JP2008514812A - 膜形成のための前駆体およびルテニウム含有膜を形成するための方法 - Google Patents
膜形成のための前駆体およびルテニウム含有膜を形成するための方法 Download PDFInfo
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- JP2008514812A JP2008514812A JP2007532987A JP2007532987A JP2008514812A JP 2008514812 A JP2008514812 A JP 2008514812A JP 2007532987 A JP2007532987 A JP 2007532987A JP 2007532987 A JP2007532987 A JP 2007532987A JP 2008514812 A JP2008514812 A JP 2008514812A
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- film
- ruthenium
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- 239000002243 precursor Substances 0.000 title claims abstract description 120
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910052707 ruthenium Inorganic materials 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims description 44
- 230000015572 biosynthetic process Effects 0.000 title claims description 21
- 239000002904 solvent Substances 0.000 claims abstract description 69
- 230000008021 deposition Effects 0.000 claims abstract description 14
- 229910001927 ruthenium tetroxide Inorganic materials 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims description 94
- 239000000758 substrate Substances 0.000 claims description 90
- 239000003638 chemical reducing agent Substances 0.000 claims description 43
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 claims description 35
- 239000011261 inert gas Substances 0.000 claims description 31
- 229910001925 ruthenium oxide Inorganic materials 0.000 claims description 31
- 239000007789 gas Substances 0.000 claims description 29
- 238000000151 deposition Methods 0.000 claims description 24
- HHBBIOLEJRWIGU-UHFFFAOYSA-N 4-ethoxy-1,1,1,2,2,3,3,4,5,6,6,6-dodecafluoro-5-(trifluoromethyl)hexane Chemical compound CCOC(F)(C(F)(C(F)(F)F)C(F)(F)F)C(F)(F)C(F)(F)C(F)(F)F HHBBIOLEJRWIGU-UHFFFAOYSA-N 0.000 claims description 23
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- 239000010703 silicon Substances 0.000 claims description 20
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- 229910016062 BaRuO Inorganic materials 0.000 description 3
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- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
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- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 3
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
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- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(iv) oxide Chemical compound O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- RVZRBWKZFJCCIB-UHFFFAOYSA-N perfluorotributylamine Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)N(C(F)(F)C(F)(F)C(F)(F)C(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F RVZRBWKZFJCCIB-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical class [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
