WO2019097768A1 - ルテニウム化合物、薄膜形成用原料及び薄膜の製造方法 - Google Patents
ルテニウム化合物、薄膜形成用原料及び薄膜の製造方法 Download PDFInfo
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- WO2019097768A1 WO2019097768A1 PCT/JP2018/028271 JP2018028271W WO2019097768A1 WO 2019097768 A1 WO2019097768 A1 WO 2019097768A1 JP 2018028271 W JP2018028271 W JP 2018028271W WO 2019097768 A1 WO2019097768 A1 WO 2019097768A1
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- WIPO (PCT)
- Prior art keywords
- thin film
- compound
- raw material
- ruthenium
- ruthenium compound
- Prior art date
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- 239000010409 thin film Substances 0.000 title claims abstract description 121
- 239000002994 raw material Substances 0.000 title claims abstract description 69
- 150000003304 ruthenium compounds Chemical class 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title abstract description 31
- 150000001875 compounds Chemical class 0.000 claims abstract description 58
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims abstract description 32
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 12
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 67
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 230000015572 biosynthetic process Effects 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 19
- 238000000151 deposition Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 18
- 230000008016 vaporization Effects 0.000 claims description 17
- 229910052707 ruthenium Inorganic materials 0.000 abstract description 27
- 230000008018 melting Effects 0.000 abstract description 14
- 238000002844 melting Methods 0.000 abstract description 14
- 239000002243 precursor Substances 0.000 description 43
- 239000007789 gas Substances 0.000 description 40
- 239000010408 film Substances 0.000 description 39
- 229910052751 metal Inorganic materials 0.000 description 31
- 239000002184 metal Substances 0.000 description 31
- 238000000231 atomic layer deposition Methods 0.000 description 28
- -1 CVD method Chemical class 0.000 description 26
- 238000005229 chemical vapour deposition Methods 0.000 description 20
- 238000005755 formation reaction Methods 0.000 description 20
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 17
- 239000000203 mixture Substances 0.000 description 16
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 15
- 230000008021 deposition Effects 0.000 description 14
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 239000007788 liquid Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 10
- 239000003960 organic solvent Substances 0.000 description 10
- 238000001816 cooling Methods 0.000 description 9
- 229910044991 metal oxide Inorganic materials 0.000 description 9
- 150000004706 metal oxides Chemical class 0.000 description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N methyl pentane Natural products CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 230000001590 oxidative effect Effects 0.000 description 8
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- 229910052786 argon Inorganic materials 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 238000005160 1H NMR spectroscopy Methods 0.000 description 5
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- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 5
- 125000004429 atom Chemical group 0.000 description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 5
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- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 5
- QEGNUYASOUJEHD-UHFFFAOYSA-N 1,1-dimethylcyclohexane Chemical compound CC1(C)CCCCC1 QEGNUYASOUJEHD-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
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- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical class C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 4
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 4
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
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- 238000011156 evaluation Methods 0.000 description 3
- DLEDOFVPSDKWEF-UHFFFAOYSA-N lithium butane Chemical compound [Li+].CCC[CH2-] DLEDOFVPSDKWEF-UHFFFAOYSA-N 0.000 description 3
- 229910052752 metalloid Inorganic materials 0.000 description 3
- 150000002738 metalloids Chemical class 0.000 description 3
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- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 3
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 2
- PAMIQIKDUOTOBW-UHFFFAOYSA-N 1-methylpiperidine Chemical compound CN1CCCCC1 PAMIQIKDUOTOBW-UHFFFAOYSA-N 0.000 description 2
- 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 2
- OISVCGZHLKNMSJ-UHFFFAOYSA-N 2,6-dimethylpyridine Chemical compound CC1=CC=CC(C)=N1 OISVCGZHLKNMSJ-UHFFFAOYSA-N 0.000 description 2
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- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- RYEXTBOQKFUPOE-UHFFFAOYSA-M magnesium;propane;chloride Chemical compound [Mg+2].[Cl-].CC[CH2-] RYEXTBOQKFUPOE-UHFFFAOYSA-M 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 150000002737 metalloid compounds Chemical class 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
- NFWSQSCIDYBUOU-UHFFFAOYSA-N methylcyclopentadiene Chemical compound CC1=CC=CC1 NFWSQSCIDYBUOU-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 1
- DWFKOMDBEKIATP-UHFFFAOYSA-N n'-[2-[2-(dimethylamino)ethyl-methylamino]ethyl]-n,n,n'-trimethylethane-1,2-diamine Chemical compound CN(C)CCN(C)CCN(C)CCN(C)C DWFKOMDBEKIATP-UHFFFAOYSA-N 0.000 description 1
- LSHROXHEILXKHM-UHFFFAOYSA-N n'-[2-[2-[2-(2-aminoethylamino)ethylamino]ethylamino]ethyl]ethane-1,2-diamine Chemical compound NCCNCCNCCNCCNCCN LSHROXHEILXKHM-UHFFFAOYSA-N 0.000 description 1
- GVWISOJSERXQBM-UHFFFAOYSA-N n-methylpropan-1-amine Chemical compound CCCNC GVWISOJSERXQBM-UHFFFAOYSA-N 0.000 description 1
- XHFGWHUWQXTGAT-UHFFFAOYSA-N n-methylpropan-2-amine Chemical compound CNC(C)C XHFGWHUWQXTGAT-UHFFFAOYSA-N 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- VFFHPIPFEAPMHP-UHFFFAOYSA-N n-tert-butyl-n'-ethylethanimidamide Chemical compound CCN=C(C)NC(C)(C)C VFFHPIPFEAPMHP-UHFFFAOYSA-N 0.000 description 1
- UHBQRZPQMZBHGB-UHFFFAOYSA-N n-tert-butyl-n'-ethylpropanimidamide Chemical compound CCN=C(CC)NC(C)(C)C UHBQRZPQMZBHGB-UHFFFAOYSA-N 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- WSGCRAOTEDLMFQ-UHFFFAOYSA-N nonan-5-one Chemical compound CCCCC(=O)CCCC WSGCRAOTEDLMFQ-UHFFFAOYSA-N 0.000 description 1
- 239000012434 nucleophilic reagent Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- BTNXBLUGMAMSSH-UHFFFAOYSA-N octanedinitrile Chemical compound N#CCCCCCCC#N BTNXBLUGMAMSSH-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- OOFGXDQWDNJDIS-UHFFFAOYSA-N oxathiolane Chemical compound C1COSC1 OOFGXDQWDNJDIS-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- GIDBEKINLBHYLA-UHFFFAOYSA-I pentachlororuthenium Chemical compound Cl[Ru](Cl)(Cl)(Cl)Cl GIDBEKINLBHYLA-UHFFFAOYSA-I 0.000 description 1
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 description 1
- GTCCGKPBSJZVRZ-UHFFFAOYSA-N pentane-2,4-diol Chemical compound CC(O)CC(C)O GTCCGKPBSJZVRZ-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- XRVCFZPJAHWYTB-UHFFFAOYSA-N prenderol Chemical compound CCC(CC)(CO)CO XRVCFZPJAHWYTB-UHFFFAOYSA-N 0.000 description 1
- 229950006800 prenderol Drugs 0.000 description 1
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 235000015067 sauces Nutrition 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- BHRZNVHARXXAHW-UHFFFAOYSA-N sec-butylamine Chemical compound CCC(C)N BHRZNVHARXXAHW-UHFFFAOYSA-N 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
- C07F15/0006—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table compounds of the platinum group
- C07F15/0046—Ruthenium compounds
-
- 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
- C23C16/18—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 from metallo-organic compounds
-
- 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]
-
- 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
-
- 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
- H01L21/02—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
-
- 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
- H01L21/02—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
-
- 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
- H01L21/02—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
-
- 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
- H01L21/02—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
- H01L21/28568—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 the conductive layers comprising transition metals
Definitions
- the present invention relates to a novel ruthenium compound having a specific structure, a raw material for forming a thin film containing the compound, and a method for producing a thin film containing a ruthenium using the raw material.
