JP2005536063A - Ｈｉｇｈ−ｋ金属酸化物の原子層堆積 - Google Patents
Ｈｉｇｈ−ｋ金属酸化物の原子層堆積 Download PDFInfo
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- JP2005536063A JP2005536063A JP2004529511A JP2004529511A JP2005536063A JP 2005536063 A JP2005536063 A JP 2005536063A JP 2004529511 A JP2004529511 A JP 2004529511A JP 2004529511 A JP2004529511 A JP 2004529511A JP 2005536063 A JP2005536063 A JP 2005536063A
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- 238000000231 atomic layer deposition Methods 0.000 title claims abstract description 36
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 28
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 28
- 229910052751 metal Inorganic materials 0.000 claims abstract description 32
- 239000002184 metal Substances 0.000 claims abstract description 32
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 229910000449 hafnium oxide Inorganic materials 0.000 claims abstract description 11
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims abstract description 11
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 41
- 239000000758 substrate Substances 0.000 claims description 24
- 229910052710 silicon Inorganic materials 0.000 claims description 16
- 239000010703 silicon Substances 0.000 claims description 16
- 239000003990 capacitor Substances 0.000 claims description 9
- 239000010410 layer Substances 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 7
- 239000012212 insulator Substances 0.000 claims description 6
- 239000002356 single layer Substances 0.000 claims description 6
- 229910052735 hafnium Inorganic materials 0.000 claims description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- 125000002524 organometallic group Chemical group 0.000 abstract description 5
- 239000000376 reactant Substances 0.000 abstract description 3
- 150000002739 metals Chemical class 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 28
- 201000011452 Adrenoleukodystrophy Diseases 0.000 description 25
