JP5313171B2 - ルテニウムベースの膜を基板上に形成するための方法 - Google Patents
ルテニウムベースの膜を基板上に形成するための方法 Download PDFInfo
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
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Description
本願は、2007年2月21日に出願された米国仮特許出願第60/890,916号の優先権を主張し、全ての目的のために、その全体が参照によってここに組入れられる。
発明の分野
この発明は一般に、半導体製造の分野に関する。より具体的には、本発明はルテニウム含有膜を基板上に形成する方法に関する。
ルテニウムおよび酸化ルテニウムのようなルテニウム化合物は、次世代DRAMにおけるキャパシタ電極材料としての使用に有望と考えられる。アルミナ、五酸化タンタル、酸化ハフニウム、およびバリウム-ストロンチウムチタナート(BST)のような高誘電率の材料(別名、high-k材料)は、今日、これらのキャパシタ電極のために使用される。しかしながら、これらのhigh-k材料は、ポリシリコン、シリコン、およびアルミニウムの酸化をもたらしてキャパシタンスの損失を生じさせる600℃もの高温を用いて製造される。一方で、ルテニウムおよび酸化ルテニウムの両方は高酸化耐性および高導電性を示し、キャパシタ電極材料としての用途に適切である。それらはまた、酸素拡散バリアとして有効に機能する。ルテニウムは、ランタノイド酸化物のためのゲート金属用にも提案されている。さらに、ルテニウムは白金び他の貴金属化合物よりも、オゾンによって、ならびに酸素を用いたプラズマによって容易にエッチングされる。メッキされた銅からlow-k材料を分離するバリア層として、およびシード層としてのルテニウムの使用も、近年、注目されてきている。
半導体製造プロセスおいて基板上に膜を提供するための新規な方法および配合がここに記載される。開示された方法および配合は、少なくとも2つの不燃性フッ素化溶媒の混合物中に溶解された四酸化ルテニウムの混合物を利用する。
- 各不燃性フッ素化溶媒が一般式CxHyFzOtNuを持つ(ここで、
x ≧ 3、
y + z ≦ 2 x + 2、
z ≧ 1、
t ≧ 0、
u ≧ 0、
t + u ≧ 0であり、
x、y、z、tおよびuは全て整数である)、
- 溶媒の混合物は、メチルノナフルオロブチルエーテルと、エチルノナフルオロブチルエーテルとの混合物である、
- 溶媒混合物は、およそ10体積%ないし90体積%、好ましくはおよそ30体積%のメチルノナフルオロブチルエーテルを含む、
- 溶媒混合物は、およそ10体積%ないし90体積%、好ましくはおよそ70体積%のエチルノナフルオロブチルエーテルを含む、
- 前駆体は、およそ1 ppm未満の水分を含む、
- 前駆体は、およそ1 ppm未満の会合されていない、または遊離の酸素(O2)を含む、
- チャンバー中の圧力は、およそ0.01 torrないしおよそ1000 torrに維持される、
- 膜は、50℃ないし800℃、好ましくはおよそ100℃ないしおよそ600℃の温度に維持された基板上に堆積される、
- ガス状還元剤が反応チャンバーに導入され、ルテニウム含有膜が、還元剤と前駆体の反応によって基板上に堆積される、
- 還元剤は水素、空気または酸素のうちの1つである、
- 還元剤および前駆体が反応チャンバーに同時に導入される、
- 前駆体が液体状で気化器に導入される、
- 前駆体は少なくとも部分的に気化され、蒸気状の前駆体を形成する、
- 液体状の前駆体が、イナートガスによって加圧され、気化器に導入される、
- 液体状の前駆体の少なくとも99%が気化器中で気化される、
- 実質的に全ての液体状の前駆体が気化器中で気化される、
- 液体状の前駆体が、およそ10℃ないしおよそ80℃の温度で気化される、
- 基板は半導体製造に適切なシリコンタイプの基板である、および、
- 基板はセラミックベースの基板である。
一般に、本発明は、半導体製造プロセスにおいて基板上に膜を提供するための方法に関し、反応チャンバーと、該反応チャンバー内に収容された基板とを提供することを含む。ルテニウムベースの前駆体混合物が提供され、該前駆体は、少なくとも2つの不燃性フッ素化溶媒の混合物と、該溶媒混合物中に溶解された四酸化ルテニウムと、およそ100 ppm未満の水分とを含む。ルテニウム含有膜は、その後、基板上に堆積される。
本発明のいくつかの態様において、溶媒混合物は少なくとも2つの溶媒から作られ、各溶媒は一般式CxHyFzOtNuに従って記述され、ここで、
x ≧ 3、
y + z ≦ 2 x + 2、
z ≧ 1、
t ≧ 0、
u ≧ 0、
t + u ≧ 0であり、
x、y、z、tおよびuは全て整数である。
- ルテニウム膜と、
- 酸化ルテニウム膜(RuO2膜)と、
- ルテナート膜と
を含む。
一つの態様によれば、ルテニウム膜は、ガス状のルテニウムベースの前駆体と、ガス状還元剤とを、基板を保持する反応チャンバーに導入し、該前駆体と該還元剤を反応させることによって基板上にルテニウムを堆積させることによって形成される。
いくつかの態様によれば、ルテニウムベースの前駆体は、基板を保持する反応チャンバーにガス状で導入される。このルテニウムベースの前駆体は、バブラー装置によって、または直接気化装置を通してガス状で反応チャンバーに導入され得る。この場合、基板は、前駆体中のRuO4が分解されて固体の酸化ルテニウム(二酸化ルテニウム)が生成する温度まで加熱される。RuO4の分解によって生成した固体の酸化ルテニウムが基板上に堆積する。ガス状前駆体中のRuO4を伴う不燃性フッ素化溶媒混合物は、この酸化ルテニウムの堆積の間に分解せず、それ故、それが酸化ルテニウム膜中に取り込まれることも防止される。固体の酸化ルテニウム(RuO2)は、ガス状RuO4のための分解触媒として機能する。その結果、一旦、熱の適用下でガス状RuO4が分解され、この分解によって生成した固体の酸化ルテニウムが基板上に堆積されると、ガス状RuO4は、加熱温度が下がった時でさえも十分に分解され得る。