- Materials for forming thin films containing elemental ruthenium show specific electrical properties and are applied to various applications.
- it is used as an electrode material of a memory element represented by a DRAM element, a resistive film, a diamagnetic film used for a recording layer of a hard disk, a catalyst material for a polymer electrolyte fuel cell, and the like.
- Examples of the method for producing the above-mentioned thin film include a sputtering method, an ion plating method, a coating thermal decomposition method, a MOD method such as a sol-gel method, and a chemical vapor deposition method.
- a sputtering method an ion plating method
- a coating thermal decomposition method a coating thermal decomposition method
- a MOD method such as a sol-gel method
- a chemical vapor deposition method there are many advantages such as excellent composition controllability, excellent step coverage, suitable for mass production, and possibility of hybrid accumulation, so chemical chemistry including ALD (Atomic Layer Deposition) method
- ALD Atomic Layer Deposition
- the phase growth (hereinafter sometimes referred to simply as "CVD") method is the optimum manufacturing process.
- Patent Document 1 discloses a ruthenium compound in which a ketoimine group having two carbonyl groups and two specific structures is bonded to ruthenium, but does not describe the ruthenium compound of the present invention.
- the ruthenium compound disclosed in Patent Document 1 is not a compound sufficiently satisfactory as a raw material for chemical vapor deposition because the melting point is 100 ° C. or higher.
- the properties required of the compound (precursor) used as the raw material are that the melting point is low and the liquid can be transported, and the viscosity of the liquid is low , The vapor pressure is large and easy to vaporize, and the thermal stability is high.
- the ALD method it is required to have a temperature region applicable to the ALD method called an ALD window.
- an ALD window a temperature region applicable to the ALD method.
- ruthenium compounds used in the ALD method compounds having an ALD window, high vapor pressure, and low melting point have been sought, but compounds that can be sufficiently satisfactory in these respects with respect to conventional ruthenium compounds There was no.
- an object of the present invention is to provide a ruthenium compound having a high vapor pressure and a melting point lower than that of conventionally known compounds, a thin film forming material containing the compound and a thin film forming ruthenium containing film using the raw material It is to provide a manufacturing method of
- the present invention relates to a ruthenium compound represented by the following general formula (1):
- R 1 to R 3 each independently represent an alkyl group having 1 to 5 carbon atoms. However, when R 1 is a methyl group, R 2 and R 3 are different groups.
- the present invention also provides a thin film-forming raw material containing the ruthenium compound represented by the above general formula (1).
- the present invention vaporizes the raw material for thin film formation according to claim 2 to obtain a vapor containing the ruthenium compound, a step of introducing the vapor into a treatment atmosphere, and decomposing the compound.
- the present invention provides a method for producing a thin film containing ruthenium atoms on the surface of a substrate, which comprises the step of depositing the compound on the substrate by chemical reaction or both.
- a ruthenium compound having a high vapor pressure and a low melting point can be obtained, which is suitable as a thin film forming material for a CVD method, and in particular, because it has an ALD window, ALD It can be preferably used as a raw material for forming a thin film for a process.
- the ruthenium compound of the present invention is a compound represented by the above general formula (1), and is a compound in which carbon monoxide is added to a ruthenium atom.
- the ruthenium compound of the present invention is suitable as a precursor of a thin film manufacturing method having a vaporization process such as a CVD method, and is a precursor applicable to the ALD method, and in particular, as a precursor used in the ALD method. It is suitable.
- R 1 to R 3 each independently represent an alkyl group having 1 to 5 carbon atoms. However, when R 1 is a methyl group, R 2 and R 3 are different groups.
- examples of the alkyl group having 1 to 5 carbon atoms represented by R 1 to R 3 include methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl and sec-yl.
- examples include tributyl, isobutyl, n-pentyl, secondary pentyl, tertiary pentyl, isopentyl and neopentyl.
- R 1, R 2 and R 3 is appropriately selected by the method of manufacturing the thin film to be applied.
- R ⁇ 1 >, R ⁇ 2 > and R ⁇ 3 > turns into a liquid state under normal temperature normal pressure, and vapor pressure becomes large is preferable.
- R 1 is methyl, ethyl or n-propyl are preferable because of their high vapor pressure, and among them, methyl or ethyl is particularly preferable.
- R 3 is preferably tertiary butyl since the melting point is low, R 3 is tertiary butyl, and R 2 is methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl Those in which R 3 is tertiary butyl and R 2 is ethyl are particularly preferable because of their low melting points.
- R 1 is methyl or ethyl
- R 3 is tert-butyl and R 2 is ethyl
- R 1 is methyl
- Particularly preferred is one in which 3 is tert-butyl and R 2 is ethyl since the melting point is particularly low and the viscosity of the liquid state at 25 ° C. is low.
- R 1 , R 2 and R 3 can be arbitrarily selected depending on the solubility in the solvent used, the thin film formation reaction and the like.
- ruthenium compound of the present invention include, for example, the following compound Nos. 1 to No. 217 are mentioned.
