JP2005537639A - アルコールを用いて金属酸化物を形成するシステムおよび方法 - Google Patents
アルコールを用いて金属酸化物を形成するシステムおよび方法 Download PDFInfo
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- JP2005537639A JP2005537639A JP2004531531A JP2004531531A JP2005537639A JP 2005537639 A JP2005537639 A JP 2005537639A JP 2004531531 A JP2004531531 A JP 2004531531A JP 2004531531 A JP2004531531 A JP 2004531531A JP 2005537639 A JP2005537639 A JP 2005537639A
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Images
Classifications
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
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Abstract
Description
本発明は、蒸着工程中に1または2以上のアルコールと、1または2以上の金属含有前駆体化合物を用いて基板上に金属酸化物層を形成する方法に関する。このような前駆体化合物および方法は、半導体基板または基板アセンブリ上への金属酸化物層の形成に特に好適である。
キャパシタやゲート等のマイクロ電子デバイスが何年にもわたって絶えず小型化してきたために、集積回路技術において従来より用いられてきた材料がその性能限界に近づいている状況に至っている。一般に、シリコン(すなわち、ドープしたポリシリコン)は好まれる基板であり、二酸化ケイ素(SiO2)はしばしばシリコンとともに誘電材料として用いられてマイクロ電子デバイスを構成してきた。しかし、最新のマイクロデバイスにおいて所望されるように、SiO2層が1nmまで薄くなると(すなわち、厚さがわずか4または5分子)、層を通り抜けて流れるトンネル電流のために、もはや、層が絶縁体として有効に機能することはない。
、望ましくない残留塩素もまた、形成されてしまう可能性がある。さらに、ジルコニウムおよびハフニウムのアルキルは一般的に不安定であり、市販されていない。これらは、また、結果として生じる膜に炭素を残す可能性がある。
本発明は、基板上に金属酸化物層を蒸着する方法を提供する。このような蒸着方法は、1または2以上のアルコールを1または2以上のの金属有機アミン前駆体化合物(例えば、アルキルアミンまたはアルキルイミン−アルキルアミン)および/または金属アルキル前駆体化合物と化合させることによってその層を形成することを含む。重要なことには、本発明の方法は水または強力な酸化剤を用いることが必要ではなく、したがって、所望の金属酸化物層と基板との間に望ましくない酸化物の界面層が生じたり一番上の層よりも下にある他の層を酸化したりするという諸問題を緩和(通常は回避)する。通常、そして好ましくは、この層は誘電体層である。
いて、M1およびM2はそれぞれ互いに独立して金属であり、R1、R2、R3、およびR4はそれぞれ互いに独立して水素または有機基であり、wは0から4であり、zは1から8であり、qは1から5であり、w、z、およびqは、金属の酸化状態に依存する。
応ガス)から基板上に所望の層を堆積させる、蒸着法のことを指す。前駆体化合物と何らかの反応ガスとをほぼ同時に用いることを伴う「単純な」CVD法とは異なり、「パルス」CVDはこのような材料を堆積チャンバ内へと交互にパルス供給するが、原子層堆積すなわちALD(以下でより詳細に説明する)において通常なされる前駆体と反応ガス流との混合の厳密な回避は行わない。
本発明は、式R(OH)r、ただしrは1から3(好ましくは1)、で表される1または2以上のアルコールと、式M1(NR1)w(NR2R3)z(式I)、M2R4 q(式II)、または式IIのルイス塩基付加物で表される1または2以上の金属含有前駆体化合物を用いて、基板(好ましくは半導体基板または基板アセンブリ)上に金属酸化物層を形成する方法を提供する。式IおよびIIにおいて、M1およびM2はそれぞれ互いに独立してあらゆる金属(主族、遷移金属、ランタノイド)であり、R1、R2、およびR3のそれぞれは互いに独立して水素または有機基であり、wは0から4(好ましくは0から2)であり、zは1から8(好ましくは2から6)であり、qは1から5(好ましくは2から3)であり、w、z、およびqは、金属の酸化状態に依存する。