- 208000010796 X-linked adrenoleukodystrophy Diseases 0.000 description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 14
- 238000010926 purge Methods 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(iv) oxide Chemical compound O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 11
- 239000007789 gas Substances 0.000 description 10
- 238000011109 contamination Methods 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 7
- 239000003989 dielectric material Substances 0.000 description 7
- 235000012239 silicon dioxide Nutrition 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 6
- 229910001882 dioxygen Inorganic materials 0.000 description 6
- 239000003446 ligand Substances 0.000 description 6
- 239000007800 oxidant agent Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 229910052914 metal silicate Inorganic materials 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- NPEOKFBCHNGLJD-UHFFFAOYSA-N ethyl(methyl)azanide;hafnium(4+) Chemical compound [Hf+4].CC[N-]C.CC[N-]C.CC[N-]C.CC[N-]C NPEOKFBCHNGLJD-UHFFFAOYSA-N 0.000 description 2
- LIWAQLJGPBVORC-UHFFFAOYSA-N ethylmethylamine Chemical compound CCNC LIWAQLJGPBVORC-UHFFFAOYSA-N 0.000 description 2
- 230000005669 field effect Effects 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 150000004760 silicates Chemical class 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- BSDOQSMQCZQLDV-UHFFFAOYSA-N butan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] BSDOQSMQCZQLDV-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- ZYLGGWPMIDHSEZ-UHFFFAOYSA-N dimethylazanide;hafnium(4+) Chemical compound [Hf+4].C[N-]C.C[N-]C.C[N-]C.C[N-]C ZYLGGWPMIDHSEZ-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 ethylmethyl Chemical group 0.000 description 1
- WZVIPWQGBBCHJP-UHFFFAOYSA-N hafnium(4+);2-methylpropan-2-olate Chemical compound [Hf+4].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-] WZVIPWQGBBCHJP-UHFFFAOYSA-N 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
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- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