- “Me” represents a methyl group
- “Et” represents an ethyl group
- "nPr” represents an n-propyl group
- "iPr” represents an isopropyl group
- “sBu” represents a second Represents a butyl group
- "tBu” represents a tertiary butyl group
- tAm represents a tertiary pentyl group.
- the compound No. 1 since the melting point is low, the compound No. 1 is obtained. 10, 31, 46, 74, 214 are preferable, and compound No. 1 is preferable. 10, 31 and 214 are more preferred. Further, from the viewpoint of vapor pressure, the compound No. 1 10 and No. 31 is preferred.
- the ruthenium compound of the present invention is not particularly limited depending on the method for producing the compound, and an amidine compound having a corresponding structure or a corresponding carbonium ruthenium compound represented by known ruthenium trichloride dichloride tricarbonyl and dodecacarbonium triruthenium. Can be obtained by reacting an alkali metal salt of an amidine compound having the following structure.
- the raw material for thin film formation of the present invention refers to the ruthenium compound of the present invention described above as a precursor of a thin film, and the form differs depending on the manufacturing process to which the raw material for thin film formation is applied.
- the raw material for forming a thin film of the present invention does not contain a metal compound other than the ruthenium compound of the present invention and a semimetal compound.
- the raw material for forming a thin film of the present invention contains a compound containing the desired metal and / or metalloid in addition to the ruthenium compound of the present invention. It can also contain the compound to contain (Hereafter, it may describe as "other precursor.”).
- the thin film forming material of the present invention may further contain an organic solvent and / or a nucleophile, as described later.
- the thin film forming material of the present invention is suitable for the CVD method and the ALD method as described above, the physical properties of the ruthenium compound of the present invention, which is a precursor, are particularly suitable for chemical vapor deposition materials (hereinafter referred to as “CVD materials It is useful as “raw material”.
- the raw material for thin film formation of this invention is a raw material for chemical vapor deposition
- the form is suitably selected by methods, such as a transport supply method of the CVD method to be used.
- the CVD raw material is vaporized into a vapor by heating and / or depressurizing in a container in which the raw material is stored (hereinafter sometimes referred to as “raw material container”), Gas transport to introduce the vapor into the deposition chamber (hereinafter also referred to as “deposition reaction part”) in which the substrate is installed, together with a carrier gas such as argon, nitrogen, or helium, which is used as needed Method, a raw material for CVD is transported in the form of liquid or solution to a vaporization chamber, vaporized by heating and / or depressurizing in the vaporization chamber to form a vapor, and the vapor is introduced into a film forming chamber There is.
- raw material container a container in which the raw material is stored
- a carrier gas such as argon, nitrogen, or helium
- the ruthenium compound itself represented by the above general formula (1) can be used as a CVD raw material.
- the ruthenium compound itself represented by the above general formula (1) or a solution in which the compound is dissolved in an organic solvent can be used as a raw material for CVD.
- These CVD materials may further contain other precursors, nucleophiles and the like.
- a method (hereinafter sometimes referred to as the “single source method”) of vaporizing and supplying the raw material for CVD independently for each component and a multi-component raw material having a desired composition in advance
- a method of vaporizing and supplying the mixed raw material mixed (hereinafter sometimes referred to as "cocktail sauce method”).
- a mixture of the ruthenium compound of the present invention and another precursor or a mixed solution of the mixture in an organic solvent can be used as a raw material for CVD.
- the mixture or mixed solution may further contain a nucleophile or the like.
- organic solvents are not particularly limited, and known organic solvents can be used.
- the organic solvent include acetic acid esters such as ethyl acetate, butyl acetate and methoxyethyl acetate; tetrahydrofuran, tetrahydropyran, ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, dibutyl ether, ethers such as dioxane; methyl Ketones such as butyl ketone, methyl isobutyl ketone, ethyl butyl ketone, dipropyl ketone, diisobutyl ketone, methyl amyl ketone, cyclohexanone and methyl cyclohexanone; hexane, cyclohexane, methylcyclohexane, dimethylcyclohexane, dimethylcyclohexane, ethylcyclohexan
- the total amount of the precursor in the raw material for CVD which is a solution in which the precursor is dissolved in the organic solvent, is 0.01 to 2.0 mol / l, particularly 0.05 to 1.0 mol / l. It is preferable to use a liter.
- the amount of the entire precursor is the amount of the ruthenium compound of the present invention when the raw material for forming a thin film of the present invention does not contain a metal compound other than the ruthenium compound of the present invention and a metalloid compound.
- the forming raw material contains a compound containing another metal in addition to the ruthenium compound and / or a compound containing a metalloid, the total amount of the ruthenium compound of the present invention and the other precursor is used.
- one or more selected from the group consisting of compounds used as organic ligands such as alcohol compounds, glycol compounds, ⁇ -diketone compounds, cyclopentadiene compounds, organic amine compounds and the like Examples thereof include compounds with silicon and metals.
- metal species of the precursor lithium, sodium, potassium, magnesium, calcium, strontium, barium, titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum, tungsten, manganese, iron, ruthenium, cobalt, rhodium , Iridium, nickel, palladium, platinum, copper, silver, gold, zinc, aluminum, gallium, indium, germanium, tin, lead, antimony, bismuth, scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium Gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium or lutetium.
- the alcohol compound used as the organic ligand of the other precursor mentioned above is methanol, ethanol, propanol, isopropyl alcohol, butanol, secondary butyl alcohol, isobutyl alcohol, tertiary butyl alcohol, pentyl alcohol, isopentyl alcohol, tertiary alcohol Alkyl alcohols such as pentyl alcohol; 2-methoxyethanol, 2-ethoxyethanol, 2-butoxyethanol, 2- (2-methoxyethoxy) ethanol, 2-methoxy-1-methylethanol, 2-methoxy-1,1 -Dimethylethanol, 2-ethoxy-1,1-dimethylethanol, 2-isopropoxy-1,1-dimethylethanol, 2-butoxy-1,1-dimethylethanol, 2- (2-methoxyethoxy) -1,1 Ether alcohols such as dimethylethanol, 2-propoxy-1,1-diethylethanol, 2-s-butoxy-1,1-diethylethanol, 3-methoxy-1,1-dimethylpropano
- glycol compounds used as organic ligands for the above other precursors include 1,2-ethanediol, 1,2-propanediol, 1,3-propanediol, 2,4-hexanediol, and 2,2- Dimethyl-1,3-propanediol, 2,2-diethyl-1,3-propanediol, 1,3-butanediol, 2,4-butanediol, 2,2-diethyl-1,3-butanediol, 2 -Ethyl-2-butyl-1,3-propanediol, 2,4-pentanediol, 2-methyl-1,3-propanediol, 2-methyl-2,4-pentanediol, 2,4-hexanediol, 2,4-dimethyl-2,4-pentanediol and the like.
