CN1914150A - 烷氧基金属化合物、薄膜形成用原料和薄膜的制造方法 - Google Patents
烷氧基金属化合物、薄膜形成用原料和薄膜的制造方法 Download PDFInfo
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- CN1914150A CN1914150A CNA2005800040188A CN200580004018A CN1914150A CN 1914150 A CN1914150 A CN 1914150A CN A2005800040188 A CNA2005800040188 A CN A2005800040188A CN 200580004018 A CN200580004018 A CN 200580004018A CN 1914150 A CN1914150 A CN 1914150A
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- Prior art keywords
- compound
- film
- alkoxide compound
- thin film
- alkyl
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- -1 Alkoxide compound Chemical class 0.000 title claims abstract description 120
- 238000000034 method Methods 0.000 title claims abstract description 60
- 239000002994 raw material Substances 0.000 title claims abstract description 35
- 239000010409 thin film Substances 0.000 title abstract description 11
- 230000015572 biosynthetic process Effects 0.000 title abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 30
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical group [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims abstract description 29
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 10
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 9
- 125000004432 carbon atom Chemical group C* 0.000 claims description 42
- 125000000217 alkyl group Chemical group 0.000 claims description 34
- 238000004519 manufacturing process Methods 0.000 claims description 34
- 239000000463 material Substances 0.000 claims description 12
- 238000002309 gasification Methods 0.000 claims description 11
- 125000001118 alkylidene group Chemical group 0.000 claims description 8
- HZVOZRGWRWCICA-UHFFFAOYSA-N methanediyl Chemical compound [CH2] HZVOZRGWRWCICA-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 abstract description 68
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 25
- 229910052710 silicon Inorganic materials 0.000 abstract description 25
- 239000010703 silicon Substances 0.000 abstract description 25
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 abstract 3
- 230000008020 evaporation Effects 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- 230000008016 vaporization Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 58
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 33
- 229910052719 titanium Inorganic materials 0.000 description 33
- 239000010936 titanium Substances 0.000 description 33
- 239000002243 precursor Substances 0.000 description 32
- 239000007789 gas Substances 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 26
- 239000000203 mixture Substances 0.000 description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 22
- 239000000126 substance Substances 0.000 description 22
- 239000007788 liquid Substances 0.000 description 21
- 238000002156 mixing Methods 0.000 description 20
- 239000002585 base Substances 0.000 description 18
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 238000011156 evaluation Methods 0.000 description 15
- 239000002904 solvent Substances 0.000 description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- 229910052760 oxygen Inorganic materials 0.000 description 13