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- H01L21/0228—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE, pulsed CVD
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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Abstract
本発明は、酸化ハフニウム、酸化ジルコニウム、及び酸化チタニウムを含む、第４族金属を含有する金属酸化物のｈｉｇｈ−ｋ誘電体層の原子層堆積（「ＡＬＤ」）に関する。より詳細には、本発明は、有機金属前駆体として金属アルキルアミドを、及び共反応物質としてオゾンを使用した第４族二金属酸化膜のＡＬＤ形成に関する。
Description
（関連出願に対するクロスリファレンス）
本出願は、引用によりその全体が本明細書に組み込まれる、「Ａｔｏｍｉｃ Ｌａｙｅｒ Ｄｅｐｏｓｉｔｉｏｎ ｏｆ Ｈｉｇｈ−ｋ Ｍｅｔａｌ Ｏｘｉｄｅｓ ｆｏｒ Ｇａｔｅ ａｎｄ Ｃａｐａｃｉｔｏｒ Ｄｉｅｌｅｃｔｒｉｃｓ」の名称で２００２年８月１８日に出願された米国特許仮出願番号第６０／４０４，３７２号の関連出願であり、これに対する優先権を主張する。
本出願は、引用によりその全体が本明細書に組み込まれる、「Ａｔｏｍｉｃ Ｌａｙｅｒ Ｄｅｐｏｓｉｔｉｏｎ ｏｆ Ｈｉｇｈ−ｋ Ｍｅｔａｌ Ｏｘｉｄｅｓ ｆｏｒ Ｇａｔｅ ａｎｄ Ｃａｐａｃｉｔｏｒ Ｄｉｅｌｅｃｔｒｉｃｓ」の名称で２００２年８月１８日に出願された米国特許仮出願番号第６０／４０４，３７２号の関連出願であり、これに対する優先権を主張する。
本発明は、ゲート及び／又はキャパシタ用途において、酸化ハフニウム（ＨｆＯ2）、酸化ジルコニウム（ＺｒＯ2）、及び酸化チタン（ＴｉＯ2）を含む、第４族の金属（第４族とは、旧ＩＵＰＡＣ方式のＩＶＡ族及びＣＡＳ方式でのＩＶＢ族に相当する新しい周期律表の表記である）を含有する金属酸化物のｈｉｇｈ−ｋ誘電体膜の原子層堆積（「ＡＬＤ」）に関する。より詳細には、本発明は、金属アルキルアミド及びオゾンを用いた第４族金属酸化膜のＡＬＤ形成に関する。
コンピュータの速度及び機能は毎年倍増しており、主に集積回路寸法の微細化によって可能にされている。現在、最新の回路の最小寸法は、シリコン中の被制御電流から制御電極（「ゲート電極」）を隔てるゲート絶縁体の厚みである。従来、ゲート絶縁体は、二酸化ケイ素（ＳｉＯ2）及び／又は窒化ケイ素（ＳｉＮ）で作られてきた。このような絶縁体の厚さは２０Åほどである。しかしながら、従来のゲート誘電体は、厚さが２０Åより薄くなると、リーク及び信頼性の欠陥を受けるようになる。
従って、代替の絶縁膜を見出す取り組みが進められている。今日まで、この取り組みの大部分は、高誘電率（ｈｉｇｈ−ｋ）材料に焦点が当てられてきた。本明細書で使用されるように、誘電率「ｋ」が酸化ケイ素の誘電率（ｋ＝３．９）より高い場合、その材料は「ｈｉｇｈ−ｋ」である。
調査されてきたｈｉｇｈ−ｋ誘電体は、二酸化ハフニウム（ＨｆＯ2）（ｋ〜２０−２５）や二酸化ジルコニウム（ＺｒＯ2）（ｋ〜２０−２５）などの第４族二金属酸化物を含む。一般に、これらの材料は、高い誘電率、良好な熱安定性、及びシリコンに対する広いバンドオフセットを示す。しかしながら、Ｖｔ（スレッショルド電圧）に関連する電荷捕捉の不安定性、及びＭＯＳＦＥＴ性能における電子移動度の低下が懸念される。集積回路デバイスのスケールが６５ｎｍノードに近づくにつれ、二酸化ケイ素に代わる、ｈｉｇｈ−ｋゲート誘電体の改良に対する必要性が急速に高まってきている。実際に、ＣＭＯＳ集積回路でのｈｉｇｈ−ｋゲート誘電体の必要性は、国際半導体技術ロードマップで認知されている。
更に、化学気相蒸着法（ＣＶＤ）のような従来技術の堆積手法は、最新の薄膜の要件に適合させることが益々不可能になっている。ＣＶＤプロセスは、改良されたステップカバレージを有するコンフォーマルな膜を形成するように調製することができるが、ＣＶＤプロセスは、多くの場合高い処理温度を必要とし、高濃度の不純物の混入を生じ、前駆体又は反応物質の使用効率が不十分である。例えば、ｈｉｇｈ−ｋゲート誘電体を製造する際の障害の１つは、ＣＶＤプロセス中で界面に酸化ケイ素層が形成されることである。別の障害は、シリコン基板上にｈｉｇｈ−ｋゲート誘電体の超薄膜を堆積する際に従来技術のＣＶＤプロセスでは限界があることである。