る(すなわち、酸化物は単一の金属酸化物または混合金属酸化物でありうる)。任意で、金属酸化物層は混合金属酸化物である(すなわち、2つ以上の金属を含む)。より好ましくは、金属酸化物層は1の金属のみを含む。
合物(すなわち、アルコールおよび金属含有前駆体化合物)中のそれぞれのRはそれぞれ互いに独立して水素または有機基であり、好ましくは有機基である。本明細書で使用する場合には、「有機基」という用語は、本発明の目的のために、脂肪基、環式基、または脂肪基と環式基との組合せ(例えば、アルカリル基およびアラルキル基)として分類される炭化水素基を意味するよう用いられる。本発明の状況において、本発明の前駆体化合物に好適な有機基は、蒸着技法を用いる金属酸化物層の形成を妨げないものである。本発明の状況において、「脂肪基」という用語は、飽和または不飽和の直鎖状または分岐状の炭化水素基を意味する。この用語は、例えばアルキル基、アルケニル基、およびアルキニル基を包含するよう用いられる。「アルキル基」という用語は、例えばメチル、エチル、n−プロピル、イソプロピル、t−ブチル、アミル、ヘプチル、等を含む、飽和の直鎖状または分岐状の一価の炭化水素基を意味する。「アルケニル基」という用語は、ビニル基等の1または2以上のオレフィン系の不飽和基(すなわち、炭素−炭素二重結合)を有する不飽和の直鎖状または分岐状の一価の炭化水素基を意味する。「アルキニル基」という用語は、1または2以上の炭素−炭素三重結合を有する不飽和の直鎖状または分岐状の一価の炭化水素基を意味する。「環式基」という用語は、脂環式基、芳香族、またはヘテロ環式基として分類される閉環状の炭化水素基を意味する。「脂環式基」という用語は、脂肪基と類似した特性を有する環式炭化水素基を意味する。「芳香族」すなわち(or)「アリール基」という用語は、単環式または多環式の芳香族炭化水素基を意味する。「ヘテロ環式基」という用語は、環の原子のうちの1または2以上が炭素以外の元素(例えば、窒素、酸素、硫黄、等)である、閉環状の炭化水素を意味する。
を含む。
く変わることがないようになっている。
されている。例えば、前駆体化合物を収容している槽の温度および気泡になるかまたはその槽を通過する不活性のキャリアガスの流れによって、堆積チャンバに搬送される前駆体材料の量を精密に制御することができる。
"Growth of SrTiO3 and BaTiO3 Thin Films by Atomic Layer Deposition," Electrochemical and Solid-State Letters, 2(10):504-506 (1999)を参照されたい)。
駆動される。したがって、ALDはCVDよりもはるかに低温で行われることが多い。ALD法の間、基板温度は、化学吸着された前駆体化合物(複数可)とその下にある基板表面との間の完全な結合を維持し前駆体化合物(複数可)の分解を防止するのに十分低い温度に維持される。この温度はまた、前駆体化合物(複数可)の凝縮を回避するのに十分高い。通常基板温度は、約25℃から約400℃(好ましくは約150℃から約300℃)の範囲内に保たれ、これは一般に、CVD法において現在用いられている温度よりも低い。したがって、この温度で第1の化学種すなわち前駆体化合物が化学吸着される。第2の化学種すなわち前駆体化合物の表面反応は、第1の前駆体の化学吸着と実質的に同じ温度で起こり得るが、より好ましくないが実質的に異なる温度でも起こりうる。明らかに、当業者が判断していくらかの小さな温度変化は生じる可能性があるが、それでもこれは、第1の前駆体の化学吸着温度で生じるのと統計学的に同じ反応速度を供給することによって、実質的に同じ温度であり得る。そうではなく、化学吸着と次の反応とは厳密に同じ温度で行われてもよい。
パシタ構成を図1ないし図3を参照して説明する。図1を参照して、半導体ウエハー個片(fragment)10は、本発明の方法によって形成されたキャパシタ構成25を含む。ウエハー個片10は、内部に導電性の拡散領域14を形成した基板12を含む。基板12は例えば単結晶シリコンを含んでもよい。基板12の上に、通常ボロフォスフォシリケート(ホウ素リンケイ酸、borophosphosilicate)ガラス(BPSG)である絶縁層16が、拡散領域14へのコンタクト開口18を内部に設けた状態で設けられる。導電性材料20および酸化物層18を図示のように平坦化した状態で、コンタクト開口18を導電性材料20で充填する。材料20は、例えばタングステンまたは導電性を有するようドープしたポリシリコン等、いかなる好適な導電性材料であってもよい。キャパシタ構成25が層16およびプラグ20の上に設けられ、プラグ20を介してノード14に電気接続される。