- beta-diketone compound used as an organic ligand of said other precursor acetylacetone, hexane-2,4-dione, 5-methylhexane-2,4-dione, heptane-2,4-dione , 2-methylheptane-3,5-dione, 5-methylheptane-2,4-dione, 6-methylheptane-2,4-dione, 2,2-dimethylheptane-3,5-dione, 2,6 -Dimethylheptane-3,5-dione, 2,2,6-trimethylheptane-3,5-dione, 2,2,6,6-tetramethylheptane-3,5-dione, octane-2,4-dione 2,2,6-trimethyloctane-3,5-dione, 2,6-dimethyloctane-3,5-dione, 2,9-dimethylnonane-4,6-d
- cyclopentadiene compounds used as the organic ligands of the above other precursors cyclopentadiene, methylcyclopentadiene, ethylcyclopentadiene, propylcyclopentadiene, isopropylcyclopentadiene, butylcyclopentadiene, sec-butylcyclopentadiene, Examples include isobutyl cyclopentadiene, tert-butyl cyclopentadiene, dimethyl cyclopentadiene, tetramethyl cyclopentadiene and the like.
- Examples of the organic amine compound used as the organic ligand of the above other precursor include methylamine, ethylamine, propylamine, isopropylamine, butylamine, secondary butylamine, tertiary butylamine, isobutylamine, dimethylamine, diethylamine and dipropyl Examples include amines, diisopropylamine, ethylmethylamine, propylmethylamine, isopropylmethylamine and the like.
- the other precursors mentioned above are known in the art and their methods of preparation are also known.
- the inorganic salt of the metal described above or the hydrate thereof is reacted with an alkali metal alkoxide of the alcohol compound, for example.
- a precursor can be produced.
- metal inorganic salts or hydrates thereof include metal halides, nitrates and the like
- alkali metal alkoxides include sodium alkoxide, lithium alkoxide, potassium alkoxide and the like.
- the other precursor mentioned above is preferably a compound having similar thermal and / or oxidative degradation behavior to the ruthenium compound of the present invention in the case of the single source method, and in the case of the cocktail source method, the heat and / or the oxide.
- the reaction does not occur during mixing due to chemical reaction or the like.
- the raw material for forming a thin film of the present invention may optionally contain a nucleophile in order to impart the stability of the ruthenium compound of the present invention and other precursors.
- a nucleophile ethylene glycol ethers such as glyme, diglyme, triglyme, tetraglyme, 18-crown-6, dicyclohexyl-18-crown-6, 24-crown-8, dicyclohexyl-24-crown-8 Crown ethers such as dibenzo-24-crown-8, ethylenediamine, N, N'-tetramethylethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenehexamine, 1,1,4,7,7- Polyamines such as pentamethyldiethylenetriamine, 1,1,4,7,10,10-hexamethyltriethylenetetramine, triethoxytriethyleneamine, cyclic polyamines such as cyclam and cycle
- the raw material for thin film formation of the present invention is made to contain as much as possible no impurity metal element other than the component which constitutes this, impurity halogen such as impurity chlorine, and impurity organic.
- the impurity metal element content is preferably 100 ppb or less and more preferably 10 ppb or less for each element.
- the total amount is preferably 1 ppm or less, more preferably 100 ppb or less.
- the film is used as a gate insulating film, gate film or barrier layer of LSI, it is necessary to reduce the content of alkali metal elements and alkaline earth metal elements which affect the electric characteristics of the obtained thin film.
- the total amount of the organic impurities is preferably 500 ppm or less, more preferably 50 ppm or less, and most preferably 10 ppm or less.
- the precursor, the organic solvent, and the nucleophile for reducing the respective water content It is better to remove water as much as possible before use.
- the water content of each of the precursor, the organic solvent and the nucleophile is preferably 10 ppm or less, more preferably 1 ppm or less.
- the raw material for thin film formation of the present invention is preferably made to contain particles as little as possible.
- the number of particles larger than 0.3 ⁇ m is preferably 100 or less in 1 mL of liquid phase, and larger than 0.2 ⁇ m
- the number of particles is more preferably 1000 or less in 1 mL of liquid phase, and most preferably the number of particles larger than 0.2 ⁇ m is 100 or less in 1 mL of liquid phase.
- a vapor obtained by vaporizing the raw material for thin film deposition of the present invention and a reactive gas used as needed Is introduced into the film forming chamber (processing atmosphere) in which the precursor is installed, and then the precursor is decomposed on the substrate, chemically reacted, or both to grow and deposit a metal-containing thin film on the substrate surface It is by CVD method.
- CVD method No particular limitation is imposed on the method of transporting and supplying the raw material, the deposition method, the production conditions, the production apparatus, and the like, and known general conditions and methods can be used.
- Examples of the reactive gas to be used according to the above requirements include oxygen, ozone, nitrogen dioxide, nitrogen monoxide, water vapor, hydrogen peroxide, formic acid, acetic acid, acetic anhydride and the like as an oxidizing gas.
- Examples of reducing substances include hydrogen
- examples of producing nitrides include organic amine compounds such as monoalkylamines, dialkylamines, trialkylamines and alkylenediamines, hydrazine, ammonia and the like. One or more of these can be used.
- ozone since the raw material for thin film formation of the present invention has good reactivity with ozone, it is preferable to use ozone when using one kind of reactive gas, and two or more kinds of reactive gases are preferable.
- thermal CVD to react a raw material gas or a raw material gas with a reactive gas by heat alone to deposit a thin film
- plasma CVD using heat and plasma photo CVD using heat and light
- thermal And photoplasma CVD using light and plasma thermal And photoplasma CVD using light and plasma
- ALD in which the deposition reaction of CVD is divided into elementary processes and deposition is performed stepwise at the molecular level.
- Examples of the material of the substrate include: silicon; ceramics such as silicon nitride, titanium nitride, tantalum nitride, titanium oxide, titanium nitride, ruthenium oxide, ruthenium oxide, zirconium oxide, hafnium oxide, and lanthanum oxide; glass; metals such as metallic cobalt Be
- the shape of the substrate may be plate-like, spherical, fibrous or scaly.
- the substrate surface may be flat or may have a three-dimensional structure such as a trench structure.
- the above-mentioned production conditions include a reaction temperature (substrate temperature), a reaction pressure, a deposition rate and the like.
