JP5290488B2 - 酸化物、ケイ酸塩及びリン酸塩の気相成長 - Google Patents
酸化物、ケイ酸塩及びリン酸塩の気相成長 Download PDFInfo
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- JP5290488B2 JP5290488B2 JP2002530823A JP2002530823A JP5290488B2 JP 5290488 B2 JP5290488 B2 JP 5290488B2 JP 2002530823 A JP2002530823 A JP 2002530823A JP 2002530823 A JP2002530823 A JP 2002530823A JP 5290488 B2 JP5290488 B2 JP 5290488B2
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- tetramethylpiperidide
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- 229910019142 PO4 Inorganic materials 0.000 title claims description 16
- 235000021317 phosphate Nutrition 0.000 title abstract description 19
- 150000003013 phosphoric acid derivatives Chemical class 0.000 title abstract description 6
- 150000004760 silicates Chemical class 0.000 title description 3
- 239000000758 substrate Substances 0.000 claims abstract description 57
- 229910052751 metal Inorganic materials 0.000 claims description 79
- 239000002184 metal Substances 0.000 claims description 79
- 238000000034 method Methods 0.000 claims description 71
- 238000000151 deposition Methods 0.000 claims description 55
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 40
- 125000000217 alkyl group Chemical group 0.000 claims description 35
- 229910052710 silicon Inorganic materials 0.000 claims description 33
- 239000010703 silicon Substances 0.000 claims description 32
- 150000001875 compounds Chemical class 0.000 claims description 31
- 239000000463 material Substances 0.000 claims description 30
- 150000002736 metal compounds Chemical class 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 26
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 19
- 229910052698 phosphorus Inorganic materials 0.000 claims description 19
- 239000011574 phosphorus Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- 150000002739 metals Chemical class 0.000 claims description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 16
- 239000010452 phosphate Substances 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 15
- 229910044991 metal oxide Inorganic materials 0.000 claims description 15
- 239000001301 oxygen Substances 0.000 claims description 15
- 229910052760 oxygen Inorganic materials 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 150000004706 metal oxides Chemical class 0.000 claims description 12
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- 150000001408 amides Chemical class 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
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- 150000002902 organometallic compounds Chemical class 0.000 claims description 8
- LXQDURMACZWAQQ-UHFFFAOYSA-N 5-propan-2-ylcyclopenta-1,3-diene Chemical compound CC(C)[C-]1C=CC=C1 LXQDURMACZWAQQ-UHFFFAOYSA-N 0.000 claims description 7
- SINKOGOPEQSHQD-UHFFFAOYSA-N cyclopentadienide Chemical compound C=1C=C[CH-]C=1 SINKOGOPEQSHQD-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 6
- DGVVJWXRCWCCOD-UHFFFAOYSA-N naphthalene;hydrate Chemical compound O.C1=CC=CC2=CC=CC=C21 DGVVJWXRCWCCOD-UHFFFAOYSA-N 0.000 claims description 6
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 5
- 125000004429 atom Chemical group 0.000 claims description 5
- VEFXTGTZJOWDOF-UHFFFAOYSA-N benzene;hydrate Chemical group O.C1=CC=CC=C1 VEFXTGTZJOWDOF-UHFFFAOYSA-N 0.000 claims description 5
- VYXHVRARDIDEHS-QGTKBVGQSA-N (1z,5z)-cycloocta-1,5-diene Chemical class C\1C\C=C/CC\C=C/1 VYXHVRARDIDEHS-QGTKBVGQSA-N 0.000 claims description 4
- QMVYKBHBPAIDKO-UHFFFAOYSA-N 1,2,3,5-tetramethyl-4-propan-2-ylcyclopenta-1,3-diene Chemical compound CC(C)c1c(C)c(C)c(C)[c-]1C QMVYKBHBPAIDKO-UHFFFAOYSA-N 0.000 claims description 4
- GVBQJUYCOGRYRE-UHFFFAOYSA-N 5-butylcyclopenta-1,3-diene Chemical compound CCCC[C-]1C=CC=C1 GVBQJUYCOGRYRE-UHFFFAOYSA-N 0.000 claims description 4
- AFEDCUJOGZYIMY-UHFFFAOYSA-N 5-propylcyclopenta-1,3-diene Chemical compound CCC[C-]1C=CC=C1 AFEDCUJOGZYIMY-UHFFFAOYSA-N 0.000 claims description 4
- XWVMGDDMXTWPGA-UHFFFAOYSA-N CCC1=CC=CC=[C-]1 Chemical class CCC1=CC=CC=[C-]1 XWVMGDDMXTWPGA-UHFFFAOYSA-N 0.000 claims description 4
- BJISZDCMBMQNIY-UHFFFAOYSA-N benzene Chemical compound [C-]1=CC=CC=C1 BJISZDCMBMQNIY-UHFFFAOYSA-N 0.000 claims description 4
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- 125000003709 fluoroalkyl group Chemical group 0.000 claims description 4
- SYSQUGFVNFXIIT-UHFFFAOYSA-N n-[4-(1,3-benzoxazol-2-yl)phenyl]-4-nitrobenzenesulfonamide Chemical class C1=CC([N+](=O)[O-])=CC=C1S(=O)(=O)NC1=CC=C(C=2OC3=CC=CC=C3N=2)C=C1 SYSQUGFVNFXIIT-UHFFFAOYSA-N 0.000 claims description 4
