族
・ C6の芳香環およびそれらの誘導体
o LnMXy、式中、
・ 一部の実施形態では、nは1~6であり、
・ 一部の実施形態では、nは1~4または3~4である。
・ 一部の実施形態では、yは0~2であり、
・ 一部の実施形態では、yは0~1である。
・ Lは疎水性リガンドであり、
・ 一部の実施形態では、LはCpまたはC1~C4のアルキルリガンドである。
・ Xは親水性リガンドであり、
・ 一部の実施形態では、Xはアルキルアミン、アルコキシドまたはハロゲン化物リガンドである。
・ Mは金属であり(群の13元素、B、Gaを含む)、
・ 一部の実施形態では、Mは+Iから最大+VIの酸化状態を有する。
o 一部の実施形態では、Mは+IVから+Vの酸化状態を有する。
・ 一部の実施形態では、Mは遷移金属であり得る。
o 一部の実施形態では、MはTi、Ta、Nb、W、Mo、Hf、Zr、VまたはCrである。
・ 一部の実施形態では、MはHf、Zr、TaまたはNbである。
・ 一部の実施形態では、MはZrである。
o 一部の実施形態では、MはCo、Fe、Ni、CuまたはZnである。
o 一部の実施形態では、金属はWでもMoでもない。
・ 一部の実施形態では、Mは希土類金属であり得る。
o 一部の実施形態では、MはLa、CeまたはYである。
・ 一部の実施形態では、Mは2~13の群からの金属であり得る。
o 一部の実施形態では、MはBa、Sr、Mg、CaまたはScである。
・ 一部の実施形態では、Mは貴金属ではない。
図5~7は、有機パッシベーション層に対して、無機誘電体上に金属酸化物を選択的に堆積させ得ることを説明する。実験では、無機パッシベーション層は、上記の通り選択的に形成され得る、堆積したポリマー、特にポリイミドを備える。
・ ビス(メチルシクロペンタジエニル)メトキシメチルジルコニウム(IV)と水(H2O)とを交互に堆積したZrO2であって、275~325℃の温度で、ポリイミドに対する選択性を、自然酸化物の上方の25nm超に維持
・ TiCl4と水とを交互に堆積したTiO2であって、ポリイミドに対する選択性を、250℃で約100サイクル、および300℃で100サイクルよりさらに多いサイクルに維持
・ ビス(メチルシクロペンタジエニル)メトキシメチルハフニウム(IV)と水(H2O)とを交互に堆積したものから堆積したHfO2であって、280℃の温度で、ポリイミドに対する選択性を、自然酸化物の上方の25nm超に維持
上で述べた通り、自己組織化単分子層(SAM)は、有機パッシベーション層の堆積を阻害する働きをし、それゆえ、他の表面上への有機パッシベーション層の選択的堆積を促進し得る。それゆえ、用語「遮断」は単に標識であり、100%非活性化の有機パッシベーション層の堆積を必ずしも暗示していない。本明細書の他の部分で述べる通り、不完全な選択性でも、エッチバックプロセス後に、完全に選択的な構造を得るのに充分であり得る。
図11~15は、パッシベーション遮断層に対する、誘電材料上での有機パッシベーション層の選択的形成を、パッシベーション遮断層により促進し得ることを説明する。
本明細書に記載する選択的堆積プロセスで使用してもよい、好適な反応器の例は、アリゾナ州フェニックスのASM America, Inc.、およびオランダ、アルメレのASM Europe B.V.より入手可能な、F-120(登録商標)反応器、Pulsar(登録商標)反応器、例を挙げると、Pulsar 3000(登録商標)またはPulsar 2000(登録商標)、およびAdvance(登録商標)400 Series反応器などの市販のALD機器を含む。これらのALD反応器に加えて、CVD反応器、VDP反応器およびMLD反応器を含む、有機パッシベーション層の成長を可能にする多くの他の種類の反応器を用い得る。
図17を参照すると、一部の実施形態では、上記の通り、第2表面上への、ZrO2などの誘電体の選択的堆積後に、第1表面の選択的パッシベーションによって、第2表面上への選択的堆積を達成し得る。図示するフローチャートでは、第1表面は金属製(例えば、集積回路の層間誘電体、すなわち、ILDの中の埋め込み金属特徴部)であることができ、第2表面は誘電体(例えば、ILD)であり得る。パッシベーションは、ステップ1で、一部の第2表面に対して、第1表面上に選択的に堆積する、ポリマーまたは他の有機材料を備え得る。続いて、時には、選択性を完全なものにする「クリーンアップ」エッチングと称される、ポリマーのエッチバックを実施して、第1表面からポリマーのすべてを除去することなく、ステップ2で第2表面上に堆積されていてもよいポリマーを除去する。ポリマーがパッシベーション層として働くため、ステップ3で誘電材料が第2表面上に選択的に堆積する。ステップ3では、いかなる数の好適な誘電材料を使用してもよい。一部の実施形態では、ZrO2、および遷移金属酸化物もしくは酸化アルミニウムなどの他の金属酸化物、またはSiO2系材料の上方でのエッチング選択性、もしくはSiO2系材料をエッチングする状況における遅いエッチング速度を有する混合物を含む、他の誘電酸化物より誘電材料を選択してもよい。一部のそのような金属酸化物は、高いk値、特に5より高い、またはさらに10より高いk値を有してもよいにもかかわらず、薄く、メタライゼーション構造で有意な寄生容量を避ける位置に設置され、有利にも、酸化シリコン材料の選択的エッチングに対して、表面のマスキングを可能にする。他の実施形態では、誘電体は、酸化シリコン系材料であり得るが、本明細書に記載する通り、エッチングマスクとして機能を果たすよう、より厚くてもよい。図17のステップ4では、ポリマーパッシベーションを第1表面から除去する。