- the reaction temperature is preferably 100 ° C. or higher at which the compound of the present invention sufficiently reacts, more preferably 150 ° C. to 400 ° C., and particularly preferably 200 ° C. to 350 ° C.
- the reaction pressure is preferably 10 Pa to atmospheric pressure in the case of thermal CVD or photo CVD, and preferably 10 Pa to 2000 Pa in the case of using plasma.
- the deposition rate can be controlled by the supply conditions of the raw material (evaporation temperature, evaporation pressure), the reaction temperature, and the reaction pressure.
- a deposition rate of 0.01 nm / min to 100 nm / min is preferable, and a deposition rate of 1 nm / min to 50 nm / min is preferable because a large deposition speed may deteriorate the properties of the obtained thin film, and a small deposition speed may cause productivity problems. Is more preferred.
- the number of cycles is controlled to obtain a desired film thickness.
- the above-mentioned production conditions further include the temperature and pressure at the time of vaporizing the thin film forming material to form a vapor.
- the step of vaporizing the thin film forming material to obtain vapor may be performed in the material container or may be performed in the vaporizing chamber.
- the thin film-forming material of the present invention is preferably evaporated at 0 ° C. to 150 ° C.
- the pressure in the raw material container and the pressure in the vaporization chamber are both 1 Pa to 10000 Pa.
- the thin film production method of the present invention adopts the ALD method, and the raw material for thin film formation is vaporized into vapor by the above-mentioned transport supply method, and the raw material introduction step of introducing the vapor into the film forming chamber, A precursor thin film forming step of forming a precursor thin film on the surface of the substrate by the compound in the vapor; an exhausting step of exhausting an unreacted compound gas; and a chemical reaction of the precursor thin film with a reactive gas, It may have a metal-containing thin film forming step of forming a thin film containing metal on the surface of the substrate.
- the raw material introduction step described above is performed.
- steam are the same as that of what was demonstrated by the manufacturing method of the thin film by CVD method.
- the precursor thin film is formed on the surface of the substrate by bringing the vapor introduced into the film forming chamber into contact with the surface of the substrate (precursor thin film forming step). At this time, the substrate may be heated or the film formation chamber may be heated to apply heat.
- the precursor thin film formed in this step is a thin film formed from the compound of the present invention, or a thin film formed by decomposition and / or reaction of a part of the compound of the present invention, and the target metal oxide It has a composition different from that of the object thin film.
- Room temperature to 500 ° C. is preferable, and 150 ° C. to 350 ° C. is more preferable for the substrate temperature when this step is performed.
- the pressure of the system (in the deposition chamber) when this step is performed is preferably 1 Pa to 10000 Pa, and more preferably 10 Pa to 1000 Pa.
- unreacted compound gas and by-produced gas are exhausted from the film formation chamber (exhaust process).
- Unreacted compound gas and by-produced gas are ideally exhausted completely from the film forming chamber, but they do not necessarily have to be exhausted completely.
- an evacuation method a method of purging the inside of the system with an inert gas such as nitrogen, helium, argon, a method of evacuation by depressurizing the inside of the system, a method combining these, etc. may be mentioned.
- the degree of pressure reduction is preferably 0.01 Pa to 300 Pa, and more preferably 0.01 Pa to 100 Pa.
- an oxidizing gas is introduced into the film forming chamber as a reactive gas, and the action of the oxidizing gas or the action of the oxidizing gas and heat causes metal oxidation from the precursor thin film obtained in the previous precursor thin film forming step.
- a metal thin film (a metal oxide-containing thin film forming step). Room temperature to 500 ° C. is preferable, and 150 to 350 ° C. is more preferable as a temperature when heat is applied in this step.
- the pressure of the system (in the deposition chamber) when this step is performed is preferably 1 Pa to 10000 Pa, and more preferably 10 Pa to 1000 Pa.
- the compounds of the present invention have good reactivity with oxidizing gases, so that high-quality metal oxide thin films with low residual carbon content can be obtained.
- thin film deposition by a series of operations including the above-mentioned raw material introducing step, precursor thin film forming step, exhausting step and metal oxide containing thin film forming step
- One cycle may be repeated several times until a thin film having the required film thickness is obtained.
- unreacted compound gas and reactive gas oxidative gas in the case of forming a metal oxide thin film
- by-product gas It is preferable to carry out the next cycle after evacuating the
- energy such as plasma, light, voltage or the like may be applied, or a catalyst may be used.
- the time of applying the energy and the time of using the catalyst are not particularly limited. For example, at the time of compound gas introduction in the raw material introduction step, heating at the precursor thin film deposition step or metal oxide-containing thin film formation step, exhaust gas in the system at the exhaust step, oxidizing gas in the metal oxide-containing thin film formation step It may be at the time of introduction, or may be between the above steps.
- annealing may be performed in an inert atmosphere, in an oxidizing atmosphere, or in a reducing atmosphere to obtain better electrical characteristics. If embedding is required, a reflow process may be provided.
- the temperature in this case is 200 ° C. to 1000 ° C., preferably 250 ° C. to 500 ° C.
- the apparatus for manufacturing a thin film using the raw material for thin film formation of the present invention can use a known apparatus for chemical vapor deposition.
- the apparatus include an apparatus capable of bubbling a precursor as shown in FIG. 1 and an apparatus having a vaporization chamber as shown in FIG. Further, as shown in FIG. 3 and FIG. 4, an apparatus capable of performing plasma processing on a reactive gas can be mentioned.
- an apparatus capable of simultaneously processing a large number of wafers using a batch furnace can also be used.
- the thin film produced using the raw material for thin film formation of the present invention can be formed of a desired kind of metal, oxide ceramic, nitride ceramic, glass or the like by appropriately selecting other precursors, reactive gases and production conditions. It can be a thin film.
- the thin film is known to exhibit electrical properties, optical properties and the like, and is applied to various applications.
- metal ruthenium thin films, ruthenium oxide thin films, ruthenium alloys, ruthenium-containing composite oxide thin films and the like can be mentioned.
- ruthenium alloys include Pt-Ru alloys.
- the ruthenium-containing composite oxide thin film for example, SrRuO 3.
- Example 1 Compound No. 1 Synthesis of 10 To a reaction flask, 16 g of N '-(tert-butyl) -N-ethylacetimidamide and 225 mL of dehydrated THF were added and mixed well. To the resulting solution was added dropwise 72.6 mL of a hexane solution (1.55 M) of normal butyl lithium under ice cooling, and the mixture was stirred for 1 hour.
- Example 2 Compound No. Synthesis of No. 31
- 10 g of N ′-(tert-butyl) -N-ethylpropionimidamide and 120 mL of dehydrated THF were added and thoroughly mixed.