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 12
- 239000011734 sodium Substances 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 229910052786 argon Inorganic materials 0.000 description 11
- 239000002131 composite material Substances 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 11
- UXFQFBNBSPQBJW-UHFFFAOYSA-N 2-amino-2-methylpropane-1,3-diol Chemical compound OCC(N)(C)CO UXFQFBNBSPQBJW-UHFFFAOYSA-N 0.000 description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 10
- IIEWJVIFRVWJOD-UHFFFAOYSA-N ethylcyclohexane Chemical compound CCC1CCCCC1 IIEWJVIFRVWJOD-UHFFFAOYSA-N 0.000 description 10
- 229910052708 sodium Inorganic materials 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 9
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 8
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 8
- 238000004821 distillation Methods 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- 229910052726 zirconium Inorganic materials 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 7
- 150000001414 amino alcohols Chemical class 0.000 description 7
- 238000000231 atomic layer deposition Methods 0.000 description 7
- 238000009835 boiling Methods 0.000 description 7
- 229940125904 compound 1 Drugs 0.000 description 7
- 229940125782 compound 2 Drugs 0.000 description 7
- 238000000151 deposition Methods 0.000 description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 7
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 6
- SJRJJKPEHAURKC-UHFFFAOYSA-N N-Methylmorpholine Chemical compound CN1CCOCC1 SJRJJKPEHAURKC-UHFFFAOYSA-N 0.000 description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 6
- 125000003545 alkoxy group Chemical group 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 6
- 239000006200 vaporizer Substances 0.000 description 6
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 5
- 150000001298 alcohols Chemical class 0.000 description 5
- 229910052797 bismuth Inorganic materials 0.000 description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 5
- 239000012159 carrier gas Substances 0.000 description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 5
- 125000005843 halogen group Chemical group 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- PAMIQIKDUOTOBW-UHFFFAOYSA-N 1-methylpiperidine Chemical compound CN1CCCCC1 PAMIQIKDUOTOBW-UHFFFAOYSA-N 0.000 description 4
- AFABGHUZZDYHJO-UHFFFAOYSA-N 2-Methylpentane Chemical compound CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 description 4
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 4
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 4
- CEPICIBPGDWCRU-UHFFFAOYSA-N [Si].[Hf] Chemical compound [Si].[Hf] CEPICIBPGDWCRU-UHFFFAOYSA-N 0.000 description 4
- 125000003368 amide group Chemical group 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 229940126214 compound 3 Drugs 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000005194 fractionation Methods 0.000 description 4
- TXGJTWACJNYNOJ-UHFFFAOYSA-N hexane-2,4-diol Chemical compound CCC(O)CC(C)O TXGJTWACJNYNOJ-UHFFFAOYSA-N 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- 239000012808 vapor phase Substances 0.000 description 4
- 239000003039 volatile agent Substances 0.000 description 4
