JP2013239745A - 銅の相互接続体のための窒化コバルト層及びそれらを形成する方法 - Google Patents
銅の相互接続体のための窒化コバルト層及びそれらを形成する方法 Download PDFInfo
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Abstract
【解決手段】集積回路のための相互接続構造体に、銅線の核形成、成長及び接着を促進する窒化コバルトの層が組み込まれる。銅の拡散バリヤーとして機能し、かつ窒化コバルトと下地の絶縁体の間の接着性も増加させる、窒化タングステン又は窒化タンタルなどの耐熱性の金属窒化物又は金属炭化物層上に窒化コバルトを堆積してよい。窒化コバルトは、新規なコバルトアミジナート前駆体からの化学気相成長により形成され得る。窒化コバルト上に堆積された銅層は、高い電気伝導度を示し、マイクロエレクトロニクスにおける銅伝導体の電気化学的な堆積のための種層として機能できる。
【選択図】図1
Description
ビス(アルキル−イミド)ビス(ジアルキルアミド)タングステン(VI)化合物の蒸気に基板を曝露する1つ以上のサイクルを包含し、それによれば、蒸気の少なくとも一部分が自己制御式プロセスにより基板の表面に吸着し;次に、その表面が追加量のビス(アルキル−イミド)ビス(ジアルキルアミド)タングステン(VI)化合物と反応するべく調製されるように、その表面を活性化するアンモニア蒸気に基板を曝露する。典型的なALDプロセスのさらなる詳細は、参照により全体で本明細書に援用される国際公開第2004/007796号パンフレットに見出される。
WN、Co4N及びCuのCVD
上部にSiO2の絶縁層を有するシリコンウエハーを基板として使用した。トレンチ及びホールをSiO2層の一部の領域でエッチングした。
WN、Co及びCuのCVD
コバルト金属が窒化コバルトの代わりに堆積されること以外は、実施例1を繰り返す。実施例1に従って事前に形成されたWN上にコバルト金属を堆積した。240℃の基板温度での約0.03Torrのビス(N−tert−ブチル−N’−エチル−プロピオンアミジナト)コバルト(II)、0.5Torrの水素及び0.5Torrの窒素の蒸気混合物からの20分間のCVDにより、Coを形成した。約2nm厚のCoの層をWN上に堆積した。Coを堆積した後、銅を実施例1に記載のようにして堆積した。
WN、Co4N+Co3N及びCuのCVD
CoxNの堆積中、0.3Torrのアンモニア、0.2Torrの水素を使ったこと以外は実施例1を繰り返す。この堆積は、約2nm厚のCoxN層を製造するのに十分なほど長い4分間で行なわれた。同一条件下で製造されたより厚い膜上のRBS分析は、窒素に対するコバルトの比xが3〜4であることを決定した。電子回折は、この膜の主要な相は、一部の六方晶形のCo3Nを伴ったCo4Nであることを確認した。
WN、Co3N及びCuのCVD
CoxNの堆積中に0.5Torrのアンモニアを使い、かつ水素を全く使わないこと以外は実施例1を繰り返す。この堆積は、約2nm厚のCoxN層を作るのに十分なほど長い4分間で行なわれた。同一条件下で作られたより厚い膜上のRBS分析は、窒素に対するコバルトの比xが約3であることを決定した。電子回折は、膜の構造が六方晶形のCo3Nであることを確認した。
WN、Co4N及びCuのCVD
銅層が(1,1,1,5,5,5−ヘキサフルオロアセトアセトナト)銅(I)トリメチルビニルシランから堆積されること以外は実施例1を繰り返す。100℃の基板温度での約0.4Torrの(1,1,1,5,5,5−ヘキサフルオロアセトアセトナト)銅(I)トリメチルビニルシラン、1Torrの水素及び2Torrの窒素の蒸気混合物からの30秒間のCVDにより、銅の種層が形成される。約7nm厚の銅層を堆積させる。
次の4つの反応により、ビス(N−tert−ブチル−N’−エチル−プロピオンアミジナト)コバルト(II)の合成が行なわれた。全ての反応及び操作は、不活性雰囲気のボックス又は標準的なシュレンク(Schlenk)法のいずれかを用いて純窒素雰囲気下で行なわれた。テトラヒドロフラン(THF)、塩化メチレン(CH2Cl2)及びペンタンは、イノベーティブ・テクノロジー社の溶媒精製システムを用いて乾燥され、4Å(4×10−10m)モレキュラーシーブの上で保管された。ブチルチリウム、塩化tert‐ブチル、エチルアミン、プロピオニトリル、CoCl2及びFeCl3を受け取ったままの状態で使用した。