従って、均一な化学量論、厚さ、コンフォーマル・カバレージ、急峻な界面、及び平滑な表面を有し、並びに粒界、クラック、及びピンホールが低減された材料を純粋な形態で堆積させるための改良された方法を開発する取り組みが進められている。ＡＬＤは開発されることになる最新の方法である。ＡＬＤでは前駆体及び共反応物質は、交互にされるパルス及びパージにより成長する膜の表面に別々に導かれ、パルスサイクル当たりに１つの単層成長膜を生成する。層の厚さはパルスサイクルの総数によって制御される。ＡＬＤはＣＶＤに対して幾つかの利点を有する。ＡＬＤは、低温度化に向かう産業界の傾向に一致する、比較的低い温度で行うことができ、コンフォーマルな薄膜層を生成することができる。更に有利なことには、ＡＬＤは、原子スケールで膜厚を制御することができ、「ナノエンジニア」の複合薄膜に使用することができる。従って、ＡＬＤの更なる開発が大いに望まれる。
ジルコニウム−テトラ−ブトキシドを使用する酸化ジルコニウムのＡＬＤの形成が報告されている。米国特許第６，４６５，３７１号（「Ｌｉｍ」）を参照されたい。加えて、ハフニウムテトラ−ジメチル−アミド（「ＴＤＭＡＨｆ」）とハフニウムテトラ−エチルメチル−アミド（「Ｈｆ−ＴＥＭＡ」）を使用する酸化ハフニウムのＡＬＤ形成が報告されている。Ｒ．Ｇｏｒｄｏｎ他、「Ｖａｐｏｒ Ｄｅｐｏｓｉｔｉｏｎ Ｏｆ Ｍｅｔａｌ Ｏｘｉｄｅｓ Ａｎｄ Ｓｉｌｉｃａｔｅｓ ： Ｐｏｓｓｉｂｌｅ Ｇａｔｅ Ｉｎｓｕｌａｔｏｒｓ Ｆｏｒ Ｆｕｔｕｒｅ Ｍｉｃｒｏｅｌｅｃｔｒｏｎｉｃｓ」Ｃｈｅｍ．Ｍａｓｔｅｒ、２００１年、ｐ２４６３〜２４６４、及び、Ｋ．Ｋｕｋｌｉ、「Ａｔｏｍｉｃ Ｌａｙｅｒ Ｄｅｐｏｓｉｔｉｏｎ ｏｆ Ｈａｆｎｉｕｍ Ｄｉｏｘｉｄｅ Ｆｉｌｍｓ Ｆｒｏｍ Ｈａｆｎｉｕｍ Ｔｅｔｒａｋｉｓ （ｅｔｈｙｌｍｅｔｈｙｌａｍｉｄｅ） Ａｎｄ Ｗａｔｅｒ」、Ｃｈｅｍ．Ｖａｐ．Ｄｅｐｏｓｉｔｉｏｎ、２００２年、第８巻 第５号、ｐ１９９〜２０４をそれぞれ参照されたい。しかしながら、これらの引用文献のどれも、酸化剤としてオゾンと組み合わせた有機金属前駆体としての金属アルキルアミドの好適な使用を教示していない。
本発明は、ゲート及び／又はキャパシタ誘電体用途で二酸化ケイ素と置き換えるための、酸化ハフニウム（ＨｆＯ2）、酸化ジルコニウム（ＺｒＯ2）、酸化チタニウム（ＴｉＯ2）を含むｈｉｇｈ−ｋ第４族金属酸化膜を形成するＡＬＤプロセスを提供する。最も好適な金属酸化物は酸化ハフニウムである。二酸化ハフニウムは優れた熱安定生を示すので、界面での二酸化ケイ素の成長がより少なくなる。
本方法は、原子層堆積プロセスを伴い、ここでは、金属アルキルアミドとオゾンの個別のパルスが基板を収容する反応チャンバに導入されて、基板上で金属酸化膜を成長させる。本方法は目標厚さの膜が達成されるまで繰り返される。
より詳細には、本方法は以下のパルスサイクルを必要とする。
第１に、金属アルキルアミドをパルス化して反応チャンバ中に送り、第２に、未反応金属アルキルアミド及び副生成物に関して反応チャンバをパージし、第３に、オゾンガスをパルス化して反応チャンバに送り、最後に第４に、未反応オゾン及び副生成物に関して反応チャンバをパージする。代替として、最初にオゾンをパルス化して送りパージして、続いて金属アルキルアミド前駆体のパルス化とパージが続く。パルスサイクルは目標膜厚を得るのに必要な回数だけ何度も繰り返し行う。
第１に、金属アルキルアミドをパルス化して反応チャンバ中に送り、第２に、未反応金属アルキルアミド及び副生成物に関して反応チャンバをパージし、第３に、オゾンガスをパルス化して反応チャンバに送り、最後に第４に、未反応オゾン及び副生成物に関して反応チャンバをパージする。代替として、最初にオゾンをパルス化して送りパージして、続いて金属アルキルアミド前駆体のパルス化とパージが続く。パルスサイクルは目標膜厚を得るのに必要な回数だけ何度も繰り返し行う。
ＡＬＤプロセスでオゾンを使用することにより、水蒸気などの従来の酸化剤とは対照的に、結果として得られる金属酸化膜中で固定され捕捉される電荷が有意に減少する。更に、ＡＬＤプロセスでオゾンを使用することにより、酸素ガスなどの従来の酸化剤とは対照的に、ＡＬＤプロセスに必要な動作温度が有意に低下する。
ＡＬＤプロセスでの有機金属前駆体としての金属アルキルアミドの使用は、金属アルキルや金属アルコキシドなどの他の前駆体と比較して結果として得られる膜の炭素汚染が有意に減少する。これは特に、アルキルアミドのリガンドがエチルメチルリガンドである金属アルキルアミドの場合にあてはまる。