きる。個々の実施形態において、キャパシタ電極全体が導電性障壁層材料を含んでもよい。
連続的な方法でパルス状に弁を開くコンピュータ制御下の空圧弁を有する図4に示す構成のチャンバを、作動した。チャンバには、Ti(NMe2)4(マサチューセッツ州ニューベリーポート市のストレム・ケミカル)とイソプロピルアルコール(ニュージャージー州パーシパニー市のジェネラル・ケミカル)とを収容している2つの槽がつながっていた。基板は一番上の層としてドープしたポリシリコンを有するシリコンウエハーであり、堆積に備えて220℃に維持された。
連続的な方法でパルス状に弁を開くコンピュータ制御下の空圧弁を有する図4に示す構成のチャンバを、作動可能な状態にした。チャンバには、Hf(NMe2)4(マサチューセッツ州ニューベリーポート市のストレム・ケミカル)とイソプロピルアルコール(ニュージャージー州パーシパニー市のジェネラル・ケミカル)とを収容している2つの槽がつ
ながっていた。Hf(NMe2)4前駆体を40℃まで加熱する一方、イソプロピルアルコールは周囲温度のままであった。基板は一番上の層としてドープしたポリシリコンを有するシリコンウエハーであり、堆積に備えて215℃に維持された。
Claims (49)
- 半導体基板または基板アセンブリを設けること、
式R(OH)rで表される少なくとも1のアルコールを供給すること、
式M1(NR1)w(NR2R3)z(式I)、M2R4 q(式II)、または式IIのルイス塩基付加物で表される少なくとも1の金属含有前駆体化合物を供給すること、
および蒸着法を用いて、前記両前駆体化合物を、前記半導体基板または基板アセンブリの1または2以上の表面上に接触させることにより、金属酸化物層を形成することを含む、半導体構造の製造方法;
前記式において、
Rは有機基であり、rは1から3であり、
M1およびM2はそれぞれ互いに独立して金属であり、
R1、R2、R3、およびR4はそれぞれ互いに独立して水素または有機基であり、
wは0から4であり、
zは1から8であり、
qは1から5であり、
w、z、およびqは、金属の酸化状態に依存する。 - 前記半導体基板または基板アセンブリはシリコンウエハーである、請求項1に記載の方法。
- 前記金属酸化物層は誘電体層である、請求項1に記載の方法。
- 前記金属酸化物の誘電体層は2以上の異なる金属を含む、請求項3に記載の方法。
- 前記2以上の異なる金属は合金、固溶体、またはナノラミネートの形態である、請求項4に記載の方法。
- 前記式において、M1およびM2はそれぞれ互いに独立して3、4、5、6、7、13、14族、およびランタノイドからなる金属の群から選択される、請求項1に記載の方法。
- 前記式において、M1およびM2はそれぞれ互いに独立してY、La、Pr、Nd、Gd、Ti、Zr、Hf、Nb、Ta、Al、およびSiからなる金属の群から選択される、請求項6に記載の方法。
- 前記金属酸化物層の厚さは約30Åから約80Åである、請求項1に記載の方法。
- 前記式において、それぞれのRは互いに独立して(C1〜C10)有機基である、請求項1に記載の方法。
- 前記式において、R1、R2、R3、およびR4はそれぞれ互いに独立して水素または(C1〜C6)有機基である、請求項1に記載の方法。
- 前記式において、wは0から2であり、zは2から6である、請求項1に記載の方法。
- 前記式において、qは2から3である、請求項1に記載の方法。
- 前記金属酸化物層は1の金属を含む、請求項1に記載の方法。
- 前記金属酸化物層はアナターゼ型TiO2を含む、請求項1に記載の方法。
- 堆積チャンバ内に半導体基板または基板アセンブリを設けること、
式R(OH)rで表される少なくとも1のアルコールを供給すること、
式M1(NR1)w(NR2R3)z(式I)、M2R4 q(式II)、または式IIのルイス塩基付加物で表される少なくとも1の金属含有前駆体化合物を供給すること、
前記両前駆体化合物を気化することにより、気化した両前駆体化合物を形成すること、
および該気化した両前駆体化合物を、前記半導体基板または基板アセンブリに供給することにより、該半導体基板または基板アセンブリの1または2以上の表面上に金属酸化物の誘電体層を形成することを含む、半導体構造の製造方法;