図22A~22Eは、一部の実施形態で、改良された電気的絶縁を伴うデバイスおよびデバイスを作り出すプロセスを説明する。図22Aは、図21Aに示す平面構造に類似し、埋め込み金属製特徴部2606を伴う、一部組み立てられた集積回路を説明し、埋め込み金属製特徴部2606は、周囲のlow-k材料2608によって画定される第2表面と同一平面にある、第1表面を画定する。金属製特徴部は、第1low-k誘電材料2608内に位置付けられる、Cu2610およびTaNバリア材料2612をさらに備える、第1材料を備える。
Claims (18)
- 一部の第1表面に対する前記一部の第2表面上での選択的堆積の方法であって、前記第1および第2表面は、異なる組成物を有し、前記方法は、
前記第2表面に対して前記第1表面上にポリマーを備えるパッシベーション層を選択的に形成することであって、前記第1および第2表面を第1および第2気相反応物質に交互にかつ順次曝露すること、および前記第2表面を前記パッシベーション層がないままにすること、を含む前記パッシベーション層を選択的に形成することと、
前記パッシベーション層に対して、前記第2表面上に気相反応物質より対象の層を選択的に堆積させることと、を含み、
前記第1表面は、無機誘電材料を備え、前記第2表面は金属製材料を備え、
前記パッシベーション層を選択的に形成することは、前記第2表面上にパッシベーション遮断層を形成することと、続いて、前記パッシベーション遮断層に対して、前記第1表面上に前記パッシベーション層を選択的に蒸着することと、を含む、方法。 - 前記パッシベーション層を選択的に形成することは、前記第1表面上に触媒剤なしで実施される、請求項1に記載の方法。
- 前記第1表面は、金属製材料を備え、前記第2表面は、無機誘電材料を備える、請求項1に記載の方法。
- 前記対象の層を選択的に堆積させることは、前記第2表面上に誘電材料を堆積させることを含む、請求項3に記載の方法。
- 前記対象の層を選択的に堆積させることは、前記第2表面上に金属酸化物を堆積させることを含む、請求項3に記載の方法。
- 前記対象の層を選択的に堆積させることは、前記第1表面上にいくらかポリマーを残したまま、前記第2表面からいかなるポリマーをもエッチングすることを含む、請求項3に記載の方法。
- 前記第2表面上に前記対象の層を選択的に堆積させた後に、前記対象の層を除去せずに、前記第1表面から前記パッシベーション層を選択的に除去することをさらに含む、請求項3に記載の方法。
- 選択的に除去することは、基板をプラズマに曝露することを含む、請求項7に記載の方法。
- 選択的に除去することは、100℃から400℃の間の温度で基板をエッチング液に曝露することを含む、請求項7に記載の方法。
- 前記対象の層を選択的に堆積させることは、金属層を堆積させることを含む、請求項1に記載の方法。
- 前記パッシベーション層に対して、前記金属層上に誘電層を選択的に堆積させることをさらに含む、請求項10に記載の方法。
- 前記第2表面上に前記対象の層を選択的に堆積させた後、前記対象の層を除去せずに、前記第1表面から前記パッシベーション層を選択的に除去することを、さらに含む、請求項11に記載の方法。
- 前記パッシベーション層を選択的に形成することは、選択的原子層堆積を含む、請求項1に記載の方法。
- 前記パッシベーション層を選択的に形成することは、前記第1表面上に前記第2表面よりも多量のパッシベーション層を堆積すること、および前記第1表面上にいくらかポリマーを残したまま、前記第2表面からいかなるポリマーをもエッチングすることを含む、請求項1に記載の方法。
- 前記対象の層は、前記第1表面と重複する、請求項1に記載の方法。
- 前記ポリマーは、ポリイミドを含む、請求項1に記載の方法。
- 前記ポリマーは、ポリアミドを含む、請求項1に記載の方法。
- 前記第2表面上に前記対象の層を選択的に堆積させた後に、前記対象の層を除去せずに、前記第1表面から前記パッシベーション層を選択的に除去することをさらに含み、前記パッシベーション層は前記第1表面に向けて堆積され、前記パッシベーション層が直接堆積された前記第1表面の材料は、前記パッシベーション層を選択的に除去した後に残る、請求項1に記載の方法。
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