- 238000005160 1H NMR spectroscopy Methods 0.000 description 3
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 3
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000000137 annealing Methods 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 238000009530 blood pressure measurement Methods 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000002716 delivery method Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 description 3
- 125000005594 diketone group Chemical group 0.000 description 3
- 150000002170 ethers Chemical class 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 3
- 229910017053 inorganic salt Inorganic materials 0.000 description 3
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 description 3
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 3
- 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 3
- 125000004115 pentoxy group Chemical group [*]OC([H])([H])C([H])([H])C([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 3
- 229920000768 polyamine Polymers 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N propylene glycol Substances CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 3
- 239000012048 reactive intermediate Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 150000003527 tetrahydropyrans Chemical class 0.000 description 3
- 238000000427 thin-film deposition Methods 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- QEGNUYASOUJEHD-UHFFFAOYSA-N 1,1-dimethylcyclohexane Chemical compound CC1(C)CCCCC1 QEGNUYASOUJEHD-UHFFFAOYSA-N 0.000 description 2
- 229940058015 1,3-butylene glycol Drugs 0.000 description 2
- QBPPRVHXOZRESW-UHFFFAOYSA-N 1,4,7,10-tetraazacyclododecane Chemical compound C1CNCCNCCNCCN1 QBPPRVHXOZRESW-UHFFFAOYSA-N 0.000 description 2
- MDAXKAUIABOHTD-UHFFFAOYSA-N 1,4,8,11-tetraazacyclotetradecane Chemical compound C1CNCCNCCCNCCNC1 MDAXKAUIABOHTD-UHFFFAOYSA-N 0.000 description 2
- AKPLTHZVVWBOPT-UHFFFAOYSA-N 2,2-diethylbutane-1,3-diol Chemical compound CCC(CC)(CO)C(C)O AKPLTHZVVWBOPT-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
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 2
- 125000004200 2-methoxyethyl group Chemical group [H]C([H])([H])OC([H])([H])C([H])([H])* 0.000 description 2
- AIDLAEPHWROGFI-UHFFFAOYSA-N 2-methylbenzene-1,3-dicarboxylic acid Chemical compound CC1=C(C(O)=O)C=CC=C1C(O)=O AIDLAEPHWROGFI-UHFFFAOYSA-N 0.000 description 2
- MSXVEPNJUHWQHW-UHFFFAOYSA-N 2-methylbutan-2-ol Chemical compound CCC(C)(C)O MSXVEPNJUHWQHW-UHFFFAOYSA-N 0.000 description 2
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- KDSNLYIMUZNERS-UHFFFAOYSA-N 2-methylpropanamine Chemical compound CC(C)CN KDSNLYIMUZNERS-UHFFFAOYSA-N 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 2
- 229910052688 Gadolinium Inorganic materials 0.000 description 2
- 241000588731 Hafnia Species 0.000 description 2
- 229910052689 Holmium Inorganic materials 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- WRQNANDWMGAFTP-UHFFFAOYSA-N Methylacetoacetic acid Chemical compound COC(=O)CC(C)=O WRQNANDWMGAFTP-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- ZCQWOFVYLHDMMC-UHFFFAOYSA-N Oxazole Chemical compound C1=COC=N1 ZCQWOFVYLHDMMC-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 229910052777 Praseodymium Inorganic materials 0.000 description 2