前記式において、
Rは有機基であり、rは1から3であり、
M1およびM2はそれぞれ互いに独立して金属であり、
R1、R2、R3、およびR4はそれぞれ互いに独立して水素または有機基であり、
wは0から4であり、
zは1から8であり、
qは1から5であり、
w、z、およびqは、金属の酸化状態に依存する。 - 前記両前駆体化合物は不活性のキャリアガスの存在下で気化される、請求項15に記載の方法。
- 前記式において、M1およびM2はそれぞれ互いに独立して3、4、5、6、7、13、14族、およびランタノイドからなる金属の群から選択される、請求項15に記載の方法。
- 前記両前駆体化合物の気化および供給は化学蒸着法を用いて達成される、請求項15に記載の方法。
- 前記半導体基板または基板アセンブリの温度は約100℃から約600℃である、請求項18に記載の方法。
- 前記半導体基板または基板アセンブリは、圧力が約0.1トールから約10トールの堆積チャンバ内にある、請求項18に記載の方法。
- 前記両前駆体化合物の気化および供給は、複数の堆積サイクルを含む原子層堆積法を用いて達成される、請求項18に記載の方法。
- 前記金属含有層は、原子層堆積法中のそれぞれの堆積サイクル中に、前記両前駆体化合物を交互に導入することにより形成される、請求項21に記載の方法。
- 前記半導体基板または基板アセンブリの温度は、約25℃から約400℃である、請求項21に記載の方法。
- 前記半導体基板または基板アセンブリは、圧力が約10-4トールから約1トールの堆積チャンバ内にある、請求項21に記載の方法。
- 前記金属酸化物層は1の金属を含む、請求項15に記載の方法。
- 基板を設けること、
式R(OH)rで表される少なくとも1のアルコールを供給すること、
式M1(NR1)w(NR2R3)z(式I)、M2R4 q(式II)、または式IIのルイス塩基付加物で表される少なくとも1の金属含有前駆体化合物を供給すること、
および蒸着法を用いて、前記両前駆体化合物を、前記基板上に接触させることにより、金属酸化物層を形成することを含む、基板上に金属酸化物層を形成する方法;
前記式において、
Rは有機基であり、rは1から3であり、
M1およびM2はそれぞれ互いに独立して金属であり、
R1、R2、R3、およびR4はそれぞれ互いに独立して水素または有機基であり、
wは0から4であり、
zは1から8であり、
qは1から5であり、
w、z、およびqは、金属の酸化状態に依存する。 - 前記基板はシリコンウエハーである、請求項26に記載の方法。
- 前記式において、M1およびM2は、それぞれ互いに独立して3、4、5、6、7、13、14族、およびランタノイドからなる金属の群から選択される、請求項26に記載の方法。
- 前記式において、M1およびM2はそれぞれ互いに独立してY、La、Pr、Nd、Gd、Ti、Zr、Hf、Nb、Ta、Al、およびSiからなる金属の群から選択される、請求項28に記載の方法。
- 前記金属酸化物層の厚さは約30Åから約80Åである、請求項26に記載の方法。
- 前記式において、それぞれのRは互いに独立して(C1〜C10)有機基である、請求項26に記載の方法。
- 前記式において、R1、R2、R3、およびR4はそれぞれ互いに独立して水素または(C1〜C6)有機基である、請求項26に記載の方法。
- 前記式において、wは0から2であり、zは2から6である、請求項26に記載の方法。
- 前記式において、qは2から3である、請求項26に記載の方法。
- 前記金属酸化物は1の金属を含む、請求項26に記載の方法。
- 前記金属酸化物層はアナターゼ型TiO2を含む、請求項26に記載の方法。
- 基板を設けること、
式R(OH)rで表される少なくとも1のアルコールを供給すること、
式M1(NR1)w(NR2R3)z(式I)、M2R4 q(式II)、または式IIのルイス塩基付加物で表される少なくとも1の金属含有前駆体化合物を供給すること、
前記両前駆体化合物を気化することにより、気化した両前駆体化合物を形成すること、
および該気化した両前駆体化合物を、前記基板に供給することにより、該基板上に金属酸化物層を形成することを含む、基板上に金属酸化物層を形成する方法;
前記式において、
Rは有機基であり、rは1から3であり、
M1およびM2はそれぞれ互いに独立して金属であり、
R1、R2、R3、およびR4はそれぞれ互いに独立して水素または有機基であり、
wは0から4であり、
zは1から8であり、
qは1から5であり、
w、z、およびqは、金属の酸化状態に依存する。 - 前記両前駆体化合物の気化および供給は化学蒸着法を用いて達成される、請求項37に記載の方法。