本発明に従って生成されたｈｉｇｈ−ｋ金属酸化膜は、ゲート及びキャパシタ内の誘電体として有用である。ゲート誘電体として使用されるときには、ｈｉｇｈ−ｋ誘電体膜は、一般的にはシリコンウエーハである基板上で１つ又はそれ以上のｎ又はｐドープされたチャネル間に形成される。次に、誘電体上にｎ又はｐドープされた多結晶シリコン電極などの電極が形成されてゲートが完成する。キャパシタ誘電体として使用されるときには、ｈｉｇｈ−ｋ誘電体膜は２つの導電性プレート間に形成される。
添付図面を参照しながら本発明を詳細に説明する。
本発明は、ゲート及び／又はキャパシタ誘電体用途において二酸化ケイ素に代わるｈｉｇｈ−ｋ第４族金属酸化膜を形成するためのＡＬＤプロセスを提供する。このような金属酸化物は、酸化ハフニウム（ＨｆＯ2）、酸化ジルコニウム（ＺｒＯ2）、及び酸化チタニウム（ＴｉＯ2）を含む。最も好適な金属酸化物は酸化ハフニウムである。
本発明は、ゲート及び／又はキャパシタ誘電体用途において二酸化ケイ素に代わるｈｉｇｈ−ｋ第４族金属酸化膜を形成するためのＡＬＤプロセスを提供する。このような金属酸化物は、酸化ハフニウム（ＨｆＯ2）、酸化ジルコニウム（ＺｒＯ2）、及び酸化チタニウム（ＴｉＯ2）を含む。最も好適な金属酸化物は酸化ハフニウムである。
パルスサイクルを開始する前に、一般にシリコンウエーハである基板は、多くの場合チャンバの一方端に配置されたバルブを介して、反応チャンバ内に載置される。好ましくは、シリコンウエーハは、ネイティブの二酸化ケイ素を除去するためにフッ化水素を使用して洗浄済みである。
基板は、基板を支持して所望の反応温度まで加熱する加熱可能なウエーハホルダ上に位置している。基板が適切に位置付けられると、パルスサイクルを開始することができる。
一般的には、パルスサイクルの第１のパルスの前に、ウエーハは約１００℃から約５００℃まで、好ましくは約２００℃から約４００℃の範囲の温度まで加熱される。この温度はプロセスを通して維持される。
一般に、パルスサイクルの第１のパルスの前に、反応チャンバはまた、約０．１から５Ｔｏｒｒまで、好ましくは０．１から２Ｔｏｒｒまで加圧される。この圧力も同様にプロセスを通して維持される。
パルスサイクルは実質的に図１で示される。パルスサイクルは以下の段階を含む。
第１に、揮発性の液体金属アルキルアミドは、揮発され及びパルス化されて、気体として反応チャンバ内に送られる。金属アルキルアミドは基板の表面上に化学吸収される。一般に金属アルキルアミドは、好適には約０．１から約５秒間の範囲の時間にわたり約０．１から約１１００立方センチメートル毎分（「ｓｃｃｍ」）の範囲の流量で導入される。金属アルキルアミドは、アルゴン、窒素、又はヘリウムガスなどの不活性キャリアガスと組み合わせて導入することができる。代替として、金属アルキルアミドは、純粋な形態で導入することができる。
適切な金属アルキルアミドは次式に合致する化合物を含む。
Ｍ（ＮＲ1Ｒ2）n
式中、「Ｍ」はハフニウム、ジルコニウム、及びチタニウムを含む第４族金属、「Ｒ1」及び「Ｒ2」は、置換された又は置換されない線形の分岐及び環状アルキルから構成される群から別個に選択され、「ｎ」は４である。好ましくは「Ｒ1」及び「Ｒ2」はそれぞれ、リガンドが結果として得られる膜の炭素汚染を低減するので、メチル及びエチルなどのＣ1−Ｃ6アルキルである。更に好ましくは、リガンド「ＮＲ3Ｒ4」はエチルメチルアミドである。エチルメチルアミドのリガンドを備えた金属アルキルアミドを使用すると、金属酸化膜の炭素汚染がより少ない。例えば、Ｈｆ−ＴＥＭＡは、ハフニウムテトラメチルアミド及びハフニウムテトラエチルアミドなどの密接に関連する化合物よりも炭素汚染が少なく、同様にハフニウムテトラ−ｔ−ブトキサイドなどの関連性のない化合物よりも炭素汚染が少ない。
Ｍ（ＮＲ1Ｒ2）n
式中、「Ｍ」はハフニウム、ジルコニウム、及びチタニウムを含む第４族金属、「Ｒ1」及び「Ｒ2」は、置換された又は置換されない線形の分岐及び環状アルキルから構成される群から別個に選択され、「ｎ」は４である。好ましくは「Ｒ1」及び「Ｒ2」はそれぞれ、リガンドが結果として得られる膜の炭素汚染を低減するので、メチル及びエチルなどのＣ1−Ｃ6アルキルである。更に好ましくは、リガンド「ＮＲ3Ｒ4」はエチルメチルアミドである。エチルメチルアミドのリガンドを備えた金属アルキルアミドを使用すると、金属酸化膜の炭素汚染がより少ない。例えば、Ｈｆ−ＴＥＭＡは、ハフニウムテトラメチルアミド及びハフニウムテトラエチルアミドなどの密接に関連する化合物よりも炭素汚染が少なく、同様にハフニウムテトラ−ｔ−ブトキサイドなどの関連性のない化合物よりも炭素汚染が少ない。