- GPVVSRKZVHQKIX-UHFFFAOYSA-N 1,2,3,4,5-pentamethylcyclopenta-1,3-diene Chemical compound CC=1C(C)=C(C)[C-](C)C=1C GPVVSRKZVHQKIX-UHFFFAOYSA-N 0.000 claims description 3
- 125000003368 amide group Chemical group 0.000 claims description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- DYIPSYFMBOEWDW-UHFFFAOYSA-N 5-ethylcyclopenta-1,3-diene Chemical compound CC[C-]1C=CC=C1 DYIPSYFMBOEWDW-UHFFFAOYSA-N 0.000 claims description 2
- IIEWJVIFRVWJOD-UHFFFAOYSA-N ethylcyclohexane Chemical compound CCC1CCCCC1 IIEWJVIFRVWJOD-UHFFFAOYSA-N 0.000 claims 4
- 235000016068 Berberis vulgaris Nutrition 0.000 claims 3
- 241000335053 Beta vulgaris Species 0.000 claims 3
- 101150039077 CRCP gene Proteins 0.000 claims 3
- 101150002402 Smcp gene Proteins 0.000 claims 3
- WLNIUEYAQZRJFS-UHFFFAOYSA-N bis[bis(trimethylsilyl)amino]tin Chemical compound C[Si](C)(C)N([Si](C)(C)C)[Sn]N([Si](C)(C)C)[Si](C)(C)C WLNIUEYAQZRJFS-UHFFFAOYSA-N 0.000 claims 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 2
- 239000010931 gold Substances 0.000 claims 2
- 229910052737 gold Inorganic materials 0.000 claims 2
- HYICSHJTKJTQBT-UHFFFAOYSA-N penta-1,3-diene Chemical compound CC=CC=[CH-] HYICSHJTKJTQBT-UHFFFAOYSA-N 0.000 claims 2
- 108010000020 Platelet Factor 3 Proteins 0.000 claims 1
- 150000002009 diols Chemical class 0.000 claims 1
- WQIQNKQYEUMPBM-UHFFFAOYSA-N pentamethylcyclopentadiene Chemical compound CC1C(C)=C(C)C(C)=C1C WQIQNKQYEUMPBM-UHFFFAOYSA-N 0.000 claims 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical group [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 38
- 229910052914 metal silicate Inorganic materials 0.000 abstract description 20
- 229910001463 metal phosphate Inorganic materials 0.000 abstract description 14
- 238000000231 atomic layer deposition Methods 0.000 description 67
- 239000002243 precursor Substances 0.000 description 63
- 239000010408 film Substances 0.000 description 57
- 230000008021 deposition Effects 0.000 description 52
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 35
- 239000000376 reactant Substances 0.000 description 34
- 238000005229 chemical vapour deposition Methods 0.000 description 29
- -1 lanthanum silicates Chemical class 0.000 description 23
- 239000012159 carrier gas Substances 0.000 description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 21
- 239000000243 solution Substances 0.000 description 20
- 239000007788 liquid Substances 0.000 description 17
- 239000007983 Tris buffer Substances 0.000 description 14
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 13
- 229910052735 hafnium Inorganic materials 0.000 description 12
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 12
- HLDBBQREZCVBMA-UHFFFAOYSA-N hydroxy-tris[(2-methylpropan-2-yl)oxy]silane Chemical compound CC(C)(C)O[Si](O)(OC(C)(C)C)OC(C)(C)C HLDBBQREZCVBMA-UHFFFAOYSA-N 0.000 description 12
- 229910052746 lanthanum Inorganic materials 0.000 description 12
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 11
- 239000007789 gas Substances 0.000 description 11
- 229910000449 hafnium oxide Inorganic materials 0.000 description 11
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 11
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 11
- 239000012686 silicon precursor Substances 0.000 description 11
- 230000009257 reactivity Effects 0.000 description 10
- 239000000377 silicon dioxide Substances 0.000 description 10
- 235000012239 silicon dioxide Nutrition 0.000 description 10
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 9
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 9
- 229910052752 metalloid Inorganic materials 0.000 description 9
- 229910052727 yttrium Inorganic materials 0.000 description 9
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 9
- 229910052726 zirconium Inorganic materials 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 8
- 230000008901 benefit Effects 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- WZPMZMCZAGFKOC-UHFFFAOYSA-N diisopropyl hydrogen phosphate Chemical group CC(C)OP(O)(=O)OC(C)C WZPMZMCZAGFKOC-UHFFFAOYSA-N 0.000 description 8
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 8
- 229910001386 lithium phosphate Inorganic materials 0.000 description 8
- 239000012528 membrane Substances 0.000 description 8
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 8
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 description 8