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- YRAJNWYBUCUFBD-UHFFFAOYSA-N 2,2,6,6-tetramethylheptane-3,5-dione Chemical compound CC(C)(C)C(=O)CC(=O)C(C)(C)C YRAJNWYBUCUFBD-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 241000872931 Myoporum sandwicense Species 0.000 description 1
- 229920001774 Perfluoroether Polymers 0.000 description 1
- 101100023111 Schizosaccharomyces pombe (strain 972 / ATCC 24843) mfc1 gene Proteins 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- JFWLFXVBLPDVDZ-UHFFFAOYSA-N [Ru]=O.[Sr] Chemical compound [Ru]=O.[Sr] JFWLFXVBLPDVDZ-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
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- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
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- 229910052788 barium Inorganic materials 0.000 description 1
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- 238000009835 boiling Methods 0.000 description 1
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- 229910052736 halogen Inorganic materials 0.000 description 1
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- 229910000311 lanthanide oxide Inorganic materials 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
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- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
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- 150000003303 ruthenium Chemical class 0.000 description 1
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- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 description 1
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- 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
- C23C16/44—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
- C23C16/455—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 introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45519—Inert gas curtains
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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
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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
- C23C16/06—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 metallic 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
- 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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- 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
- C23C16/44—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
- C23C16/455—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 introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—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
- 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
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—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