- To the resulting solution was added dropwise 36.7 ml of a hexane solution (1.55 M) of normal butyl lithium under ice cooling, and the mixture was stirred for 1 hour.
- 7.0 g of ruthenium trichloride tricarbonyl and 273 mL of dehydrated THF were added to a separately prepared reaction flask and thoroughly mixed, and then the above-mentioned reaction solution was added dropwise under ice-cooling.
- the reaction solution was heated to reflux at 80 ° C. for 10 hours after being stirred at room temperature for 2 hours. After stirring, the mixture was returned to room temperature and filtered. The obtained filtrate was subjected to solvent removal at an oil bath of 75 ° C. under reduced pressure. The obtained ruthenium complex was distilled at an oil bath of 145 ° C. and 15 Pa to obtain 0.95 g of a pale yellow viscous liquid.
- Example 3 Compound No. 3 Synthesis of 46 Into a reaction flask, 5.5 g of ruthenium trichloride tricarbonyl and 80 mL of dehydrated THF were added and thoroughly mixed. Under ice-cooling, a THF solution of N, N'-diisopropyl-propionamidinatolithium prepared from 5.7 g of N, N'-diisopropylcarbodiimide and 1.58 g of ethyllithium was added dropwise to the obtained suspension under ice-cooling. After stirring at room temperature for 19 hours, desolvation was carried out under reduced pressure at 75 ° C. in an oil bath. The formed ruthenium complex was placed in a flask, connected to a Kugelrohr purification apparatus, and distilled at a heating temperature of 125 ° C. and 27 Pa to obtain 0.5 g of a yellow viscous solid.
- Example 4 Compound No. 4 Synthesis of 74
- 5.2 g of ruthenium trichloride tricarbonyl and 80 mL of dehydrated THF were added and mixed well.
- To the obtained suspension was added dropwise a THF solution of N, N'-diisopropyl-butylamidinamagnesium chloride prepared from 5.4 g of N, N'-diisopropylcarbodiimide and 4.3 g of propylmagnesium chloride under ice-cooling. .
- desolvation was carried out under reduced pressure at 75 ° C. in an oil bath.
- the formed ruthenium complex was placed in a flask, connected to a Kugelrohr purification apparatus, and distilled at a heating temperature of 145 ° C. and 42 Pa to obtain 0.6 g of a brown viscous liquid (crystallized at room temperature).
- Example 5 Compound No. 5 Synthesis of 214 Into a reaction flask, 4.9 g of ruthenium trichloride tricarbonyl and 80 mL of dehydrated THF were added and thoroughly mixed. Under ice-cooling, a THF solution of N, N′-diisopropyl-pentylamidinalithium prepared from 5.1 g of N, N′-diisopropylcarbodiimide and 2.5 g of normal butyllithium was added dropwise to the obtained suspension under ice-cooling. After stirring at room temperature for 19 hours, desolvation was carried out under reduced pressure at 75 ° C. in an oil bath. The formed ruthenium complex was placed in a flask, connected to a Kugelrohr purification apparatus, and distilled at a heating temperature of 150 ° C. and 55 Pa to obtain 0.5 g of a brown viscous liquid.
- Example 6 Production of metal ruthenium thin film Compound No. 6
- the metal ruthenium thin film was manufactured on the silicon wafer by ALD method of the following conditions using 10 as a raw material for atomic layer deposition method, and the apparatus shown in FIG.
- the thin film obtained was confirmed for its composition by X-ray photoelectron spectroscopy, the obtained thin film was metal ruthenium, and the residual carbon content was less than 1.0 atom%.
- the film thickness was measured by the X-ray reflectance method, and the average value was calculated. The average film thickness was 26.4 nm, and the average film thickness obtained per cycle was 0.05 nm.
- Substrate Silicon wafer reaction temperature (silicon wafer temperature): 350 ° C.
- Reactive Gas Oxygen
- Example 7 Preparation of metal ruthenium thin film Compound No. 7 was used as a raw material for atomic layer deposition. A ruthenium metal thin film was produced under the same conditions as in Example 6 except that 31 was used. When the thin film obtained was confirmed for its composition by X-ray photoelectron spectroscopy, the obtained thin film was metal ruthenium, and the residual carbon content was less than 1.0 atom%. The film thickness was measured by the X-ray reflectance method, and the average value was calculated. The average film thickness was 25.7 nm, and the average film thickness obtained per cycle was 0.05 nm.
- Example 8 Preparation of Ruthenium Metal Thin Film Compound No. 1 was used as a raw material for atomic layer deposition.
- a ruthenium metal thin film was manufactured under the same conditions as in Example 6 except that 46 was used.
- the thin film obtained was confirmed for its composition by X-ray photoelectron spectroscopy, the obtained thin film was metal ruthenium, and the residual carbon content was less than 1.0 atom%.
- the film thickness was measured by the X-ray reflectance method, and the average value was calculated. The average film thickness was 26.3 nm, and the average film thickness obtained per cycle was 0.05 nm.
- Example 9 Production of metal ruthenium thin film Compound No.
- the metal ruthenium thin film was manufactured on the silicon wafer by ALD method of the following conditions using 10 as a raw material for atomic layer deposition method, and the apparatus shown in FIG.
- the thin film obtained was confirmed for its composition by X-ray photoelectron spectroscopy, the obtained thin film was metal ruthenium, and the residual carbon content was less than 1.0 atom%.
- the film thickness was measured by the X-ray reflectance method, and the average value was calculated. The average film thickness was 15 nm, and the average film thickness obtained per cycle was 0.03 nm.
- Substrate silicon wafer reaction temperature (silicon wafer temperature); 350 ° C.
- Reactive Gas Hydrogen
- pressure in the raw material container The raw material for atomic layer deposition method vaporized under the condition of 100 Pa is introduced into a film forming chamber, and deposition is performed for 30 seconds under system pressure: 100 Pa.
- (2) Remove the undeposited material by argon purge for 15 seconds.
- Reactive gas is introduced into the film forming chamber and reacted at a system pressure of 100 Pa for 60 seconds. (4) Remove the unreacted first reactive gas and by-product gas by argon purge for 15 seconds.
- Comparative Example 3 Production of Metallic Ruthenium Thin Film
- a metallic ruthenium thin film was produced under the same conditions as in Example 6 except that the comparative compound 2 was used as a raw material for atomic layer deposition method.
- the thin film obtained was confirmed for its film composition by X-ray photoelectron spectroscopy, the obtained thin film was metal ruthenium, and the residual carbon content was 6.0 atom%.