- 前記両前駆体化合物の気化および供給は、複数の堆積サイクルを含む原子層堆積法を用いて達成される、請求項37に記載の方法。
- 前記金属酸化物層は1の金属を含む、請求項37に記載の方法。
- その上側に第1の電極を有する基板を設けること、
式R(OH)rで表される少なくとも1のアルコールを供給すること、
式M1(NR1)w(NR2R3)z(式I)、M2R4 q(式II)、または式IIのルイス塩基付加物で表される少なくとも1の金属含有前駆体化合物を供給すること、
前記両前駆体化合物を気化することにより、気化した両前駆体化合物を形成すること、
該気化した両前駆体化合物を、前記基板に供給することにより、該基板の前記第1の電極上に金属酸化物の誘電体層を形成すること、
および該誘電体層上に第2の電極を形成することを含む、メモリデバイス構造の製造方法;
前記式において、
Rは有機基であり、rは1から3であり、
M1およびM2はそれぞれ互いに独立して金属であり、
R1、R2、R3、およびR4はそれぞれ互いに独立して水素または有機基であり、
wは0から4であり、
zは1から8であり、
qは1から5であり、
w、z、およびqは、金属の酸化状態に依存する。 - 前記両前駆体化合物の気化および供給は化学蒸着法を用いて達成される、請求項41に記載の方法。
- 前記両前駆体化合物の気化および供給は、複数の堆積サイクルを含む原子層堆積法を用いて達成される、請求項41に記載の方法。
- 前記金属酸化物の誘電体層は2以上の異なる金属を含む、請求項41に記載の方法。
- 前記2以上の異なる金属は合金、固溶体、またはナノラミネートの形態である、請求項44に記載の方法。
- 前記金属酸化物の誘電体層は、ZrO2、HfO2、Ta2O3、Al2O3、TiO2、およびランタノイド酸化物のうちの1または2以上を含む、請求項41に記載の方法。
- 内部に基板を配置した蒸着チャンバと、
式R(OH)rで表される1または2以上のアルコールを含む1または2以上の容器と、
式M1(NR1)w(NR2R3)z(式I)、M2R4 q(式II)、または式IIのルイス
塩基付加物で表される1または2以上の前駆体化合物を含む1または2以上の容器を備える蒸着装置;
前記式において、
Rは有機基であり、rは1から3であり、
M1およびM2はそれぞれ互いに独立して金属であり、
R1、R2、R3、およびR4はそれぞれ互いに独立して水素または有機基であり、
wは0から4であり、
zは1から8であり、
qは1から5であり、
w、z、およびqは、金属の酸化状態に依存する。 - 前記基板はシリコンウエハーである、請求項47に記載の装置。
- 前記両前駆体を前記蒸着チャンバへと移動させる不活性のキャリアガスの1または2以上の発生源をさらに備える、請求項47に記載の装置。
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JP2021503547A (ja) * | 2017-11-19 | 2021-02-12 | アプライド マテリアルズ インコーポレイテッドApplied Materials,Incorporated | 金属表面上の金属酸化物のaldのための方法 |
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CN1688742A (zh) | 2005-10-26 |
KR20050057087A (ko) | 2005-06-16 |
US20060172485A1 (en) | 2006-08-03 |
TW200422426A (en) | 2004-11-01 |
US7410918B2 (en) | 2008-08-12 |
AU2003262902A1 (en) | 2004-03-19 |
CN100422383C (zh) | 2008-10-01 |
EP1534875A1 (en) | 2005-06-01 |
US20050136689A9 (en) | 2005-06-23 |
WO2004020690A1 (en) | 2004-03-11 |
TWI320061B (en) | 2010-02-01 |
KR101003214B1 (ko) | 2010-12-21 |
US20040043632A1 (en) | 2004-03-04 |
US7041609B2 (en) | 2006-05-09 |
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