- 229910052773 Promethium Inorganic materials 0.000 description 2
- RWRDLPDLKQPQOW-UHFFFAOYSA-N Pyrrolidine Chemical compound C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 229910052772 Samarium Inorganic materials 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 241000534944 Thia Species 0.000 description 2
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-UHFFFAOYSA-N 0.000 description 2
- 229910052775 Thulium Inorganic materials 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- GTZOZDOTOWNSJH-UHFFFAOYSA-N [O].CCCCCCC Chemical compound [O].CCCCCCC GTZOZDOTOWNSJH-UHFFFAOYSA-N 0.000 description 2
- ZBGXSVQAJGTDDB-UHFFFAOYSA-N [Y].[Hf] Chemical compound [Y].[Hf] ZBGXSVQAJGTDDB-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 150000001622 bismuth compounds Chemical class 0.000 description 2
- 235000019437 butane-1,3-diol Nutrition 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 2
- 125000004093 cyano group Chemical group *C#N 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- YSSSPARMOAYJTE-UHFFFAOYSA-N dibenzo-18-crown-6 Chemical compound O1CCOCCOC2=CC=CC=C2OCCOCCOC2=CC=CC=C21 YSSSPARMOAYJTE-UHFFFAOYSA-N 0.000 description 2
- 238000004455 differential thermal analysis Methods 0.000 description 2
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 2
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 2
- 150000002363 hafnium compounds Chemical class 0.000 description 2
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- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- OGHBATFHNDZKSO-UHFFFAOYSA-N propan-2-olate Chemical compound CC(C)[O-] OGHBATFHNDZKSO-UHFFFAOYSA-N 0.000 description 1
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- ODZPKZBBUMBTMG-UHFFFAOYSA-N sodium amide Chemical compound [NH2-].[Na+] ODZPKZBBUMBTMG-UHFFFAOYSA-N 0.000 description 1
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- 239000012312 sodium hydride Substances 0.000 description 1
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- 238000010189 synthetic method Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
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- 229910052718 tin Inorganic materials 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- AYDYYQHYLJDCDQ-UHFFFAOYSA-N trimethylbismuthane Chemical compound C[Bi](C)C AYDYYQHYLJDCDQ-UHFFFAOYSA-N 0.000 description 1
- ZHXAZZQXWJJBHA-UHFFFAOYSA-N triphenylbismuthane Chemical compound C1=CC=CC=C1[Bi](C=1C=CC=CC=1)C1=CC=CC=C1 ZHXAZZQXWJJBHA-UHFFFAOYSA-N 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
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
Images
Classifications
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- C07C215/00—Compounds containing amino and hydroxy groups bound to the same carbon skeleton
- C07C215/02—Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton
- C07C215/04—Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being saturated
- C07C215/06—Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being saturated and acyclic
- C07C215/08—Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being saturated and acyclic with only one hydroxy group and one amino group bound to the carbon skeleton