- the film thickness was measured by the X-ray reflectance method, and the average value was calculated. The average film thickness was 10 nm, and the average film thickness obtained per cycle was 0.02 nm.
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Abstract
Description
即ち、本発明は、下記一般式(1)で表されるルテニウム化合物に関する:
なお、下記化学式中の「Me」はメチル基を表し、「Et」はエチル基を表し、「nPr」はn-プロピル基を表し、「iPr」はイソプロピル基を表し、「sBu」は第二ブチル基を表し、「tBu」は第三ブチル基を表し、「tAm」は第三ペンチル基を表す。
また、堆積速度は、原料の供給条件(気化温度、気化圧力)、反応温度、反応圧力によりコントロールすることができる。堆積速度は、大きいと得られる薄膜の特性が悪化する場合があり、小さいと生産性に問題を生じる場合があるので、0.01nm/分~100nm/分が好ましく、1nm/分~50nm/分がより好ましい。また、ALD法の場合は、所望の膜厚が得られるようにサイクルの回数でコントロールされる。
[実施例1]化合物No.10の合成
反応フラスコに、N‘-(tert-ブチル)-N-エチルアセトイミドアミド16gと脱水THF225mLを加え、十分に混合した。得られた溶液に、氷冷下、ノルマルブチルリチウムのヘキサン溶液(1.55M)を72.6mL滴下し、1時間攪拌した。別途用意した反応フラスコに、二塩化ルテニウムトリカルボニル13.1gと脱水THF511mLを加え十分に混合したのち、氷冷下にて前述した反応溶液を滴下した。反応溶液は15時間の室温攪拌ののち、80℃にて4時間加熱還流を実施した。攪拌後、室温に戻し濾過をした。得られた濾液は減圧下、オイルバス75℃にて脱溶媒を実施した。得られたルテニウム錯体をオイルバス135℃、13Paにて蒸留して淡黄色粘状液体を6.41g得た。
(1)常圧TG-DTA
質量50%減少温度:216℃(760Torr、Ar流量:100ml/分、昇温10℃/分)
(2)減圧TG-DTA
質量50%減少温度:138℃(10Torr、Ar流量:50ml/分、昇温10℃/分)
(3)1H-NMR(重ベンゼン)
1.01-1.08ppm(6H,multiplet)、1.18-1.26ppm(18H,multiplet)、1.48-1.53ppm(6H,multiplet)、2.86-3.10ppm(4H,multiplet)
(4)元素分析(理論値)
C:49.4%(49.18%)、H:7.8%(7.80%)、N:12.7%(12.75%)
反応フラスコに、N‘-(tert-ブチル)-N-エチルプロピオンイミドアミド10.35gと脱水THF120mLを加え、十分に混合した。得られた溶液に、氷冷下、ノルマルブチルリチウムのヘキサン溶液(1.55M)を36.7ml滴下し、1時間攪拌した。別途用意した反応フラスコに二塩化ルテニウムトリカルボニル7.0gと脱水THF273mLを加え十分に混合したのち、氷冷下にて前述した反応溶液を滴下した。反応溶液は2時間の室温攪拌ののち、80℃にて10時間加熱還流を実施した。攪拌後、室温に戻し濾過をした。得られた濾液を減圧下、オイルバス75℃にて脱溶媒を実施した。得られたルテニウム錯体をオイルバス145℃、15Paにて蒸留して淡黄色粘状液体を0.95g得た。
(1)常圧TG-DTA
質量50%減少温度:224℃(760Torr、Ar流量:100ml/分、昇温10℃/分)
(2)減圧TG-DTA
質量50%減少温度:151℃(10Torr、Ar流量:50ml/分、昇温10℃/分)
(3)1H-NMR(重ベンゼン)
0.86-0.97ppm(6H,multiplet)、1.06-1.09ppm(6H,multiplet)、1.21-1.30ppm(18H,multiplet)、1.89-1.98ppm(4H,multiplet)、2.83-3.11ppm(4H,multiplet)
(4)元素分析(理論値)
C:51.3%(51.37%)、H:8.0%(8.19%)、N:12.0%(11.98%)
反応フラスコに、二塩化ルテニウムトリカルボニル5.5gと脱水THF80mLを加え、十分に混合した。得られた懸濁液に氷冷下、N,N’-ジイソプロピルカルボジイミド5.7gとエチルリチウム1.58gより調製したN,N‘-ジイソプロピル-プロピオンアミジナトリチウムのTHF溶液を滴下した。室温にて19時間撹拌後、減圧下オイルバス75℃にて脱溶媒を実施した。生成したルテニウム錯体をフラスコに入れ、クーゲルロール精製装置に接続し、加熱温度125℃、27Paにて蒸留を行い、黄色粘性固体0.5gを得た。
(1)常圧TG-DTA
質量50%減少温度:222℃(760Torr、Ar流量:100ml/分、昇温10℃/分)
(2)減圧TG-DTA
質量50%減少温度:153℃(10Torr、Ar流量:50ml/分、昇温10℃/分)
(3)1H-NMR(重ベンゼン)
0.82-0.86ppm(3H、triplet)、1.00-1.01(3H、doublet)、1.15-1.16ppm(6H,doublet)、1.22-1.24(3H、doublet)、1.75-1.90ppm(2H,multiplet)、3.29-3.38ppm(1H,septet)、3.59-3.69ppm(1H,septet)
(4)元素分析(理論値)
C:51.5%(51.37%)、H:8.2%(8.19%)、N:11.8%(11.98%)
反応フラスコに、二塩化ルテニウムトリカルボニル5.2gと脱水THF80mLを加え、十分に混合した。得られた懸濁液に氷冷下、N,N’-ジイソプロピルカルボジイミド5.4gとプロピルマグネシウムクロリド4.3gより調製したN,N‘-ジイソプロピル-ブチルアミジナトマグネシウムクロリドのTHF溶液を滴下した。室温にて19時間撹拌後、減圧下オイルバス75℃にて脱溶媒を実施した。生成したルテニウム錯体をフラスコに入れ、クーゲルロール精製装置に接続し、加熱温度145℃、42Paにて蒸留を行い、褐色粘性液体(室温にて結晶化)0.6gを得た。
(1)常圧TG-DTA
質量50%減少温度:222℃(760Torr、Ar流量:100ml/分、昇温10℃/分)
(2)減圧TG-DTA
質量50%減少温度:157℃(10Torr、Ar流量:50ml/分、昇温10℃/分)
(3)1H-NMR(重ベンゼン)