- 230000002378 acidificating effect Effects 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 7
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- 125000001827 mesitylenyl group Chemical group [H]C1=C(C(*)=C(C([H])=C1C([H])([H])[H])C([H])([H])[H])C([H])([H])[H] 0.000 description 7
- 150000002737 metalloid compounds Chemical class 0.000 description 7
- 238000006557 surface reaction Methods 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
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- 238000005481 NMR spectroscopy Methods 0.000 description 6
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- 239000012688 phosphorus precursor Substances 0.000 description 6
- VSAISIQCTGDGPU-UHFFFAOYSA-N tetraphosphorus hexaoxide Chemical compound O1P(O2)OP3OP1OP2O3 VSAISIQCTGDGPU-UHFFFAOYSA-N 0.000 description 6
- MSXVEPNJUHWQHW-UHFFFAOYSA-N 2-methylbutan-2-ol Chemical compound CCC(C)(C)O MSXVEPNJUHWQHW-UHFFFAOYSA-N 0.000 description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
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- 239000000460 chlorine Substances 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
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- 150000001298 alcohols Chemical class 0.000 description 4
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- 238000000572 ellipsometry Methods 0.000 description 4
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- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(iv) oxide Chemical compound O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 4
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- 239000000843 powder Substances 0.000 description 4
- 238000005001 rutherford backscattering spectroscopy Methods 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- KCIKCCHXZMLVDE-UHFFFAOYSA-N silanediol Chemical compound O[SiH2]O KCIKCCHXZMLVDE-UHFFFAOYSA-N 0.000 description 4
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- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 4
- 229910020175 SiOH Inorganic materials 0.000 description 3
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- 239000003989 dielectric material Substances 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 3
- AXPPAKIFWZPHCR-UHFFFAOYSA-N lithium;bis[ethyl(dimethyl)silyl]azanide Chemical compound [Li+].CC[Si](C)(C)[N-][Si](C)(C)CC AXPPAKIFWZPHCR-UHFFFAOYSA-N 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
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- 239000000126 substance Substances 0.000 description 3
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- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 3
- 238000009834 vaporization Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
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- 238000000560 X-ray reflectometry Methods 0.000 description 2
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- 125000003342 alkenyl group Chemical group 0.000 description 2
- 125000005233 alkylalcohol group Chemical group 0.000 description 2
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- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 description 2
- ZDYNTRMQDURVDM-UHFFFAOYSA-N bis(trimethylsilyl)azanide;lanthanum(3+) Chemical compound [La+3].C[Si](C)(C)[N-][Si](C)(C)C.C[Si](C)(C)[N-][Si](C)(C)C.C[Si](C)(C)[N-][Si](C)(C)C ZDYNTRMQDURVDM-UHFFFAOYSA-N 0.000 description 2
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- 238000011109 contamination Methods 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- UCQFCFPECQILOL-UHFFFAOYSA-N diethyl hydrogen phosphate Chemical compound CCOP(O)(=O)OCC UCQFCFPECQILOL-UHFFFAOYSA-N 0.000 description 2
- 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 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 description 2
- ORJFXWYTRPGGRK-UHFFFAOYSA-N hydroxy-tris(2-methylbutan-2-yloxy)silane Chemical compound CCC(C)(C)O[Si](O)(OC(C)(C)CC)OC(C)(C)CC ORJFXWYTRPGGRK-UHFFFAOYSA-N 0.000 description 2
- 239000010416 ion conductor Substances 0.000 description 2
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- 150000002738 metalloids Chemical class 0.000 description 2
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- 229910052759 nickel Inorganic materials 0.000 description 2
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- 239000003960 organic solvent Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 229910001392 phosphorus oxide Inorganic materials 0.000 description 2