- 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
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
- H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
- H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table
- H01L21/28556—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table by chemical means, e.g. CVD, LPCVD, PECVD, laser CVD
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
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Abstract
Description
本発明は、基板上へのルテニウム含有膜形成または膜堆積のための前駆体(これ以降は、ルテニウム含有膜形成前駆体と呼ぶ)、およびルテニウム含有膜を形成するための方法に関する。
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、次世代のDRAMのキャパシタ電極材料として最も期待されると考えられる材料である。アルミナ、五酸化タンタル、酸化ハフニウム、およびチタン酸バリウム−ストロンチウム(BST)のような高誘電率の材料が、現在のところこれらのキャパシタ電極に使われている。しかしながらこれらの材料は600℃ほどの高い温度を用いて製造され、これはポリシリコン、シリコンおよびアルミニウムの酸化をもたらし、キャパシタンスの損失を引き起こす。一方でルテニウムおよび酸化ルテニウムの双方は高い耐酸化性と高い伝導性とを示し、キャパシタ電極材料としての用途に適している。これらはまた、酸素拡散バリアとして有効に機能する。ルテニウムは、また、酸化ランタニドのためのゲート金属についても提案されている。加えて、ルテニウムは、白金および他の貴金属化合物と比べて、オゾンおよび酸素を用いるプラズマによってより容易にエッチングされる。low−k材料を銅めっきから分離するためのバリア層としての、およびシード層としてのルテニウムの使用は近年注目されている。
本発明は、ルテニウム含有膜の製造に非常に有用であり、貯蔵または保持中に爆発の危険性を示さず、かつ安定剤の不存在下でも分解を起こさない膜形成前駆体を提供する。
少なくとも1つの基板を含む反応チャンバ中に上記した少なくとも1種の膜形成のための前駆体を導入することにより、基板上にルテニウム含有膜を堆積する工程であって、ここで上記前駆体をガス状態で導入する工程
を含む。
上記反応チャンバ中にガス状の還元剤を導入し、これによって、上記ガス状の前駆体と上記ガス状の還元剤とを反応させることにより少なくとも1つの基板上にルテニウムを堆積する工程
を含む。
ガス状の前駆体を反応チャンバに導入する工程、
反応チャンバをこの中に不活性ガスを注入することによりパージする工程、
その後、ガス状の還元剤を反応チャンバ中に導入する工程、
反応チャンバをこの中に不活性ガスを注入することによりパージする工程、
その結果、基板上で酸化ルテニウムを還元する工程
を含んでいてもよい。
ガス状の前駆体の導入工程を、所望の膜厚が得られるまで繰り返す工程
を含んでいてもよい。
ガス状の前駆体、ガス状の有機金属化合物、および酸素含有ガスを同時に、または別個のパルスで、基板を保持している反応チャンバ中に導入する工程と、
上記前駆体、有機金属化合物、および上記酸素含有ガスを反応させることにより基板の表面上にルテニウム酸塩膜を堆積する工程
とを含む。
膜形成前駆体は、不燃性溶媒、好ましくは一般式CxHyFzOtNu(式中2x+2y≦y+zであり、2≦x≦15であり、z>yであり、t+u≧1であり、x、y、z、tおよびuは自然数である)を有するフッ素化された溶媒中に溶解した四酸化ルテニウム(RuO4)である。
ルテニウム含有膜は、少なくとも本発明の膜形成前駆体をガス状の形態で、基板を保持している反応チャンバ中に導入することにより、基板上にルテニウム含有膜を堆積することにより形成される。
2−1)ルテニウム膜を形成するための方法
2−2)酸化ルテニウム膜(RuO2膜)を形成するための方法、および
2−3)ルテニウム酸塩膜を形成するための方法。
ルテニウム膜を、ガス状の形態の本発明の膜形成前駆体とガス状の還元剤とを基板を保持している反応チャンバ中に導入すること、および上記前駆体と還元剤を反応させることにより基板上にルテニウムを堆積することにより形成する。
本発明の膜形成前駆体をガス状の形態で、基板を保持する反応チャンバ中に導入する。この膜形成前駆体を、上記したバブラ系によりガス状の形態で反応チャンバ中に導入することができる。この場合において、基板を、前駆体中のRuO4が分解され、固体の酸化ルテニウム(二酸化ルテニウム)が生じる温度にまで加熱する。RuO4の分解により生じる固体の酸化ルテニウムが基板上に堆積する。ガス状の前駆体中のRuO4を伴う上記したフッ素化された溶媒は、酸化ルテニウムのこの堆積中には分解せず、従って、酸化ルテニウム膜中へのその取り込みは回避される。固体の酸化ルテニウム(RuO2)は、ガス状のRuO4の分解触媒として機能する。結果として、一度ガス状のRuO4が加熱により分解し、この分解により生じる固体の酸化ルテニウムが基板上に堆積すると、ガス状のRuO4を、加熱温度が低下した場合においても十分に分解することができる。
ルテニウム酸塩膜を、上記したガス状の形態にある膜形成前駆体およびガス状の有機金属化合物を基板を保持している反応チャンバ中に導入し、含酸素ガスの存在下で前駆体と有機金属化合物とを反応させ、それにより基板の表面上にルテニウム酸塩を堆積することにより形成する。
本発明を例を通じて以下にさらに詳しく説明するが、本発明はこれらの例により限定されない。
反応チャンバにシリコン基板と、またその表面に二酸化ケイ素膜を有するシリコン基板を入れた。コンテナに3−エトキシ−1,1,1,2,3,4,4,5,5,6,6,6−ドデカフルオロ−2−トリフルオロメチルヘキサン(Novec HFE−7500,3M社の商品名)中に0.12重量%の濃度で溶解させた四酸化ルテニウム(RuO4)を含む膜形成前駆体を入れた。窒素に同伴されたRuO4およびHFE−7500を、コンテナ中で窒素をバブリングすることにより反応チャンバ中へと導入した。水素を窒素に対して0.5体積%の濃度で同じ反応チャンバ中に導入した。反応チャンバ中の全圧を10torrに設定し、基板温度を300℃とした。このように続けると、両方の基板上にルテニウム金属膜の堆積を生じた。ルテニウム金属堆積速度は、約9Å/分であった。