収率38g、81%。1H NMR(CDCl3,25℃,ppm):1.0−1.1(2t,6H,CH2CH3)、1.30(s,9H,C(CH3)3)、2.03(q,2Η,CCH2CH3)、3.16(q,4H,NCH2CH3)。
収率、34g、71%。 mp:−17℃. 1H NMR(C6D6,25℃,ppm):−100.7(br,3H)、−30.6(br,9H)、86.7(br,3H)、248.5(br,2H)、268.8(br,2H)。 CoC18H38N4の計算分析値:C,58.52;H,10.37;N,15.16、 実測値:C,58.36;H,10.66;N,14.87。
酸化コバルトのCVD
200℃の基板温度におけるビス(N−tert−ブチル−N’−エチル−プロピオンアミジナト)コバルト(II)、水蒸気及び窒素ガスの蒸気混合物からのCVDで、酸化コバルト(II),CoOの膜を形成した。
酸化銅のCVD及びCu種層の形成
140℃の基板温度における0.4Torrの(N,N’−ジ−sec−ブチル−アセトアミジナト)銅(I)の二量体、4Torrの水蒸気及び4Torrの窒素ガスの蒸気混合物からのCVDで、酸化銅(I),Cu2Oの膜を形成した。還元プロセス中の膜及び基板の温度を約50℃に上げるのに十分なほど強い水素プラズマによる1分間の還元によって、Cu2Oを銅金属に変えることができた。
酸窒化銅のCVD及びCu種層の形成
160℃の基板温度における0.4Torrの(N,N’−ジ−sec−ブチル−アセトアミジナト)銅(I)の二量体の蒸気、3Torrの水蒸気、1Torrのアンモニアガス及び4Torrの窒素ガスの蒸気混合物からのCVDで、酸窒化銅(I)の膜を形成した。RBS分析が、おおよそCu0.7O0.2N0.1の組成を与えた。還元プロセス中の膜及び基板の温度を約50℃に上げるのに十分なほど強い水素プラズマによる1分間の還元によって、酸窒化銅膜を銅金属膜に変えることができた。この銅金属膜は、非常に平坦で約0.5nmのRMS粗さを有した。
鉄のCVD
230℃の基板温度におけるビス(N−tert‐ブチル−N’−エチル−プロピオンアミジナト)鉄(II)、水素及び窒素ガスの蒸気混合物からのCVDで、金属鉄の膜を形成した。
窒化鉄のCVD
180℃の基板温度でのビス(N−tert−ブチル−N’−エチル−プロピオンアミジナト)鉄(II)、アンモニア及び窒素ガスの蒸気混合物からのCVDで、導電性の窒化鉄,Fe3Nの膜を形成した。
酸化鉄のCVD
150℃の基板温度での約0.03Torrのビス(N−tert‐ブチル−N’−エチル−プロピオンアミジナト)鉄(II)、0.5Torrの水蒸気及び1.5Torrの窒素ガスの蒸気混合物からのCVDが、酸化鉄(II),FeOの膜を形成した。
マンガンのCVD
400℃の基板温度での約0.03Torrのビス(N,N’−ジイソプロピルアセトアミジナト)マンガン(II)、1Torrの水素ガス及び1Torrの窒素ガスの蒸気混合物からのCVDで、導電性のマンガン金属の膜を形成した。その抵抗率は390μΩ・cmである。
酸化マンガンのCVD
160℃の基板温度での約0.03Torrのビス(N,N’−ジイソプロピルアセトアミジナト)マンガン(II)、0.5Torrの水蒸気及び1.5Torrの窒素ガスの蒸気混合物からのCVDで、酸化マンガン(II),MnOの膜を形成した。
窒化マンガンのCVD
200℃の基板温度での約0.03Torrのビス(N,N’−ジイソプロピルアセトアミジナト)マンガン(II)、0.5Torrのアンモニア及び1.5Torrの窒素ガスの蒸気混合物からのCVDで、導電性の窒化マンガン(II),Mn3N2の膜を形成した。
酸化バナジウムのCVD
250℃の基板温度でのトリス(N,N’−ジイソプロピルアセトアミジナト)バナジウム(III)、水蒸気及び窒素ガスの蒸気混合物からのCVDで、導電性の酸化バナジウム(III),V2O3の膜を形成した。
酸化イットリウムのCVD
280℃の基板温度でのトリス(N,N’−ジイソプロピルアセトアミジナト)イットリウム(III)、水蒸気及び窒素ガスの蒸気混合物からのCVDで、電気絶縁性の酸化イットリウム(III),Y2O3の膜を形成した。