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 2
- 238000009832 plasma treatment Methods 0.000 description 2
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- 238000012552 review Methods 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UVVUGWBBCDFNSD-UHFFFAOYSA-N tetraisocyanatosilane Chemical compound O=C=N[Si](N=C=O)(N=C=O)N=C=O UVVUGWBBCDFNSD-UHFFFAOYSA-N 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 0 *N1[Si+]N(*)C=C1 Chemical compound *N1[Si+]N(*)C=C1 0.000 description 1
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Images
Classifications
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Description
本発明は、化学気相成長(CVD)及び原子層堆積(ALD)といったような薄膜被着プロセスにおいて使用するための新規の薬剤に関する。これらの薬剤は、一般に金属酸化物、ケイ酸塩又は金属リン酸塩或いは二酸化ケイ素と呼ばれる、金属及び/又は酸素を伴うケイ素及び/又はリンを含有する材料の被着のために使用することができる。
化学気相成長(CVD)は、蒸気相内の反応物からコーティング又は粉末といったような固体材料を形成するための広く使用されている方法である。CVD法の広範な概説が最近「非金属のCVD」,W.S.Rees, Jr., Editor, VCH Publishers, Weinheim, Germany, 1996,「化合物半導体のCVD」 ,A. C. Jonesand P. O' Brien, VCH, 1996,及び「金属CVDの化学」,T. Kodas and M. Hampden-Smith, Editors, VCH, 1994に示された。
本発明の主たる特徴には、金属ケイ酸塩、リン酸塩又は酸化物のCVD又はALD用に適合された反応性をもつ揮発性の化学的前駆体が含まれる。
1.金属ケイ酸塩及び二酸化ケイ素
本発明は、金属及びケイ素含有量がいろいろの金属ケイ酸塩を調製するための方法を提供する。この方法は、アルコキシシラノール又はアルコキシシランジオールの蒸気と、1種以上の金属又はメタロイド化合物の蒸気との反応を必要とする。化合物は、基板上、そして一部の態様では加熱された基板上に、粉末として又は膜として形成され得る。化合物は、基板上への被着に先立ち金属又はメタロイド化合物の蒸気とアルコキシシラノール又はアルコキシシランジオールの蒸気を混合することによって、基板上に形成され得る。少なくとも一部の態様では、基板を、アルコキシシラノール又はアルコキシシランジオール蒸気と、金属又はメタロイド化合物のうちの1種以上のものの蒸気に対して交互に露出させる。
本発明は、金属及びリン含有量がいろいろの金属リン酸塩を調製するための方法を提供する。この方法は、ビス(アルキル)ホスフェートの蒸気と1種以上の金属又はメタロイド化合物の蒸気の反応を伴う。化合物は、基板上そして一部の態様では加熱された基板上に、粉末又は膜として形成され得る。化合物は、基板上への被着に先立ち金属又はメタロイド化合物とビス(アルキル)ホスフェートの蒸気を混合することによって、基板上に形成され得る。少なくとも一部の態様においては、基板は、ビス(アルキル)ホスフェートの蒸気及び1種以上の金属又はメタロイド化合物の蒸気に対して交互に露出される。
少なくとも一部の態様において、金属又はメタロイドアミドが、本発明を実施する上で有用である。いくつかの例を、販売元及び/又はその合成のための参考文献と共に、表1に示す。表1内に挙げられているメタロイドは、ホウ素、ケイ素及びヒ素である。
少なくとも一部の態様において、シラノール又はリン酸塩の一部分は、金属富有ケイ酸塩及びリン酸塩を被着させるため水と置き換えられる。CVD反応装置において、水蒸気は、蒸気の入口の近くで金属前駆体の蒸気と非常に急速に反応して基板上に膜ではなくむしろ粉末を生成する傾向をもつ。ALD反応装置においては、反応物は反応装置内に交互に導入され、従って入口近くの反応が防止されそして反応は基板の表面に限定されることから、そのような早すぎる反応は回避される。しかしながら、水は表面に強く吸着する傾向をもち、従って反応物のパルスの間にALD反応装置をパージするのに長い時間がかかることがある。
液体前駆体の蒸気は、バブラー内、薄膜蒸発器内での加熱を含めた従来の方法によって、又は約100〜250℃に予熱されたキャリヤガスへの噴霧によって、形成できる。噴霧は、空気圧式又は超音波式に実施可能である。固体前駆体は、デカン、ドデカン、テトラデカン、トルエン、キシレン及びメシチレンといったような炭化水素を含めた有機溶剤に、かつエーテル、エステル、ケトン及び塩素化炭化水素と共に、溶解させることができる。液体前駆体の溶液は一般に、純粋液体よりも低い粘度を有し、そのため、場合によっては、純粋液体ではなくむしろ溶液を噴霧し蒸発させる方が好ましいことがある。液体又は溶液は、薄膜蒸発器で又は加熱ゾーン内への液体の直接注入によって蒸発させることもできる。薄膜蒸発器はArtisan Industries(Waltham, Massachusetts)により製造されている。液体の直接気化用の商業用設備はMKS Instruments(Andover, Massachusetts)、ATMI, Inc.(Danbury, Connecticut)、Novellus Systems, Inc.(San Jose, California)及びCOVA Technologies (Colorado Springs, CO)により製造されている。超音波噴霧機(ultrasonic nebulizer)は、Sonotek Corporation (Milton, New York)及びCetac Technologies (Omaha, Nebraska)により製造されている。
n=(Peq−Pdep)(V/RT1) (14)
(式中のRは気体定数である)に従うものと仮定することによって推定することができる。この式はまた、前駆体蒸気を放出するべく弁70が開放している短かい時間に弁70を通して管90からのキャリヤガスがチャンバ60内に入らないということも仮定している。前駆体蒸気とキャリヤガスとの混合が弁70の開放時間中に起こらなければ、より多量の前駆体蒸気を、チャンバ60内の残留前駆体蒸気が全てキャリヤガスにより置き換えられた場合の最大値、すなわち、
n=(Peq)(V/RT1) (15)
に至るまで、送給することができる。比較的高い蒸気圧(Peq≫Pdep)をもつ前駆体については、前駆体量のこれら2つの推定値の間に大きな差異はない。
n=(Peq/Ptot)(Ptot−Pdep)(V/RT1) (16)
なお、式中のVはチャンバ10内の蒸気空間30の体積である。この投入分は、弁230を開放することにより送給される。管90からのキャリヤガスが弁230開放時間中に体積30の中に入った場合には、この推定値よりも幾分か大きい量を送給することができる。体積Vを充分大きいものにすることによって、表面反応を飽和させるのに間違いなく充分大きい前躯体投入量を送給することができる。蒸気圧Peqが低すぎて所要体積Vが非実際的なほどに大きくなる場合には、体積Vからの追加投入量を、その他の反応物の投入量の送給に先立ち送給することができる。
トリス(tert−ブトキシ)シラノールのメシチレン溶液(1重量%)を、0.4L/分で窒素ガスが流れる外径1/16インチのT字継手に6ml/時の速度で圧送した。結果として発生した霧状物は、250℃に加熱した管内に流れ込んだ。テトラキス(エチルメチルアミド)ジルコニウムのメシチレン溶液(1重量%)を、0.4L/分で窒素ガスが流れるもう1つのT字継手に12ml/時の速度で圧送した。結果として発生した霧状物は、同じ加熱された管内に流入した。ガスの圧力は、液体窒素トラップを経由してガラス管の出口に取り付けられた真空ポンプにより5Torrに維持した。管の内部に設置されたケイ素及びガラス状炭素の基板に、管の長さに沿って厚みの変動するケイ酸ジルコニウムの膜でコーティングを施した。ラザフォード後方散乱分光法で膜を分析すると、ガラス状炭素上に被着した膜についてZrSi2O6という組成が得られた。膜内には炭素又は窒素は検出されなかった。ケイ素上に被着した膜の屈折率は、楕円偏光法により約1.6であることが分かった。
前駆体を連続的にではなく5秒の間隔をおいた交番パルスで注入したという点を除いて、例1を反復した。同様の組成、つまりZrSi2O6の膜が、加熱ゾーンの全長に沿って均一の厚みで被着した。厚みは1サイクルあたり約0.3nmであった。
テトラキス(エチルメチルアミド)ジルコニウムの代わりにテトラキス(エチルメチルアミド)ハフニウムを用いて、例1を反復した。およそHfSi2O6という組成の膜が形成された。膜中には炭素又は窒素は検出されなかった。ケイ素上に被着した膜の屈折率は、楕円偏光法により約1.6であることが分かった。
前駆体を連続的にではなく5秒の間隔をおいた交番パルスで注入したという点を除いて、例3を反復した。同様の組成、つまりHfSi2O6の膜が、加熱ゾーンの全長に沿って均一の厚みで被着した。厚みは1サイクルあたり約0.3nmであった。
テトラキス(エチルメチルアミド)ジルコニウムの代わりにトリス(tert−ブチル(トリメチルシリル)アミド)イットリウムを用いて例1を反復した。およそY2Si2O7の組成の膜が形成された。膜中には炭素又は窒素は検出されなかった。ケイ素上に被着した膜の屈折率は、楕円偏光法により約1.6であることが分かった。