いくつかの態様において、ルテナート膜が、先述した特定のガス状のルテニウムベースの前駆体と、ガス状有機金属化合物とを、基板を保持する反応チャンバーへと導入し、該前駆体と該有機金属化合物を、酸素化ガスの存在下で反応させ、それによって基板の表面にルテナートを堆積させることによって生成される。
以下の非限定的な例は、本発明の態様をさらに説明するために設けられている。しかしながら、例は、全て包括的であることを意図したものではなく、ここで記載された本発明の範囲を限定することを意図したものではない。
48%のHFE-7100と52%のHFE-7200との溶媒混合物中に溶解された四酸化ルテニウムから作られたルテニウム前駆体を、完全な直接気化(気化器中に液体が残らないものと定義される)に対応する前駆体液体流量を決定するために、種々の気化器温度で直接気化させた。液体前駆体を加圧し、それを気化器へ流すために、高純度のアルゴンをキャリアーガスとして使用した。気化器の出口でのベースの真空圧力は67 torrであり、ガラスビーズで充填されたガラスのU字管を気化器として使用した。
Claims (19)
- 半導体製造プロセスにおいて基板上に膜を形成するための方法であって、
a) 反応チャンバーと、前記チャンバー内に収容された基板とを提供すること、
b) ルテニウムベースの前駆体を提供すること、ここで前記前駆体は、
1) メチルノナフルオロブチルエーテルおよびエチルノナフルオロブチルエーテルを含む溶媒混合物と、
2) 前記溶媒混合物中に溶解された四酸化ルテニウムと、
3) 100 ppm未満の水分と
を含み、および
c) ルテニウム含有膜を前記基板上に堆積させること
を含む方法。 - 前記溶媒混合物が、
a) 10体積%ないし90体積%のメチルノナフルオロブチルエーテルと、
b) 10体積%ないし90体積%のエチルノナフルオロブチルエーテルと
を含む請求項1の方法。 - 前記溶媒混合物が、
a) 30体積%のメチルノナフルオロブチルエーテルと、
b) 70体積%のエチルノナフルオロブチルエーテルと
を含む請求項2の方法。 - 前記前駆体が、1 ppm未満の水分を含む請求項1の方法。
- 前記前駆体が、1 ppm未満の会合されていない酸素をさらに含む請求項1の方法。
- 前記反応チャンバー中の圧力が0.01 torrないし1000 torrに維持される請求項1の方法。
- 前記膜堆積工程が、50℃ないし800℃の基板温度で実行される請求項1の方法。
- 前記膜堆積工程が、100℃ないし600℃の基板温度で実行される請求項7の方法。
- 前記反応チャンバーにガス状還元剤を導入すること、および前記前駆体を前記ガス状還元剤と反応させることによって、ルテニウム含有膜を前記基板上に少なくとも部分的に堆積させることをさらに含む請求項1の方法。
- 前記還元剤が水素である請求項10の方法。
- 前記還元剤が空気または酸素である請求項10の方法。
- 前記還元剤と前記前駆体とを前記チャンバーに同時に導入することをさらに含む請求項10の方法。
- a) 最初は液体状である前記前駆体を気化器に導入すること、
b) 少なくとも部分的に蒸気状である前駆体を形成するために前記前駆体を気化させること、および
c) 前記蒸気状の前駆体を前記反応チャンバーに導入すること
をさらに含む請求項1の方法。 - 前記液体状の前駆体をイナートガスで加圧することによって、前記液体状の前駆体を前記気化器に導入することをさらに含む請求項14の方法。
- 前記液体状の前駆体の少なくとも99%を気化させることをさらに含む請求項14の方法。
- 前記蒸気状の前駆体を形成するために、全ての液体状の前駆体が気化される請求項14の方法。
- 10℃ないし80℃の温度で前記前駆体を気化させることをさらに含む請求項14の方法。
- 前記基板が、半導体製造のために適切なシリコン基板である請求項1の方法。
- 前記基板がセラミックベースの材料である請求項1の方法。
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Application Number | Priority Date | Filing Date | Title |
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US89091607P | 2007-02-21 | 2007-02-21 | |
US60/890,916 | 2007-02-21 | ||
PCT/IB2008/050637 WO2008102320A2 (en) | 2007-02-21 | 2008-02-21 | Methods for forming a ruthenium-based film on a substrate |
US12/034,776 US7906175B2 (en) | 2007-02-21 | 2008-02-21 | Methods for forming a ruthenium-based film on a substrate |
US12/034,776 | 2008-02-21 |
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JP2010519412A JP2010519412A (ja) | 2010-06-03 |
JP5313171B2 true JP5313171B2 (ja) | 2013-10-09 |
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US (2) | US7906175B2 (ja) |
EP (1) | EP2132357B1 (ja) |
JP (1) | JP5313171B2 (ja) |
KR (1) | KR101483318B1 (ja) |
CN (1) | CN101617065B (ja) |
WO (1) | WO2008102320A2 (ja) |
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US20080214003A1 (en) | 2008-09-04 |
US20110171836A1 (en) | 2011-07-14 |
KR20090115155A (ko) | 2009-11-04 |
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