第２に、反応チャンバは、例えば不活性パージガス又は真空パージを使用して、未反応有機金属前駆体及び副生成物に関してパージされる。不活性パージガスは、アルゴン、窒素、及びヘリウムガスを含む。パージガスは、ほぼ約０．１から約５秒までの範囲の時間にわたってほぼ約０．１から約１１００ｓｃｃｍの流量で反応チャンバ中にパルス化されて送られる。
第３に、オゾンガスは、ほぼ約０．１から約５秒の範囲の時間にわたってほぼ約０．１から約１１００ｓｃｃｍの流量で反応チャンバ中にパルス化されて送られる。オゾンは、アルゴン、窒素、又はヘリウムガスなどの不活性ガスと共に導入することができる。もしくは、オゾンは純粋な形態で添加してもよい。しかしながら「純粋な」とは、酸素ガスが全く存在しないことを意味するものではない。酸素ガスはオゾンに対する前駆体であり、通常はオゾン中に汚染物質としてある程度までは残存する。オゾンは、有機金属前駆体の単一層でリガンドとして機能し、金属酸化物を形成するために金属群を結合する活性酸素を提供すると考えられている。
酸素ガス及び水蒸気などの従来の酸化剤とは異なり、ＡＬＤプロセスでオゾンを使用することによって、結果として得られる金属シリケートに固定及び捕捉される電荷が減少する。加えて、必要な動作温度が低くなる。従来は、酸素ガス及び水蒸気はＡＬＤプロセスでは好適な酸化剤とされていたのに対し、オゾンは酸化剤として認められてはいたが、比較的不安定性が高いことから好ましいものではなかった。しかしながら、オゾンはＡＬＤによる金属シリケート膜の形成において実際には好適な酸化剤であることが見出された。酸素ガスが４００℃近傍又はこれより高い動作温度を必要とするのに対して、オゾンは３００℃より低い動作温度が可能である。結果として得られる膜において水蒸気がヒドロキシル汚染を引き起こすのに対して、オゾンはこうした汚染のない膜を生成する。
最後に第４に、反応チャンバは、未反応オゾン及び副生成物に関してパージされる。この第２のパージ段階は一般に、第１のパージ段階と同様の形態で行われる。
これでＡＬＤプロセスの１サイクルが完了する。最終的に、基板上への１つの単層の第４族金属酸化膜形成が結果として得られる。その後、パルスサイクルは、所望の膜厚を得るために必要なだけ何回も繰り返される。層ごとのＡＬＤ成長は、大きな基板面積にわたって優れたカバレージをもたらし、優れたステップカバレージをもたらす。
本発明に従って形成される好適な第４族金属酸化膜は、酸化ハフニウム（ＨｆＯ2）、酸化ジルコニウム（ＺｒＯ2）、及び酸化チタニウム（ＴｉＯ2）を含む。最も好適な金属酸化膜は酸化ハフニウムである。酸化ハフニウムは、優れた熱安定性を示すので、界面の二酸化ケイ素成長がより少なくなる。
酸化ハフニウム単一層は、Ｈｆ−ＴＥＭＡをパルス化して送り、続いてパージして、次いでオゾンをパルス化して送り、続いて第２のパージを行うことによって、シリコン基板上に好適に形成される。この場合、より高い圧力、より長い前駆体パルス時間（より低い流量）、より高いウエーハ温度、及びより短いオゾンパージ時間によって、結果としてより高い堆積率が得られる。良好な均一性は、より低いプロセス圧力、及びより低いウエーハ温度から得られる。パージ時間を短くすると望ましくない粒子の形成がより少なくなる。
Ｈｆ−ＴＥＭＡ前駆体を使用した酸化ハフニウムの堆積は、好ましくは、２５０−３００℃の範囲のウエーハ温度、０．５Ｔｏｒｒの処理圧力、７０℃のソースキャニスタ温度で行われる。好ましくは、ウエーハを収容するチャンバは、１２０秒の時間期間を超えて予圧縮及び事前加熱される。次いで、以下のパルスサイクルが実行される。第１に、アルゴンの前駆体を流量２３０ｓｃｃｍで２．５秒間パルス化してチャンバに送り、第２に、アルゴンを流量１０４０ｓｃｃｍで１秒間パルス化してチャンバに送り、第３に、１８０ｇ／ｍ３の濃度のオゾンを３５０ｓｃｃｍの流量で２秒間チャンバにパルス化して送り、最後に第４に、アルゴンを１０５０ｓｃｃｍのパルスレートで３秒間パルス化してチャンバに送る。パルスサイクルは５８回繰り返し行い、結果として約６６Åの膜厚を得る。マイナス１ボルトにおけるリーク電流密度（アンペア／ｃｍ2）は、約１．０８Ｅ−０７（アンペア／ｃｍ2）である。
本発明のＡＬＤプロセスを用いて、ゲート及びキャパシタ構造で使用するｈｉｇｈ−ｋ誘電体を生成することができる。例えば該プロセスを用いて、ドープシリコンウエーハなどの基板上にｈｉｇｈ−ｋ金属酸化膜を形成し、ドープポリシリコンなどの導電層を備えた構造体をキャッピングすることによってゲートを生成することができる。あるいは、本プロセスを用いて、２つの導電プレート間にｈｉｇｈ−ｋ金属酸化膜を形成することによってキャパシタを生成することができる。