酸窒化銅の堆積
CuONの堆積が、36mmの内径(ID)を有する管状炉型反応器内で行なわれた。銅(I)N,N’−ジ−sec−ブチルアセトアミジナート([Cu(sBu−Me−amd)]2)が、N2キャリアガスの40sccmのバブリングによって輸送されるCu前駆体として使用される。バブラー温度は、Cu前駆体の融点が77℃であるためにCu前駆体が液相として保たれる130℃であった。全てのガス管線、バブラー及びバルブは、良好な温度均一性を維持するオーブン内に配置された。いずれのキャリアガスもない室温で容器から蒸発させられる酸素源として、H2Oを使用した。測定されたN2流量によってチャンバの圧力増加と比較することにより調整されたニードルバルブによって、水蒸気の流量を制御した。NH3を窒素源(その流量を質量流量コントローラーで制御した)として供給した。反応性ガス(H2O及びNH3)の全流量を40sccmに保ち、H2O:NH3の比を40:0、30:10、20:20、10:30又は0:40の値に設定した。反応管(36mmのID)に入れて十分な混合を行なう直前に、この反応ガスを小さい(5mmのID)管内でCu前駆体の蒸気と混ぜた。8Torrの全チャンバ圧下、140〜220℃の基板温度でこの膜を堆積した。基板を室温〜50℃程度の温度に加熱するH2遠隔プラズマによって、この膜を還元した。トロイダルプラズマ発電機(アストロン(ASTRON(登録商標))i型AX7670,MKS)が、プラズマ点火の際に180sccmのAr、そして200sccmのH2(解離励起において還元剤として機能する)を供給した。還元時間を30〜180秒に変えた。100nmの熱酸化物を有するSiウエハーを基板として使用した。20nm厚にスパッタリングすることによりRuを堆積させて、CVD前に大気に曝露した。
Claims (37)
- 相互接続構造体を規定する、基板表面上に位置する共形窒化コバルト層;及び
前記窒化コバルト層の上に位置する銅含有導電層
を含む、基板上に形成された集積回路の相互接続構造体。 - さらに、窒化コバルト層と基板の間に拡散バリヤーを含む、請求項1に記載の構造体。
- 窒化コバルトが、CoxNの組成(xは約1〜10である)を有する、請求項1に記載の構造体。
- 窒化コバルトが、CoxNの組成(xは約2〜6である)を有する、請求項1に記載の構造体。
- 窒化コバルトが、CoxNの組成(xは約3〜5である)を有する、請求項1に記載の構造体。
- 拡散バリヤーが、窒化タンタル、炭化タンタル、窒化タングステン、炭化タングステン及びこれらの混合物からなる群から選択される、請求項2に記載の構造体。
- 窒化コバルト層が、化学蒸着された層である、請求項1に記載の相互接続構造体。
- 拡散バリアー層が、化学蒸着された層である、請求項2に記載の相互接続構造体。
- 銅含有導電層の少なくとも一部分が、化学蒸着された層である、請求項1に記載の相互接続構造体。
- 銅含有導電層の少なくとも一部分が、電気化学的に堆積された層である、請求項1に記載の相互接続構造体。
- コバルトアミジナートの蒸気を含むガス状混合物からの化学気相成長によって、基板上に共形窒化コバルト層を堆積して、集積回路構造の相互接続構造体を規定する工程;及び
窒化コバルト層の上に、銅を含む導電層を堆積する工程
を含む、基板上に形成された集積回路の相互接続構造体の製造方法。 - コバルトアミジナートが、式[Co(AMD)2]、及び構造式
- コバルトアミジナートが、ビス(N−tert‐ブチル−N’−エチル−プロピオンアミジナト)コバルト(II)である、請求項12に記載の方法。
- さらにガス状混合物が還元剤を含む、請求項11に記載の方法。
- 還元剤が二水素である、請求項14に記載の方法。
- 銅含有導電層の少なくとも一部分が、化学蒸着により堆積される、請求項11に記載の方法。
- 銅含有導電層の少なくとも一部分が、電気化学的な堆積により堆積される、請求項16に記載の方法。
- 銅含有導電層の少なくとも一部分が、銅アミジナートの蒸気を含むガス状混合物から堆積される、請求項11に記載の方法。
- 銅アミジナートが、式[Cu(AMD)]2、及び構造式
- ガス状混合物が酸素含有化合物を含み、酸化銅が第一の堆積工程で堆積される、請求項18に記載の方法。