0.75-0.79ppm(3H、triplet)、1.02-1.04(3H、doublet)、1.17-1.19ppm(6H,doublet-doublet)、1.24-1.26(3H、doublet)、1.31-1.41ppm(2H,sextet)、1.79-1.93ppm(2H,multiplet)、3.34-3.43ppm(1H,septet)、3.64-3.73ppm(1H,septet)
(4)元素分析(理論値)
C:53.4(53.31%)、H:8.5%(8.54%)、N:11.2(11.30%)
反応フラスコに、二塩化ルテニウムトリカルボニル4.9gと脱水THF80mLを加え、十分に混合した。得られた懸濁液に氷冷下、N,N’-ジイソプロピルカルボジイミド5.1gとノルマルブチルリチウム2.5gより調製したN,N‘-ジイソプロピル-ペンチルアミジナトリチウムのTHF溶液を滴下した。室温にて19時間撹拌後、減圧下オイルバス75℃にて脱溶媒を実施した。生成したルテニウム錯体をフラスコに入れ、クーゲルロール精製装置に接続し、加熱温度150℃、55Paにて蒸留を行い、褐色粘性液体0.5gを得た。
(1)常圧TG-DTA
質量50%減少温度:230℃(760Torr、Ar流量:100ml/分、昇温10℃/分)
(2)減圧TG-DTA
質量50%減少温度:162℃(10Torr、Ar流量:50ml/分、昇温10℃/分)
(3)1H-NMR(重ベンゼン)
0.79-0.83ppm(3H、triplet)、1.04-1.06(3H、doublet)、1.19-1.22ppm(8H,multiplet)、1.26-1.28(3H、doublet)、1.32-1.41ppm(2H,sextet)、1.86-2.00ppm(2H,multiplet)、3.39-3.48ppm(1H,septet)、3.69-3.78ppm(1H,septet)
(4)元素分析(理論値)
C:54.9(55.04%)、H:8.8%(8.85%)、N:10.8(10.70%)
実施例1~5で得られた本発明の化合物No.10、31、46、74および214並びに下記の比較化合物1および2について、TG-DTA測定装置を用いて、常圧雰囲気下(760torr)での加熱によってサンプル質量が50質量%減少した時点の温度(L)を確認した。Lが低いものは蒸気圧が高いことから好ましいと判断することができる。また、25℃における状態を目視で観測した。25℃において固体であるものについては、融点測定を行った。これらの結果を表1に示す。なお、下記比較化合物1および比較化合物2の化学式において「Me」はメチルを表し、「Et」はエチルを表し、「tBu」は第三ブチルを表す。
化合物No.10を原子層堆積法用原料とし、図1に示す装置を用いて以下の条件のALD法により、シリコンウエハ上に金属ルテニウム薄膜を製造した。
得られた薄膜をX線光電子分光法による薄膜組成の確認したところ、得られた薄膜は金属ルテニウムであり、残留炭素含有量は1.0atom%よりも少なかった。また、X線反射率法による膜厚測定を行い、その平均値を算出したところ、膜厚は平均26.4nmであり、1サイクル当たりに得られる膜厚は平均0.05nmであった。
基板:シリコンウェハ
反応温度(シリコンウエハ温度):350℃
反応性ガス:酸素
下記(1)~(4)からなる一連の工程を1サイクルとして、500サイクル繰り返した:
(1)原料容器温度:140℃、原料容器内圧力:100Paの条件で気化させた原子層堆積法用原料を成膜チャンバーに導入し、系圧力:100Paで30秒間堆積させる;
(2)15秒間のアルゴンパージにより、堆積しなかった原料を除去する;
(3)反応性ガスを成膜チャンバーに導入し、系圧力:100Paで5秒間反応させる;
(4)15秒間のアルゴンパージにより、未反応の反応性ガス及び副生ガスを除去する。
原子層堆積法用原料として化合物No.31を用いたこと以外は実施例6と同様の条件で金属ルテニウム薄膜を製造した。得られた薄膜をX線光電子分光法による薄膜組成の確認したところ、得られた薄膜は金属ルテニウムであり、残留炭素含有量は1.0atom%よりも少なかった。また、X線反射率法による膜厚測定を行い、その平均値を算出したところ、膜厚は平均25.7nmであり、1サイクル当たりに得られる膜厚は平均0.05nmであった。
原子層堆積法用原料として化合物No.46を用いたこと以外は実施例6と同様の条件で金属ルテニウム薄膜を製造した。得られた薄膜をX線光電子分光法による薄膜組成の確認したところ、得られた薄膜は金属ルテニウムであり、残留炭素含有量は1.0atom%よりも少なかった。また、X線反射率法による膜厚測定を行い、その平均値を算出したところ、膜厚は平均26.3nmであり、1サイクル当たりに得られる膜厚は平均0.05nmであった。
化合物No.10を原子層堆積法用原料とし、図1に示す装置を用いて以下の条件のALD法により、シリコンウエハ上に金属ルテニウム薄膜を製造した。
得られた薄膜をX線光電子分光法による薄膜組成の確認したところ、得られた薄膜は金属ルテニウムであり、残留炭素含有量は1.0atom%よりも少なかった。また、X線反射率法による膜厚測定を行い、その平均値を算出したところ、膜厚は平均15nmであり、1サイクル当たりに得られる膜厚は平均0.03nmであった。
基板:シリコンウェハ
反応温度(シリコンウエハ温度);350℃
反応性ガス:水素
下記(1)~(4)からなる一連の工程を1サイクルとして、500サイクル繰り返した。
(1)原料容器温度:140℃、原料容器内圧力:100Paの条件で気化させた原子層堆積法用原料を成膜チャンバーに導入し、系圧力:100Paで30秒間堆積させる。
(2)15秒間のアルゴンパージにより、堆積しなかった原料を除去する。
(3)反応性ガスを成膜チャンバーに導入し、系圧力:100Paで60秒間反応させる。
(4)15秒間のアルゴンパージにより、未反応の第一の反応性ガス及び副生ガスを除去する。
原子層堆積法用原料として比較化合物2を用いたこと以外は実施例6と同様の条件で金属ルテニウム薄膜を製造した。得られた薄膜をX線光電子分光法による薄膜組成の確認したところ、得られた薄膜は金属ルテニウムであり、残留炭素含有量は6.0atom%だった。また、X線反射率法による膜厚測定を行い、その平均値を算出したところ、膜厚は平均10nmであり、1サイクル当たりに得られる膜厚は平均0.02nmであった。
以上の結果より、本発明によれば、ALD法により高品質な金属ルテニウム薄膜を生産性よく製造することができることがわかった。
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