図２は、このようなｈｉｇｈ−ｋ誘電体をゲートに使用した例示である。図２には電界効果トランジスタ１００が断面で示されている。トランジスタは、低濃度にｐドープされたシリコン基板１１０を含み、その中にはｎドープシリコン・ソース１３０とｎドープシリコン・ドレン１４０が形成され、これらの間にチャネル領域１２０が残されている。ゲート誘電体１６０は、チャネル領域１２０の上に位置付けられる。ゲート電極１５０は、ゲート誘電体１６０の上に位置付けられるので、これだけが中間のゲート誘電体１６０によってチャネル領域１２０から隔てられる。ソース１３０とドレン１４０間に電圧差が存在するときには、ソース１３０又はドレン１４０の１つの接合が逆バイアスされるので、チャネル領域１２０を通る電流は流れない。しかしながら、ゲート電極１５０に正電圧を印加することによって、電流がチャネル領域１２０を通って流れる。ゲート誘電体１６０は、本発明のＡＬＤプロセスに従って製造されたｈｉｇｈ−ｋ金属シリケートである。
当業者であれば本発明の多くの変形が可能であることは明らかであろう。例えば、オゾンは、幾つかの方法で生成し供給することができる。加えて、ＡＬＤチャンバ、ガス分配装置、バルブ、タイミング、及びこれに類するものなどの詳細は変更される場合が多い。本明細書で必ずしも説明されていない、本発明の精神及び範囲内にある他の変形形態が存在することができる。従って、本発明は添付の請求項によってのみ限定される。
１００ 電界効果トランジスタ
１１０ ｐドープされたシリコン基板
１２０ チャネル領域
１３０ ｎドープシリコン・ソース
１４０ ｎドープシリコン・ドレン
１５０ ゲート電極
１６０ ゲート誘電体
１１０ ｐドープされたシリコン基板
１２０ チャネル領域
１３０ ｎドープシリコン・ソース
１４０ ｎドープシリコン・ドレン
１５０ ゲート電極
１６０ ゲート誘電体
Claims (12)
- 原子層を堆積することによって基板上に金属酸化膜を成長させる方法であって、
（ｉ）第４族金属（Ｈｆ、Ｚｒ、Ｔｉ）である金属のアルキルアミドとオゾンの個別のパルスを基板を収容する反応チャンバ内に導入し、
（ｉｉ）前記基板上で目標厚さの膜が達成されるまで前記段階（ｉ）を繰り返す、
ことを含む方法。 - 前記金属酸化物は酸化ハフニウムである請求項１に記載の方法。
- 前記金属アルキルアミドが化学式Ｍ（ＮＲ1Ｒ2）4を有し、式中、Ｍは第４族金属を表し、Ｒ1はエチルグループであり、Ｒ2はメチルグループである請求項１に記載の方法。
- 前記基板はシリコンである請求項１に記載の方法。
- トランジスタのゲート絶縁体を形成する方法であって、
（ｉ）第４族金属である金属のアルキルアミドとオゾンの個別のパルスを基板を収容する反応チャンバに導入することによる原子層堆積で基板上に金属酸化物の単一層を成長させ、
（ｉｉ）目標厚さの誘電体膜が達成されるまで前記段階（ｉ）を繰り返し、
（ｉｉｉ）前記誘電層の上に導電層を位置付ける、
ことを含む方法。 - 前記金属酸化物は、酸化ハフニウム、酸化ジルコニウム、及び酸化チタニウムである請求項５に記載の方法。
- 前記金属アルキルアミドが化学式Ｍ（ＮＲ1Ｒ2）4を有し、式中、Ｍは第４族金属を表し、Ｒ1はエチルグループであり、Ｒ2はメチルグループである請求項５に記載の方法。
- 前記基板はシリコンである請求項５に記載の方法。
- キャパシタを形成する方法であって、
（ｉ）第４族金属である金属のアルキルアミド前駆体とオゾンの個別のパルスを基板を収容する反応チャンバに導入することによる原子層堆積で金属酸化物の単一層を形成し、
（ｉｉ）目標厚さの膜が達成されるまで前記段階（ｉ）を繰り返し、
（ｉｉｉ）前記膜を２つの電極間に位置付ける、
ことを含む方法。 - 前記金属酸化物は、酸化ハフニウム、ＺｒＯ2、及びＴｉＯ2である請求項９に記載の方法。
- 前記金属アルキルアミドが化学式Ｍ（ＮＲ1Ｒ2）4を有し、式中、Ｍは第４族金属を表し、Ｒ1はエチルグループであり、Ｒ2はメチルグループである請求項９に記載の方法。
- 前記基板は前記２つの電極のうちの１つである請求項９に記載の方法。
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| PCT/US2003/025738 WO2004017377A2 (en) | 2002-08-18 | 2003-08-18 | Atomic layer deposition of high k metal oxides |