- ガス状混合物が酸素含有化合物及び窒素含有化合物を含み、酸窒化銅が第一の堆積工程で形成される、請求項18に記載の方法。
- さらに酸窒化銅を還元剤に曝露する工程を含む、請求項21に記載の方法。
- さらに酸化銅を還元剤に曝露する工程を含む、請求項20に記載の方法。
- リチウム、ナトリウム、カリウム、ベリリウム、カルシウム、ストロンチウム、バリウム、スカンジウム、イットリウム、ランタン及び他のランタニド金属、チタン、ジルコニウム、ハフニウム、バナジウム、ニオブ、タンタル、モリブデン、タングステン、マンガン、レニウム、鉄、ルテニウム、コバルト、ロジウム、ニッケル、パラジウム、銀、亜鉛、カドミウム、スズ、鉛、アンチモン並びにビスマスの金属群から選択された1つ以上の金属アミジナートの蒸気を含むガス状混合物に基板を曝露する工程
を含む、化学気相成長により金属含有層を形成する方法。 - ガス状混合物が窒素含有ガスを含む、請求項24に記載の方法。
- 窒素含有ガスがアンモニア又はヒドラジンである、請求項25に記載の方法。
- さらにガス状混合物が還元剤を含む、請求項26に記載の方法。
- 還元剤が二水素ガスである、請求項27に記載の方法。
- 金属アミジナートがコバルトアミジナートであり、金属含有層が窒化コバルトを含む、請求項28に記載の方法。
- ガス状混合物が還元剤を含む、請求項24に記載の方法。
- 還元剤が二水素である、請求項30に記載の方法。
- 金属アミジナートがコバルトアミジナートであり、金属含有層が基本的にコバルト金属からなる、請求項31に記載の方法。
- ガス状混合物が酸素含有ガスを含む、請求項24に記載の方法。
- 酸素含有ガスが、酸素分子(O2)、水蒸気、オゾン、又はペル化合物を含む、請求項33に記載の方法。
- 金属含有層が金属酸化物を含む、請求項34に記載の方法。
- 金属酸化物が酸化コバルトを含む、請求項35に記載の方法。
- ビス(N−tert−ブチル−N’−エチル−プロピオンアミジナト)コバルト(II)を含む組成物。
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US8461684B2 (en) | 2013-06-11 |
CN103151335A (zh) | 2013-06-12 |
KR101797880B1 (ko) | 2017-11-15 |
JP2010524264A (ja) | 2010-07-15 |
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CN101687896A (zh) | 2010-03-31 |
WO2009088522A2 (en) | 2009-07-16 |
JP2014179635A (ja) | 2014-09-25 |
TW200903718A (en) | 2009-01-16 |
EP2142682A2 (en) | 2010-01-13 |
JP5571547B2 (ja) | 2014-08-13 |
JP5890463B2 (ja) | 2016-03-22 |
CN101687896B (zh) | 2013-03-27 |
EP2142682B1 (en) | 2014-12-03 |
WO2009088522A3 (en) | 2009-12-30 |
KR101629965B1 (ko) | 2016-06-13 |
EP2857549A3 (en) | 2015-07-15 |
US7973189B2 (en) | 2011-07-05 |
US20080254232A1 (en) | 2008-10-16 |
EP2142682A4 (en) | 2011-11-09 |
JP6009419B2 (ja) | 2016-10-19 |
CN103151335B (zh) | 2016-09-28 |
KR20160030583A (ko) | 2016-03-18 |
AU2008347088A1 (en) | 2009-07-16 |
EP2857549A2 (en) | 2015-04-08 |
TWI480977B (zh) | 2015-04-11 |
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