前駆体を連続的にではなく5秒の間隔をおいた交番パルスで注入したという点を除いて、例5を反復した。同様の組成、つまりY2Si2O7の膜が、加熱ゾーンの全長に沿って均一の厚みで被着した。厚みは1サイクルあたり約0.3nmであった。組成はおよそY2Si2O7であった。
テトラキス(エチルメチルアミド)ジルコニウムの代わりにトリス(ビス(トリメチルシリル)アミド)ランタンを、メシチレンの代わりにテトラデカンを用いて、例1を反復した。La:Si比が約0.9である膜が、ガラス状炭素基板上に250℃の基板温度で形成された。膜中には炭素又は窒素は検出されなかった。
前駆体を連続的にではなく5秒の間隔をおいた交番パルスで注入したという点を除いて、例7を反復した。同様の組成の膜が、加熱ゾーンの全長に沿って均一の厚みで被着した。
液体のリチウムビス(エチルジメチルシリル)アミド(1重量部)をメシチレン(99部)と混合した。得られた溶液を、250℃に加熱した炉内で管(内径24mm)内部の被着ゾーンへ0.30L/分で流入する窒素ガスへ、T字継手へと12ml/時の速度で圧送することによって噴霧した。同時に、ジイソプロピルホスフェートの1%メシチレン溶液を、同一の管状炉内に0.30L/分で流入するもう1つの窒素キャリヤガス流中へ同じように噴霧した。ガス圧は、液体窒素トラップを経由してガラス管の出口に取り付けられた真空ポンプにより5Torrに維持した。ガラス管の底に置かれたシリコン基板上ならびに管の内部にも、薄い膜が被着した。厚みプロフィールは、管状炉へのガスの入口近くでピークを示した。膜をX線光電子分光法により分析し、リチウム、リン及び酸素を含むことがわかった。
材料を5秒の時間的間隔をおいた交番パルスで導入することに変更して、例9を反復した。被着ゾーン全体を通して厚みがほぼ一定であったという点を除き、同様のリン酸リチウム膜が被着した。
ケイ素前駆体のみを用いジルコニウム前駆体は用いずに、例1を反復した。膜は被着しなかった。
ジルコニウム前駆体のみを用いケイ素前駆体は用いずに、例1を反復した。膜は被着しなかった。
ハフニウム前駆体のみを用いケイ素前駆体は用いずに、例3を反復した。膜は被着しなかった。
イットリウム前駆体のみを用いケイ素前駆体は用いずに、例5を反復した。膜は被着しなかった。
ランタン前駆体のみを用いケイ素前駆体は用いずに、例7を反復した。膜は被着しなかった。
リン前駆体のみを用いリチウム前駆体は用いずに、例9を反復した。膜は被着しなかった。
リチウム前駆体のみを用いリン前駆体は用いずに、例9を反復した。膜は被着しなかった。
窒素キャリヤガス中へ前躯体の溶液のパルスを送給するのに自動車用燃料インジェクタ(フォードCM−4722F13Z−9F593−A型)を用いて、ALD例2、4、6、8及び10を反復した。弁が約50ミリ秒開放される毎に、約0.05mの溶液が送給された。同様の結果が得られた。
図1の装置を使用して酸化ハフニウムの層を被着させた。250℃に保った被着チャンバ内に5秒毎に交互に、0.5×10-9モル/cm2の量テトラキス(ジメチルアミド)ハフニウム蒸気及び4×10-9モル/cm2の量の水蒸気を注入した。チャンバには、0.15Torrの圧力を維持するのに充分な窒素キャリヤガスの連続流も供給した。被着チャンバは、チャンバを通る気体流の方向に対し垂直な平面内で2.3平方センチメートルの断面積であった。被着チャンバの出口は、約0.012秒で被着チャンバに等しい体積を吸い出すのに充分な能力(195リットル/分)をもつ真空ポンプに接続した。
テトラキス(ジメチルアミド)ハフニウムの代わりにテトラキス(ジメチルアミド)ジルコニウムを用いて、例12を反復した。同様の特性をもつ二酸化ジルコニウムの膜が被着した。
水蒸気の代わりにtert−ブタノール蒸気を用いて例12を反復した。同様の特性をもつ二酸化ハフニウムの膜が被着した。
テトラキス(ジメチルアミド)ハフニウム蒸気の代わりにエチルイミドトリス(ジエチルアミド)タンタル蒸気用いて、例12を反復した。Ta2O5の透明な膜が被着した。それらは、屈折率が2.2であり、1サイクルあたりの厚みが約0.06nmであった。
基板温度400℃で、ジイソプロピルホスフェートとトリメチルアルミニウムの蒸気の3×10-9モル/cm2という投入量を交互に用いてALDを実施した。おおよそAl2P4O13の組成をもつ透明なリン酸アルミニウム膜が、1サイクルあたり0.1nmの速度で被着した。それらの屈折率は約1.5であった。
基板温度300℃で、3×10-9モル/cm2の量のトリメチルアルミニウム蒸気と1.2×10-8モル/cm2の量のトリス(tert−ブトキシ)シラノール蒸気を交互に用いてALDを実施した。おおよそAl2Si8O19という組成を有する透明なケイ酸アルミニウム膜が、1サイクルあたり1nmという著しく高い速度で被着した。それらの屈折率は約1.48であった。膜の表面は非常に平滑である。原子間力顕微鏡により、厚さ150nmのケイ酸アルミニウム膜について0.8nm未満の根平均二乗粗さが測定された。シリカ基板上の厚さ2マイクロメータの膜における引張応力は、約0.2ギガパスカルであると測定された。単結晶ケイ素上に被着した同様の膜は、0.03ギガパスカルというそれより小さい引張応力を示した。厚さ6ミクロンの膜は、引張応力を原因とする亀裂や剥離を示した。
基板温度200℃で、3×10-9モル/cm2の量のトリメチルアルミニウム蒸気と3×10-8モル/cm2の量のトリス(tert−ブトキシ)シラノール蒸気を交互に用いてALDを実施した。おおよそAl2Si16O35の組成を有する透明なケイ酸アルミニウム膜が、1サイクルあたり2nmという著しく高い速度で被着した。それらの屈折率は約1.47であった。
基板温度250℃で、3×10-9モル/cm2の量のトリス(ジメチルアミノ)アルミニウム蒸気と3×10-8モル/cm2のトリス(tert−ブトキシ)シラノール蒸気を交互に用いてALDを実施した。0.1nm/サイクルの厚み及び約1.46の屈折率をもつケイ酸アルミニウム膜が形成された。
トリス(tert−ブトキシ)シラノール蒸気の代わりにトリス(tert−ペンチルオキシ)シラノール蒸気を用いて、例19を反復した。同様の結果が得られた。
トリス(ジメチルアミノ)アルミニウム蒸気とトリス(tert−ブトキシ)シラノール蒸気の投入の間に水蒸気を投入して、例19を反復した。気体流の方向に沿って0.1nm/サイクル(±1%)という非常に均一の厚みをもつ同様の膜が得られた。
テトラキス(ジメチルアミド)ハフニウム蒸気の代わりにトリス(ビス(トリメチルシリル)アミド)ランタン蒸気を用い、図2の装置を上述の通りに使用して、例12を反復した。250℃の基板温度で基板上に約2というLa:Si比をもつ透明な酸化物膜が形成された。膜中に炭素又は窒素は検出されなかった。それらの屈折率は1.7、厚さは1サイクルあたり約0.1nmである。
図2の装置を用い、トリス (2,2,6,6−テトラメチルピペリジド)ランタン蒸気と水蒸気を交互に投入してALDを実施し、酸化ランタン膜を形成することができる。
テトライソシアナトシラン蒸気及びトリス (tert−ブトキシ)シラノール蒸気を交互に投入してALDを実施し、酸化ケイ素腹を形成することができる。これらの比較的反応性が低い前駆体については、より大きい露出流束(>10-7ラングミュア)が必要とされる。
Claims (28)
- ケイ素、酸素及び1種以上の金属を含む材料を形成するための方法であって、
アルコキシシラノール及びアルコキシシランジオールのうちの一方の蒸気を金属化合物の1種以上のものの蒸気と一緒に反応させること、
を含む材料形成方法。
- ケイ素、酸素及び1種以上の金属を含む材料を形成するための方法であって、
アルコキシシラノール及びアルコキシシランジオールのうちの一方の蒸気及び金属化合物の1種以上のものの蒸気に対して交互に基板を露出させて基板上に膜を形成すること、
を含む材料形成方法。
- 化合物を基板上に膜として被着させる、請求項1に記載の方法。
- Rn基が1〜4個の炭素を含有し、同一の又は異なるものである、請求項4に記載の方法。
- Rn基が全てメチル基である、請求項5に記載の方法。
- 金属化合物が金属−窒素結合を含有する、請求項1又は2に記載の方法。
- 金属化合物が次の化合物、すなわち、Al(N(SiMe 3 ) 2 ) 3 、Al 2 (NEt 2 ) 6 、Al 2 (NEtMe) 6 、Al(N i Pr 2 ) 3 、Al 2 (NMe 2 ) 6 、Al(N(Et)CH 2 CH 2 NMe 2 )(NMe 2 ) 2 、As(NMe 2 ) 3 、As(N(Me)(SiMe 3 )) 3 、B(NMe 2 ) 3 、B(NEt 2 ) 3 、Ba(N(SiMe 3 ) 2 ) 2 、Be(NMe 2 ) 2 、Be(N(SiMe 3 ) 2 ) 2 、Be(2,2,6,6-テトラメチルピペリジド) 2 、Bi(N(SiMe 3 ) 2 ) 3 、Bi(N(Me)(SiMe 3 )) 3 、Ca(N(SiMe 3 ) 2 ) 2 、Cd(N(SiMe 3 ) 2 ) 2 、Cd(N t BuSiMe 3 ) 2 、Cd(2,2,6,6-テトラメチルピペリジド) 2 、Ce(N(SiMe 3 ) 2 ) 3 、Ce(N i Pr 2 ) 3 、Co(N(SiBuMe 2 ) 2 ) 2 、Co(N(SiEtMe 2 ) 2 ) 2 、Co(N(SiMe 3 ) 2 ) 2 、Co(N(SiMe 3 ) 2 ) 3 、Co(N(SiPrMe 2 ) 2 ) 2 、Cr(N(SiMe 3 ) 2 ) 3 、Cr(NEt 2 ) 4 、Cr(N i Pr 2 ) 3 、Cr(NMe 2 ) 4 、Cu 4 (N(SiMe 3 ) 2 ) 4 、Er(N(SiMe 3 ) 2 ) 3 、Eu(N(SiMe 3 ) 2 ) 3 、Fe(N(SiBuMe 2 ) 2 ) 2 、Fe(N(SiMe 3 ) 2 ) 2 、Fe(N(SiMe 3 ) 2 ) 3 、Ga(NMe 2 ) 3 、Ga(NEt 2 ) 3 、Ga(N(SiMe 3 ) 2 ) 3 、Ga(N t BuSiMe 3 ) 3 、Ga(2,2,6,6-テトラメチルピペリジド) 3 、Ga(N(Me)CH 2 CH 2 NMe 2 )(NMe 2 ) 2 、Gd(N(SiMe 3 ) 2 ) 3 、Ge(N(SiMe 3 ) 2 ) 2 、Ge(NEt 2 ) 4 、Ge(NMe 2 ) 4 、Ge(N t Bu 2 ) 2 、Ge(N t BuSiMe 3 ) 2 、Ge(2,2,6,6-テトラメチルピペリジド) 2 、Hf(NEt 2 ) 4 、Hf(NEtMe) 4 、Hf(NMe 2 ) 4 、Hg(N(SiMe 3 ) 2 ) 2 、Ho(N(SiMe 3 ) 2 ) 3 、In(N(SiMe 3 ) 2 ) 3 、In(2,2,6,6-テトラメチルピペリジド) 3 、KN(SiHexMe 2 ) 2 、KN(SiMe 3 ) 2 、La(N(SiMe 3 ) 2 ) 3 、La(N t BuSiMe 3 ) 3 、La(N i Pr 2 ) 3 、La(2,2,6,6-テトラメチルピペリジド) 3 、LiN(SiEtMe 2 ) 2 、LiN(SiMe 3 ) 2 、Li(2,2,6,6-テトラメチルピペリジド)、Lu(N(SiMe 3 ) 2 ) 3 、Mg(N(SiMe 3 ) 2 ) 2 、Mg(2,2,6,6-テトラメチルピペリジド) 2 、Mn(N(SiBuMe 2 ) 2 ) 2 、Mn(N(SiMe 3 ) 2 ) 2 、Mn(N(SiMe 3 ) 2 ) 3 、Mo(N t BuSiMe 3 ) 3 、Mo 2 (NEt 2 ) 6 、Mo 2 (NMe 2 ) 6 、Mo(NEt 2 ) 4 、Mo(NMe 2 ) 4 、NaN(Si n BuMe 2 ) 2 、NaN(SiMe 3 ) 2 、Nb(N(SiMe 3 ) 2 ) 3 、Nb(NEt 2 ) 4 、Nb(NEt 2 ) 5 、Nb(NMe 2 ) 5 、Nd(N(SiMe 3 ) 2 ) 3 、Nd(N i Pr 2 ) 3 、Ni(N(SiMe 3 ) 2 ) 2 、Pb(N(SiMe 3 ) 2 ) 2 、Pb(N t BuSiMe 3 ) 2 、Pr(N(SiMe 3 ) 2 ) 3 、Sb(NMe 2 ) 3 、Sb(N(Me)(SiMe 3 )) 3 、Sc(N(SiMe 3 ) 2 ) 3 、SiH 2 (NMe 2 ) 2 、SiH(NMe 2 ) 3 、Si(NMe 2 ) 4 、Si(NHMe) 4 、Si(NHn-Pr) 4 、Si(NEt 2 ) 4 、Si(NCO) 4 、Sm(N(SiMe 3 ) 2 ) 3 、Sn(N(SiMe 3 ) 2 ) 2 、Sn(NEt 2 ) 4 、Sn(NMe 2 ) 4 、Sn(N t Bu 2 ) 2 、Sn(N t Bu 2 ) 3 、Sn(N t BuSiMe 3 ) 2 、Sn(N t BuSiMe 3 ) 3 、Sn(2,2,6,6-テトラメチルピペリジド) 2 , Sr(N(SiMe 3 ) 2 ) 2 、Ta(NEt 2 ) 4 、Ta(NMe 2 ) 5 、Ta(N t Bu)(NEt 2 ) 3 、Ta(NEt)(NEt 2 ) 3 、Tb(N(SiMe 3 ) 2 ) 3 、Th(NEt 2 ) 4 、Th(NPr 2 ) 4 、Ti(N(SiMe 3 ) 2 ) 3 、Ti(NEt 2 ) 4 、Ti(N i Pr 2 ) 3 、Ti(N i Pr 2 ) 4 、Ti(NMe 2 ) 4 、T1(N(SiMe 3 ) 2 ) 3 、U(N(SiMe 3 ) 2 ) 3 、U(NEt 2 ) 4 、U(NPr 2 ) 4 、V(N(SiMe 3 ) 2 ) 3 、V(NEt 2 ) 4 、V(NMe 2 ) 4 、V(O)(NMe 2 ) 3 、W 2 (NEt 2 ) 6 、W 2 (NMeEt) 6 、W 2 (NMe 2 ) 6 、W(N t Bu) 2 (NH t Bu) 2 、W(N t Bu) 2 (NEtMe) 2 、W(N t Bu) 2 (NMe 2 ) 2 、Y(N(SiMe 3 ) 2 ) 3 、Y(N i Pr 2 ) 3 、Y(N t BuSiMe 3 ) 3 、Y(2,2,6,6-テトラメチルピペリジド) 3 、Yb(N(SiMe 3 ) 2 ) 3 、Yb(N i Pr 2 ) 3 、Zn(N(SiMe 3 ) 2 ) 2 、Zn(N t Bu 2 ) 2 、Zn(2,2,6,6-テトラメチルピペリジド) 2 , Zr(NEt 2 ) 4 、Zr(NEtMe) 4 、Zr(N i Pr 2 ) 4 、及びZr(NMe 2 ) 4 、から選択される、請求項8に記載の方法。
- 金属化合物が次の化合物、すなわち、AlMe 3 、Ba(n-PrMe 4 Cp) 2 、Ba( i Pr 4 Cp) 2 、Ba(Me 5 Cp) 2 、BeEt 2 、BiMe 3 、Ca( i Pr 4 Cp) 2 、Ca(Me 5 Cp) 2 、CdMe 2 、CeCp 3 、Ce( i PrCp) 3 、Ce(Me 4 Cp) 3 、CoCp 2 、CoCp(CO) 2 、Co(CO) 3 NO、CrCp 2 、Cr(Me 5 Cp) 2 、Cr( i PrCp) 2 、Cr(EtBz) 2 、CuCpPEt 3 、Er(Cp) 3 、Er( i PrCp) 3 、Er(BuCp) 3 、Eu(Me 4 Cp) 3 、FeCp(Me 2 NCH 2 Cp)、FeCp( l BuCp)、GaMe 3 、GdCp 3 、Gd( i PrCp) 3 、InCp 3 、In(Me 5 Cp) 3 、InMe 3 、Ir(MeCp)(l,5-COD)、La( 1 PrCp) 3 、LaCp 3 、LaCp 3 (NCCH 3 ) 2 、La(Me 2 NC 2 H 4 Cp) 3 、Mg(PrCp) 2 、Mg(EtCp) 2 、MgCp 2 、MnCp 2 、Mn(EtCp) 2 、Mn(Me 5 Cp) 2 、Mo(EtBz) 2 、NdCp 3 、Nd( i PrCp) 3 、Ni(PF 3 ) 4 、PrCp 3 、Pr( i PrCp) 3 、SbEt 3 、ScCp 3 、SmCp 3 、Sm( i PrCp) 3 、Sr( i Pr 4 Cp) 2 、Sr(Me 5 Cp) 2 、TmCp 3 、Tm( i PrCp) 3 、TICp、VCp 2 、V(EtCp) 2 、W( 1 PrCp) 2 H 2 、YCp 3 、Y(MeCp) 3 、Y( n PrCp) 3 、Y(BuCp) 3 、YbCp 3 、Yb( i PrCp) 3 、ZnEt 2 、ZnMe 2 、ZrCp 2 Me 2 、及びZr( t BuCp) 2 Me 2 (これらの式中、Cpはシクロペンタジエニドの略号であり、Me 5 Cpはペンタメチルシクロペンタジエニドを表わし、 i PrCpはイソプロピルシクロペンタジエニドを表わし、 i PrMe 4 Cpはイソプロピルテトラメチルシクロペンタジエニドの略であり、 i Pr 4 Cpはテトライソプロピルシクロペンタジエニドの略であり、EtCpはエチルシクロペンタジエニドの略であり、PrCpはプロピルシクロペンタジエニドの略であり、 i PrCpはイソプロピルシクロペンタジエニドの略であり、BuCpはブチルシクロペンタジエニドの略であり、Bzはベンゼニド、EtBzはエチルベンゼニドの異性体の混合物、1,5−CODは1,5−シクロオクタジエニドの略である)、から選択される、請求項1または2に記載の方法。
- 金属化合物が次の化合物、すなわち、Al 2 Et 3 (O-sec-Bu) 3 、B(OMe) 3 、Hf(O t Bu) 4 、Nb(OEt) 5 、Ta(OEt) 5 、Ti(O i Pr) 4 、Y(OCMe 2 CH 2 NMe 2 ) 3 、及びZr(O t Bu) 4 、から選択される、請求項1又は2に記載の方法。
- リン、酸素及び1種以上の金属を含む材料を形成するための方法であって、
ビス(アルキル)ホスフェートの蒸気を金属化合物の1種以上のものの蒸気と反応させること、
を含む材料形成方法。
- リン、酸素及び1種以上の金属を含む材料を形成するための方法であって、
ビス(アルキル)ホスフェートの蒸気と金属化合物の1種以上のものの蒸気とに対して交互に基板を露出させて基板上に膜を形成すること、
を含む材料形成方法。
- リン、酸素及び1種以上の金属を含む材料を基板上に膜として被着させる、請求項12に記載の方法。
- Rn基が1〜4個の炭素を含有し、同一の又は異なるものであることができる、請求項15に記載の方法。
- 金属化合物が金属−窒素結合を含有する、請求項12又は13に記載の方法。
- 金属化合物が次の化合物、すなわち、Al(N(SiMe 3 ) 2 ) 3 、Al 2 (NEt 2 ) 6 、Al 2 (NEtMe) 6 、Al(N i Pr 2 ) 3 、Al 2 (NMe 2 ) 6 、Al(N(Et)CH 2 CH 2 NMe 2 )(NMe 2 ) 2 、As(NMe 2 ) 3 、As(N(Me)(SiMe 3 )) 3 、B(NMe 2 ) 3 、B(NEt 2 ) 3 、Ba(N(SiMe 3 ) 2 ) 2 、Be(NMe 2 ) 2 、Be(N(SiMe 3 ) 2 ) 2 、Be(2,2,6,6-テトラメチルピペリジド) 2 、Bi(N(SiMe 3 ) 2 ) 3 、Bi(N(Me)(SiMe 3 )) 3 、Ca(N(SiMe 3 ) 2 ) 2 、Cd(N(SiMe 3 ) 2 ) 2 、Cd(N t BuSiMe 3 ) 2 、Cd(2,2,6,6-テトラメチルピペリジド) 2 、Ce(N(SiMe 3 ) 2 ) 3 、Ce(N i Pr 2 ) 3 、Co(N(SiBuMe 2 ) 2 ) 2 、Co(N(SiEtMe 2 ) 2 ) 2 、Co(N(SiMe 3 ) 2 ) 2 、Co(N(SiMe 3 ) 2 ) 3 、Co(N(SiPrMe 2 ) 2 ) 2 、Cr(N(SiMe 3 ) 2 ) 3 、Cr(NEt 2 ) 4 、Cr(N i Pr 2 ) 3 、Cr(NMe 2 ) 4 、Cu 4 (N(SiMe 3 ) 2 ) 4 、Er(N(SiMe 3 ) 2 ) 3 、Eu(N(SiMe 3 ) 2 ) 3 、Fe(N(SiBuMe 2 ) 2 ) 2 、Fe(N(SiMe 3 ) 2 ) 2 、Fe(N(SiMe 3 ) 2 ) 3 、Ga(NMe 2 ) 3 、Ga(NEt 2 ) 3 