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| DE19528746C1 (de) * | 1995-08-04 | 1996-10-31 | Siemens Ag | Verfahren zum Erzeugen einer Siliziumdioxidschicht auf Oberflächenabschnitten einer Struktur |
| FI108375B (fi) * | 1998-09-11 | 2002-01-15 | Asm Microchemistry Oy | Menetelmõ eristõvien oksidiohutkalvojen valmistamiseksi |
| US6203613B1 (en) * | 1999-10-19 | 2001-03-20 | International Business Machines Corporation | Atomic layer deposition with nitrate containing precursors |
| KR100467366B1 (ko) * | 2000-06-30 | 2005-01-24 | 주식회사 하이닉스반도체 | 원자층 증착법을 이용한 지르코늄산화막 형성방법 |
| US6844604B2 (en) * | 2001-02-02 | 2005-01-18 | Samsung Electronics Co., Ltd. | Dielectric layer for semiconductor device and method of manufacturing the same |
| US7005392B2 (en) * | 2001-03-30 | 2006-02-28 | Advanced Technology Materials, Inc. | Source reagent compositions for CVD formation of gate dielectric thin films using amide precursors and method of using same |
| KR20030018134A (ko) * | 2001-08-27 | 2003-03-06 | 한국전자통신연구원 | 조성과 도핑 농도의 제어를 위한 반도체 소자의 절연막형성 방법 |
| US6858547B2 (en) * | 2002-06-14 | 2005-02-22 | Applied Materials, Inc. | System and method for forming a gate dielectric |
| US7067439B2 (en) * | 2002-06-14 | 2006-06-27 | Applied Materials, Inc. | ALD metal oxide deposition process using direct oxidation |
| JP2005533390A (ja) * | 2002-07-18 | 2005-11-04 | アヴィザ テクノロジー インコーポレイテッド | 混合成分を有する薄膜の分子層蒸着 |
| TW200411923A (en) * | 2002-07-19 | 2004-07-01 | Asml Us Inc | In-situ formation of metal insulator metal capacitors |
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- 2003-08-18 US US10/524,814 patent/US20060258078A1/en not_active Abandoned
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| EP1535319A4 (en) | 2008-05-28 |
| CN1849703A (zh) | 2006-10-18 |
| WO2004017377A2 (en) | 2004-02-26 |
| KR20050072087A (ko) | 2005-07-08 |
| US20060258078A1 (en) | 2006-11-16 |
| CN100468648C (zh) | 2009-03-11 |
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