ルテニウム金属膜を例1に記載したように、以下のものの上に形成した:アルミナ膜、low−k膜、酸化ハフニウム(HfO2)膜、酸化ランタン(La2O3)膜、窒化タンタル(TaN)膜、酸化タンタル(Ta2O5)膜、窒化チタン(TiN)膜、BST膜、およびPZT膜。ルテニウム金属堆積速度は膜の性質に無関係であり、いずれの場合においても約9Å/分であった。加えて、ルテニウム金属は全ての場合において下地膜にしっかりと接合していた。
反応チャンバにシリコン基板およびその表面に二酸化ケイ素膜を有するシリコン基板を入れた。コンテナに例1におけるように0.12重量%濃度の同じ膜形成前駆体を入れた。窒素をコンテナ中に10sccmの流量でバブリングした。窒素に同伴されるRuO4およびHFE−7500を、RuO4ガス流量が0.07sccmとなるように0.5秒間反応チャンバ中に導入した。酸化ルテニウムの薄膜を各基板上に形成した。未反応のRuO4と随伴するHFE−7500を、窒素を用いて反応チャンバ内部をパージングすることにより除去した後に、水素を1.2sccmの流量で反応チャンバ中に1秒間導入し、窒素を希釈剤として用いた。希釈剤として用いた窒素の総流量は174sccmであった。反応チャンバ内部の圧力を4torrに維持した。基板温度を300℃に設定した。
ルテニウム金属膜を例3において記載したように、以下のものの上に形成した:アルミナ膜、low−k膜、酸化ハフニウム(HfO2)膜、酸化ランタン(La2O3)膜、窒化タンタル(TaN)膜、酸化タンタル(Ta2O5)膜、窒化チタン(TiN)膜、BST膜およびPZT膜。ルテニウム金属堆積速度は膜の性質に無関係であり、いずれの場合においてもサイクルにつき約1.9Å/分であった。さらに、全ての場合においてルテニウム金属は下地膜にしっかりと接合していた。
反応チャンバにシリコン基板およびその表面に二酸化ケイ素膜を有するシリコン基板を入れた。コンテナに例1におけるように0.12重量%濃度の同じ膜形成前駆体を入れた。窒素をコンテナ中に20sccmの流量でバブリングした。窒素に同伴されるRuO4およびHFE−7500を反応チャンバ中に導入した。反応チャンバ中の全圧を10torrに設定し、基板温度は400℃であった。これらの条件下で、約1000Åの厚さを有する非常に均一な酸化ルテニウム膜が60分で各基板上に得られた(堆積速度=約17Å/分)。得られた酸化ルテニウム膜はシリコン基板および他のシリコン基板上の二酸化ケイ素膜の両方にしっかりと接合していた。
Claims (19)
- 一般式CxHyFzOtNu(式中、2x+2y≦y+z、2≦x≦15、z>y、およびt+u≧1であり、x、y、z、tおよびuは自然数である)を有する不燃性のフッ素化された溶媒中に溶解させた四酸化ルテニウムを含む、ルテニウム含有膜形成のための前駆体。
- 前記フッ素化された溶媒が、3−エトキシペルフルオロ(2−メチルヘキサン)およびトリス(ヘプタフルオロプロピル)アミンを含む群から選択される請求項1に記載の前駆体。
- 少なくとも1枚の基板を含む反応チャンバ中に請求項1または2に記載の少なくとも1種の膜形成のための前駆体を導入することにより基板上にルテニウム含有膜を堆積する工程を含み、ここで前記前駆体はガス状の形態で導入されるルテニウム含有膜を形成する方法。
- 前記反応チャンバ中にガス状の還元剤を導入し、これにより前記ガス状の前駆体と前記ガス状の還元剤とを反応させることにより少なくとも1枚の基板上にルテニウムを堆積する工程をさらに含む請求項3に記載の方法。
- 前記還元剤が水素である請求項4に記載の方法。
- 前記反応チャンバ中の圧力を0.01torr〜1000torrに維持する請求項4または5に記載の方法。
- 前記膜堆積工程を50℃〜800℃の基板温度で行う請求項4〜6のうちの一項に記載の方法。
- 前記還元剤および前記ルテニウム前駆体を前記反応チャンバ中に同時に導入する請求項4〜7のうちの一項に記載の方法。
- 前記反応チャンバ中に前記ガス状の前駆体を導入する工程と、
前記反応チャンバをこの中に不活性ガスを注入することによりパージする工程と、
その後、定めた時間の間前記反応チャンバ中に前記ガス状の還元剤を導入する工程(以後、還元剤パルスと呼ぶ)と、
前記反応チャンバの内部をこの中に不活性ガスを注入することによりパージし、よって前記基板上の前記酸化ルテニウムを還元する工程
とを含む請求項4〜7のうちの一項に記載の方法。 - 前記ガス状の前駆体の導入工程を、例えば所望の膜厚が得られるまで繰り返す工程をさらに含む請求項9に記載の方法。
- 前記基板温度を100℃〜600℃に維持する工程を含む請求項9または10に記載の方法。
- 前記ガス状の前駆体を熱的に分解する工程と、
それにより前記基板上に酸化ルテニウム膜を堆積する工程
とを含む請求項3に記載の方法。 - 前記反応チャンバ中の全圧を0.01torr〜1000torrに維持する工程を含む請求項12に記載の方法。
- 前記基板温度を少なくとも150℃以上に維持する工程を含む請求項12または13に記載の方法。
- 前記基板が保持されている前記反応チャンバ中に前記ガス状の前駆体、ガス状の有機金属化合物、および酸素含有ガスを同時に、または別個のパルスで導入する工程と、
前記前駆体、有機金属化合物、および前記酸素含有ガスを反応させることにより前記基板の表面上にルテニウム酸塩膜を堆積する工程
とをさらに含む請求項3に記載の方法。 - 前記基板が半導体製品のためのシリコンベースのウエハである請求項3〜15のうちの一項に記載の方法。
- 前記基板がセラミックベースの材料である請求項3〜15のうちの一項に記載の方法。
- 前記基板は平らな表面でなく、***のような少なくともいくつかの曲面を含む請求項17に記載の方法。
- 前記基板がボール状の基板である請求項3〜15のうちの一項に記載の方法。
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WO2006035281A1 (en) | 2006-04-06 |
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