、Ga(N(SiMe 3 ) 2 ) 3 、Ga(N t BuSiMe 3 ) 3 、Ga(2,2,6,6-テトラメチルピペリジド) 3 、Ga(N(Me)CH 2 CH 2 NMe 2 )(NMe 2 ) 2 、Gd(N(SiMe 3 ) 2 ) 3 、Ge(N(SiMe 3 ) 2 ) 2 、Ge(NEt 2 ) 4 、Ge(NMe 2 ) 4 、Ge(N t Bu 2 ) 2 、Ge(N t BuSiMe 3 ) 2 、Ge(2,2,6,6-テトラメチルピペリジド) 2 、Hf(NEt 2 ) 4 、Hf(NEtMe) 4 、Hf(NMe 2 ) 4 、Hg(N(SiMe 3 ) 2 ) 2 、Ho(N(SiMe 3 ) 2 ) 3 、In(N(SiMe 3 ) 2 ) 3 、In(2,2,6,6-テトラメチルピペリジド) 3 、KN(SiHexMe 2 ) 2 、KN(SiMe 3 ) 2 、La(N(SiMe 3 ) 2 ) 3 、La(N t BuSiMe 3 ) 3 、La(N i Pr 2 ) 3 、La(2,2,6,6-テトラメチルピペリジド) 3 、LiN(SiEtMe 2 ) 2 、LiN(SiMe 3 ) 2 、Li(2,2,6,6-テトラメチルピペリジド)、Lu(N(SiMe 3 ) 2 ) 3 、Mg(N(SiMe 3 ) 2 ) 2 、Mg(2,2,6,6-テトラメチルピペリジド) 2 、Mn(N(SiBuMe 2 ) 2 ) 2 、Mn(N(SiMe 3 ) 2 ) 2 、Mn(N(SiMe 3 ) 2 ) 3 、Mo(N t BuSiMe 3 ) 3 、Mo 2 (NEt 2 ) 6 、Mo 2 (NMe 2 ) 6 、Mo(NEt 2 ) 4 、Mo(NMe 2 ) 4 、NaN(Si n BuMe 2 ) 2 、NaN(SiMe 3 ) 2 、Nb(N(SiMe 3 ) 2 ) 3 、Nb(NEt 2 ) 4 、Nb(NEt 2 ) 5 、Nb(NMe 2 ) 5 、Nd(N(SiMe 3 ) 2 ) 3 、Nd(N i Pr 2 ) 3 、Ni(N(SiMe 3 ) 2 ) 2 、Pb(N(SiMe 3 ) 2 ) 2 、Pb(N t BuSiMe 3 ) 2 、Pr(N(SiMe 3 ) 2 ) 3 、Sb(NMe 2 ) 3 、Sb(N(Me)(SiMe 3 )) 3 、Sc(N(SiMe 3 ) 2 ) 3 、SiH 2 (NMe 2 ) 2 、SiH(NMe 2 ) 3 、Si(NMe 2 ) 4 、Si(NHMe) 4 、Si(NHn-Pr) 4 、Si(NEt 2 ) 4 、Si(NCO) 4 、Sm(N(SiMe 3 ) 2 ) 3 、Sn(N(SiMe 3 ) 2 ) 2 、Sn(NEt 2 ) 4 、Sn(NMe 2 ) 4 、Sn(N t Bu 2 ) 2 、Sn(N t Bu 2 ) 3 、Sn(N t BuSiMe 3 ) 2 、Sn(N t BuSiMe 3 ) 3 、Sn(2,2,6,6-テトラメチルピペリジド) 2 , Sr(N(SiMe 3 ) 2 ) 2 、Ta(NEt 2 ) 4 、Ta(NMe 2 ) 5 、Ta(N t Bu)(NEt 2 ) 3 、Ta(NEt)(NEt 2 ) 3 、Tb(N(SiMe 3 ) 2 ) 3 、Th(NEt 2 ) 4 、Th(NPr 2 ) 4 、Ti(N(SiMe 3 ) 2 ) 3 、Ti(NEt 2 ) 4 、Ti(N i Pr 2 ) 3 、Ti(N i Pr 2 ) 4 、Ti(NMe 2 ) 4 、T1(N(SiMe 3 ) 2 ) 3 、U(N(SiMe 3 ) 2 ) 3 、U(NEt 2 ) 4 、U(NPr 2 ) 4 、V(N(SiMe 3 ) 2 ) 3 、V(NEt 2 ) 4 、V(NMe 2 ) 4 、V(O)(NMe 2 ) 3 、W 2 (NEt 2 ) 6 、W 2 (NMeEt) 6 、W 2 (NMe 2 ) 6 、W(N t Bu) 2 (NH t Bu) 2 、W(N t Bu) 2 (NEtMe) 2 、W(N t Bu) 2 (NMe 2 ) 2 、Y(N(SiMe 3 ) 2 ) 3 、Y(N i Pr 2 ) 3 、Y(N t BuSiMe 3 ) 3 、Y(2,2,6,6-テトラメチルピペリジド) 3 、Yb(N(SiMe 3 ) 2 ) 3 、Yb(N i Pr 2 ) 3 、Zn(N(SiMe 3 ) 2 ) 2 、Zn(N t Bu 2 ) 2 、Zn(2,2,6,6-テトラメチルピペリジド) 2 , Zr(NEt 2 ) 4 、Zr(NEtMe) 4 、Zr(N i Pr 2 ) 4 、及びZr(NMe 2 ) 4 、から選択される、請求項18に記載の方法。
- 金属化合物が次の化合物、すなわち、AlMe 3 、Ba(n-PrMe 4 Cp) 2 、Ba( i Pr 4 Cp) 2 、Ba(Me 5 Cp) 2 、BeEt 2 、BiMe 3 、Ca( i Pr 4 Cp) 2 、Ca(Me 5 Cp) 2 、CdMe 2 、CeCp 3 、Ce( i PrCp) 3 、Ce(Me 4 Cp) 3 、CoCp 2 、CoCp(CO) 2 、Co(CO) 3 NO、CrCp 2 、Cr(Me 5 Cp) 2 、Cr( i PrCp) 2 、Cr(EtBz) 2 、CuCpPEt 3 、Er(Cp) 3 、Er( i PrCp) 3 、Er(BuCp) 3 、Eu(Me 4 Cp) 3 、FeCp(Me 2 NCH 2 Cp)、FeCp( l BuCp)、GaMe 3 、GdCp 3 、Gd( i PrCp) 3 、InCp 3 、In(Me 5 Cp) 3 、InMe 3 、Ir(MeCp)(l,5-COD)、La( 1 PrCp) 3 、LaCp 3 、LaCp 3 (NCCH 3 ) 2 、La(Me 2 NC 2 H 4 Cp) 3 、Mg(PrCp) 2 、Mg(EtCp) 2 、MgCp 2 、MnCp 2 、Mn(EtCp) 2 、Mn(Me 5 Cp) 2 、Mo(EtBz) 2 、NdCp 3 、Nd( i PrCp) 3 、Ni(PF 3 ) 4 、PrCp 3 、Pr( i PrCp) 3 、SbEt 3 、ScCp 3 、SmCp 3 、Sm( i PrCp) 3 、Sr( i Pr 4 Cp) 2 、Sr(Me 5 Cp) 2 、TmCp 3 、Tm( i PrCp) 3 、TICp、VCp 2 、V(EtCp) 2 、W( 1 PrCp) 2 H 2 、YCp 3 、Y(MeCp) 3 、Y( n PrCp) 3 、Y(BuCp) 3 、YbCp 3 、Yb( i PrCp) 3 、ZnEt 2 、ZnMe 2 、ZrCp 2 Me 2 、及びZr( t BuCp) 2 Me 2 (これらの式中、Cpはシクロペンタジエニドの略号であり、Me 5 Cpはペンタメチルシクロペンタジエニドを表わし、 i PrCpはイソプロピルシクロペンタジエニドを表わし、 i PrMe 4 Cpはイソプロピルテトラメチルシクロペンタジエニドの略であり、 i Pr 4 Cpはテトライソプロピルシクロペンタジエニドの略であり、EtCpはエチルシクロペンタジエニドの略であり、PrCpはプロピルシクロペンタジエニドの略であり、 i PrCpはイソプロピルシクロペンタジエニドの略であり、BuCpはブチルシクロペンタジエニドの略であり、Bzはベンゼニド、EtBzはエチルベンゼニドの異性体の混合物、1,5−CODは1,5−シクロオクタジエニドの略である)、から選択される、請求項12または13に記載の方法。
- 金属化合物が次の化合物、すなわち、Al 2 Et 3 (O-sec-Bu) 3 、B(OMe) 3 、Hf(O t Bu) 4 、Nb(OEt) 5 、Ta(OEt) 5 、Ti(O i Pr) 4 、Y(OCMe 2 CH 2 NMe 2 ) 3 、及びZr(O t Bu) 4 、から選択される、請求項13又は14に記載の方法。
- 酸素を含む材料を形成するための方法であって、
1種以上のアレーン水和物の蒸気及び1種以上の金属化合物の蒸気に対して基板を露出させて金属酸化物を形成すること、
を含む材料形成方法。
- アレーン水和物が、ベンゼン水和物、ナフタレン水和物、置換されたベンゼン水和物又は置換されたナフタレン水和物である、請求項22に記載の方法。
- 金属酸化物を形成するための方法であって、
ジアルキルアミド、ジシリルアミド及び(アルキル)(シリル)アミド部分からなる群から選ばれるアミド基を有する1種以上の金属アミドの蒸気に対し、そして次に水又はアルコールの蒸気に対して交互に加熱表面を露出させること、
を含む金属酸化物形成方法。
- アルコールがアレーン水和物である、請求項24に記載の方法。
- 単数又は複数種の金属アミドが次の化合物、すなわち、Al(N(SiMe 3 ) 2 ) 3 、Al 2 (NEt 2 ) 6 、Al 2 (NEtMe) 6 、Al(N i Pr 2 ) 3 、Al 2 (NMe 2 ) 6 、Al(N(Et)CH 2 CH 2 NMe 2 )(NMe 2 ) 2 、As(NMe 2 ) 3 、As(N(Me)(SiMe 3 )) 3 、B(NMe 2 ) 3 、B(NEt 2 ) 3 、Ba(N(SiMe 3 ) 2 ) 2 、Be(NMe 2 ) 2 、Be(N(SiMe 3 ) 2 ) 2 、Be(2,2,6,6-テトラメチルピペリジド) 2 、Bi(N(SiMe 3 ) 2 ) 3 、Bi(N(Me)(SiMe 3 )) 3 、Ca(N(SiMe 3 ) 2 ) 2 、Cd(N(SiMe 3 ) 2 ) 2 、Cd(N t BuSiMe 3 ) 2 、Cd(2,2,6,6-テトラメチルピペリジド) 2 、Ce(N(SiMe 3 ) 2 ) 3 、Ce(N i Pr 2 ) 3 、Co(N(SiBuMe 2 ) 2 ) 2 、Co(N(SiEtMe 2 ) 2 ) 2 、Co(N(SiMe 3 ) 2 ) 2 、Co(N(SiMe 3 ) 2 ) 3 、Co(N(SiPrMe 2 ) 2 ) 2 、Cr(N(SiMe 3 ) 2 ) 3 、Cr(NEt 2 ) 4 、Cr(N i Pr 2 ) 3 、Cr(NMe 2 ) 4 、Cu 4 (N(SiMe 3 ) 2 ) 4 、Er(N(SiMe 3 ) 2 ) 3 、Eu(N(SiMe 3 ) 2 ) 3 、Fe(N(SiBuMe 2 ) 2 ) 2 、Fe(N(SiMe 3 ) 2 ) 2 、Fe(N(SiMe 3 ) 2 ) 3 、Ga(NMe 2 ) 3 、Ga(NEt 2 ) 3 、Ga(N(SiMe 3 ) 2 ) 3 、Ga(N t BuSiMe 3 ) 3 、Ga(2,2,6,6-テトラメチルピペリジド) 3 、Ga(N(Me)CH 2 CH 2 NMe 2 )(NMe 2 ) 2 、Gd(N(SiMe 3 ) 2 ) 3 、Ge(N(SiMe 3 ) 2 ) 2 、Ge(NEt 2 ) 4 、Ge(NMe 2 ) 4 、Ge(N t Bu 2 ) 2 、Ge(N t BuSiMe 3 ) 2 、Ge(2,2,6,6-テトラメチルピペリジド) 2 、Hf(NEt 2 ) 4 、Hf(NEtMe) 4 、Hf(NMe 2 ) 4 、Hg(N(SiMe 3 ) 2 ) 2 、Ho(N(SiMe 3 ) 2 ) 3 、In(N(SiMe 3 ) 2 ) 3 、In(2,2,6,6-テトラメチルピペリジド) 3 、KN(SiHexMe 2 ) 2 、KN(SiMe 3 ) 2 、La(N(SiMe 3 ) 2 ) 3 、La(N t BuSiMe 3 ) 3 、La(N i Pr 2 ) 3 、La(2,2,6,6-テトラメチルピペリジド) 3 、LiN(SiEtMe 2 ) 2 、LiN(SiMe 3 ) 2 、Li(2,2,6,6-テトラメチルピペリジド)、Lu(N(SiMe 3 ) 2 ) 3 、Mg(N(SiMe 3 ) 2 ) 2 、Mg(2,2,6,6-テトラメチルピペリジド) 2 、Mn(N(SiBuMe 2 ) 2 ) 2 、Mn(N(SiMe 3 ) 2 ) 2 、Mn(N(SiMe 3 ) 2 ) 3 、Mo(N t BuSiMe 3 ) 3 、Mo 2 (NEt 2 ) 6 、Mo 2 (NMe 2 ) 6 、Mo(NEt 2 ) 4 、Mo(NMe 2 ) 4 、NaN(Si n BuMe 2 ) 2 、NaN(SiMe 3 ) 2 、Nb(N(SiMe 3 ) 2 ) 3 、Nb(NEt 2 ) 4 、Nb(NEt 2 ) 5 、Nb(NMe 2 ) 5 、Nd(N(SiMe 3 ) 2 ) 3 、Nd(N i Pr 2 ) 3 、Ni(N(SiMe 3 ) 2 ) 2 、Pb(N(SiMe 3 ) 2 ) 2 、Pb(N t BuSiMe 3 ) 2 、Pr(N(SiMe 3 ) 2 ) 3 、Sb(NMe 2 ) 3 、Sb(N(Me)(SiMe 3 )) 3 、Sc(N(SiMe 3 ) 2 ) 3 、SiH 2 (NMe 2 ) 2 、SiH(NMe 2 ) 3 、Si(NMe 2 ) 4 、Si(NHMe) 4 、Si(NHn-Pr) 4 、Si(NEt 2 ) 4 、Si(NCO) 4 、Sm(N(SiMe 3 ) 2 ) 3 、Sn(N(SiMe 3 ) 2 ) 2 、Sn(NEt 2 ) 4 、Sn(NMe 2 ) 4 、Sn(N t Bu 2 ) 2 、Sn(N t Bu 2 ) 3 、Sn(N t BuSiMe 3 ) 2 、Sn(N t BuSiMe 3 ) 3 、Sn(2,2,6,6-テトラメチルピペリジド) 2 , Sr(N(SiMe 3 ) 2 ) 2 、Ta(NEt 2 ) 4 、Ta(NMe 2 ) 5 、Ta(N t Bu)(NEt 2 ) 3 、Ta(NEt)(NEt 2 ) 3 、Tb(N(SiMe 3 ) 2 ) 3 、Th(NEt 2 ) 4 、Th(NPr 2 ) 4 、Ti(N(SiMe 3 ) 2 ) 3 、Ti(NEt 2 ) 4 、Ti(N i Pr 2 ) 3 、Ti(N i Pr 2 ) 4 、Ti(NMe 2 ) 4 、T1(N(SiMe 3 ) 2 ) 3 、U(N(SiMe 3 ) 2 ) 3 、U(NEt 2 ) 4 、U(NPr 2 ) 4 、V(N(SiMe 3 ) 2 ) 3 、V(NEt 2 ) 4 、V(NMe 2 ) 4 、V(O)(NMe 2 ) 3 、W 2 (NEt 2 ) 6 、W 2 (NMeEt) 6 、W 2 (NMe 2 ) 6 、W(N t Bu) 2 (NH t Bu) 2 、W(N t Bu) 2 (NEtMe) 2 、W(N t Bu) 2 (NMe 2 ) 2 、Y(N(SiMe 3 ) 2 ) 3 、Y(N i Pr 2 ) 3 、Y(N t BuSiMe 3 ) 3 、Y(2,2,6,6-テトラメチルピペリジド) 3 、Yb(N(SiMe 3 ) 2 ) 3 、Yb(N i Pr 2 ) 3 、Zn(N(SiMe 3 ) 2 ) 2 、Zn(N t Bu 2 ) 2 、Zn(2,2,6,6-テトラメチルピペリジド) 2 , Zr(NEt 2 ) 4 、Zr(NEtMe) 4 、Zr(N i Pr 2 ) 4 、及びZr(NMe 2 ) 4 、から選ばれる、請求項24に記載の方法。
- 酸素及び1種以上の金属を含む材料を形成するための方法であって、
1種以上の有機金属化合物の蒸気に対し、そして次にアレーン水和物の蒸気に対して交互に表面を露出させること、
を含む材料形成方法。
- 有機金属化合物が次の化合物、すなわち、AlMe 3 、Ba(n-PrMe 4 Cp) 2 、Ba( i Pr 4 Cp) 2 、Ba(Me 5 Cp) 2 、BeEt 2 、BiMe 3 、Ca( i Pr 4 Cp) 2 、Ca(Me 5 Cp) 2 、CdMe 2 、CeCp 3 、Ce( i PrCp) 3 、Ce(Me 4 Cp) 3 、CoCp 2 、CoCp(CO) 2 、Co(CO) 3 NO、CrCp 2 、Cr(Me 5 Cp) 2 、Cr( i PrCp) 2 、Cr(EtBz) 2 、CuCpPEt 3 、Er(Cp) 3 、Er( i PrCp) 3 、Er(BuCp) 3 、Eu(Me 4 Cp) 3 、FeCp(Me 2 NCH 2 Cp)、FeCp( l BuCp)、GaMe 3 、GdCp 3 、Gd( i PrCp) 3 、InCp 3 、In(Me 5 Cp) 3 、InMe 3 、Ir(MeCp)(l,5-COD)、La( 1 PrCp) 3 、LaCp 3 、LaCp 3 (NCCH 3 ) 2 、La(Me 2 NC 2 H 4 Cp) 3 、Mg(PrCp) 2 、Mg(EtCp) 2 、MgCp 2 、MnCp 2 、Mn(EtCp) 2 、Mn(Me 5 Cp) 2 、Mo(EtBz) 2 、NdCp 3 、Nd( i PrCp) 3 、Ni(PF 3 ) 4 、PrCp 3 、Pr( i PrCp) 3 、SbEt 3 、ScCp 3 、SmCp 3 、Sm( i PrCp) 3 、Sr( i Pr 4 Cp) 2 、Sr(Me 5 Cp) 2 、TmCp 3 、Tm( i PrCp) 3 、TICp、VCp 2 、V(EtCp) 2 、W( 1 PrCp) 2 H 2 、YCp 3 、Y(MeCp) 3 、Y( n PrCp) 3 、Y(BuCp) 3 、YbCp 3 、Yb( i PrCp) 3 、ZnEt 2 、ZnMe 2 、ZrCp 2 Me 2 、及びZr( t BuCp) 2 Me 2 (これらの式中、Cpはシクロペンタジエニドの略号であり、Me 5 Cpはペンタメチルシクロペンタジエニドを表わし、 i PrCpはイソプロピルシクロペンタジエニドを表わし、 i PrMe 4 Cpはイソプロピルテトラメチルシクロペンタジエニドの略であり、 i Pr 4 Cpはテトライソプロピルシクロペンタジエニドの略であり、EtCpはエチルシクロペンタジエニドの略であり、PrCpはプロピルシクロペンタジエニドの略であり、 i PrCpはイソプロピルシクロペンタジエニドの略であり、BuCpはブチルシクロペンタジエニドの略であり、Bzはベンゼニド、EtBzはエチルベンゼニドの異性体の混合物、1,5−CODは1,5−シクロオクタジエニドの略である)、から選ばれる、請求項27に記載の方法。
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US20130122328A1 (en) | 2013-05-16 |
US9905414B2 (en) | 2018-02-27 |
US20160087066A1 (en) | 2016-03-24 |
KR20030038775A (ko) | 2003-05-16 |
KR100815009B1 (ko) | 2008-03-18 |
WO2002027063A2 (en) | 2002-04-04 |
EP1772534A3 (en) | 2007-04-25 |
US20160111276A1 (en) | 2016-04-21 |
JP2004527651A (ja) | 2004-09-09 |
US20160268121A1 (en) | 2016-09-15 |
US6969539B2 (en) | 2005-11-29 |
JP2009079297A (ja) | 2009-04-16 |
KR20070107813A (ko) | 2007-11-07 |
JP5175157B2 (ja) | 2013-04-03 |
WO2002027063A3 (en) | 2002-10-10 |
EP1327010A2 (en) | 2003-07-16 |
US8334016B2 (en) | 2012-12-18 |
US20120028478A1 (en) | 2012-02-02 |
US20040043149A1 (en) | 2004-03-04 |
KR100814980B1 (ko) | 2008-03-18 |
US20050277780A1 (en) | 2005-12-15 |
US20150118395A1 (en) | 2015-04-30 |
US7507848B2 (en) | 2009-03-24 |
EP1772534A2 (en) | 2007-04-11 |
EP1327010B1 (en) | 2013-12-04 |
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