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- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/04—Esters of silicic acids
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
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Abstract
本发明的烷氧基金属化合物以下述通式(1)表示,其适用于例如CVD法等的使化合物气化而形成薄膜的方法中所使用的薄膜形成用原料。此外,本发明的薄膜形成用原料含有该烷氧基金属化合物,本发明的薄膜的制造方法是将含有使该薄膜形成用原料气化而得到的烷氧基金属化合物的蒸汽引入到基材上,使蒸汽分解和/或进行化学反应而在基材上形成薄膜,式中,R1和R2中的之一表示碳原子数为1~4的烷基,另一个表示氢原子或者碳原子数为1~4的烷基,R3和R4表示碳原子数为1~4的烷基,A表示碳原子数为1~8的亚烷基,M表示硅原子或者铪原子,n表示4。
Description
技术领域
本发明涉及以特定的氨基醇为配位基的新型烷氧基金属化合物(烷氧基硅化合物、烷氧基铪化合物)、含有该烷氧基金属化合物的薄膜形成用原料、以及使用该薄膜形成用原料的含有硅和/或铪的薄膜的制造方法。
背景技术
含有硅或铪的薄膜主要用作高电介电容器、强电介电容器、栅绝缘膜、阻挡膜等电子元件的部件。
作为上述薄膜的制造法,可以列举出出火焰沉积(flame hydrolysisdeposition)法、溅射法、离子镀覆法、涂布热解法和溶胶凝胶法等MOD法和化学气相生长(以下有时也仅记载为CVD)法等,而由于在组成控制性和阶梯覆盖(step coverage)性方面优良、适于大批量生产以及能够混合集成等许多优点,因此包括ALD(Atomic Layer Deposition)法在内的化学气相生长法是最优选的制造方法。
在MOD法和CVD法中,作为将硅或金属供给到薄膜的前体,可以使用利用了有机配位基的化合物。作为有机配位基,报道了施予比较大的蒸气压,适于利用CVD的薄膜制造的在末端具有醚基或者二烷基氨基的醇。对于硅,专利文献1中报道了把末端具有烷氧基的醇作为配位基的硅的烷氧基化合物。另外,关于在末端具有与金属原子配位的供体基即氨基的醇用作配位基的金属化合物,在专利文献2和专利文献3中报道了钛化合物和锆化合物,在非专利文献1中报道了稀土元素化合物。
对于硅和铪,专利文献4中报道了以一级的氨基醇为配位基的烷氧基化合物。
专利文献1:特开平6-321824号公报
专利文献2:特开2000-351784号公报
专利文献3:特开2003-119171号公报
专利文献4:韩国公开专利2003-74986号公报
非专利文献1:Inorganic Chemistry,Vol.36,No.16,1997,第3545-3552页
发明内容
适用于例如CVD法等的使化合物气化而形成薄膜的方法中所使用的原料的化合物(前体)所要求的性质是,熔点低并可以在液体的状态下进行输送,蒸气压大且易于气化。另外,在制造多成分体系的薄膜时,要求在混合时或者保存时不因配位基交换反应或化学反应而变质,并要求由热和/或氧化产生的薄膜沉积时的分解行为类似。对于硅和铪,就这些观点而言,它们是不能令人十分满意的化合物。
本发明者等经过反复研究,结果发现将特定的氨基醇用作配位基而得到的烷氧基金属化合物可以解决上述问题,从而实现了本发明。
即,本发明提供了以下述通式(1)表示的烷氧基金属化合物(alkoxide compound)、含有该烷氧基金属化合物的薄膜形成用原料、以及将含有使该薄膜形成用原料气化而得到的烷氧基金属化合物的蒸汽引入到基材上,使蒸汽分解和/或进行化学反应而在基材上形成含有硅和/或铪的薄膜的薄膜制造方法。
[化学式1]
(式中,R1和R2中的之一表示碳原子数为1~4的烷基,另一个表示氢原子或者碳原子数为1~4的烷基,R3和R4表示碳原子数为1~4的烷基,A表示碳原子数为1~8的亚烷基(alkanediyl),M表示硅原子或者铪原子,n表示4。)
附图说明
图1是表示在本发明的薄膜制造方法中使用的CVD装置的一个例子的示意图。
具体实施方式
本发明的烷氧基金属化合物是以上述通式(1)表示的化合物,其特别适合作为例如CVD法或ALD法等具有气化工序的薄膜制造方法的前体。
在上述通式(1)中,M为硅原子的烷氧基硅化合物如果与众所周知的烷氧基硅化合物进行比较,则由热和/或氧产生的分解性大,对化学反应的稳定性大。此外,比类似结构的以一级的氨基醇为配位基的烷氧基金属化合物的蒸气压还大。因此,单独使用时,在薄膜制造中在能量方面处于优势,另外,与其它的前体并用时,由于易于配合分解行为,因而在控制薄膜的组成的方面处于优势。此外,在可以混合使用等操作方面也处于优势。
在上述通式(1)中,M为铪原子的烷氧基铪化合物如果与众所周知的烷氧基铪化合物进行比较,则由热和/或氧产生的分解性相同或良好,对化学反应的稳定性大。此外,比类似结构的以一级的氨基醇为配位基的烷氧基金属化合物的蒸气压还大。因此,单独使用时,在薄膜制造中在能量方面处于优势,另外,与其它的前体并用时,由于易于配合分解行为,因而在控制薄膜组成的方面处于优势。此外,即使在可以混合使用等操作方面也处于优势。
在上述通式(1)中,作为以R1、R2、R3和R4表示的碳原子数为1~4的烷基,可以列举出甲基、乙基、丙基、异丙基、丁基、仲丁基、叔丁基、异丁基。另外,在上述通式(1)中以A表示的亚烷基只要是碳原子数的总数为1~8的基团,则可以是直链,也可以是在任意的位置上具有1个或多个支链。作为该亚烷基,当末端的供体基即二烷基氨基与硅原子或者铪原子配位时,优选在能量方面是稳定结构的给予五元环或者六元环结构的基团。作为优选的亚烷基,可以列举出用下述通式(11)表示的基团。另外,本发明的烷氧基金属化合物有时也具有光学异构体,但是不能通过其光学异构性进行区别。
[化学式2]
(式中,R5~R8表示氢原子或者碳原子数为1~4的烷基,x表示0或1,式中的碳原子数的总和为1~8。)
将配位基中的末端供体基与硅原子或者铪原子配位而形成环结构的情况以下述通式(111)表示。本发明的烷氧基金属化合物用上述通式(1)代表并表示,但是与用下述通式(111)所表示的化合物没有区别,而是包含两个通式的概念。
[化学式3]
(式中,R1和R2中的之一表示碳原子数为1~4的烷基,另一个表示氢原子或者碳原子数为1~4的烷基,R3和R4表示碳原子数为1~4的烷基,A表示碳原子数为1~8的亚烷基,M表示硅原子或者铪原子,n表示4。)
作为本发明烷氧基金属化合物的具体例子,可以列举出下述化合物No.1~No.22。
在具有使化合物气化工序的薄膜的制造方法中使用本发明的烷氧基金属化合物时,优选上述的R1~R4和A具有小分子量以提供大的蒸气压,具体地,R1~R2优选为氢原子或者甲基,R3~R4优选为甲基,A优选为亚甲基。另外,在用不带有气化工序的MOD法的薄膜的制造方法中,使用本发明的烷氧基金属化合物时,R1~R4和A可以根据相对于使用的溶剂的溶解性、薄膜形成反应等任意地选择。
本发明的烷氧基金属化合物的制造方法没有特别的限制,可以利用众所周知的反应进行制造。作为制造方法,可以利用使用该氨基醇的众所周知的普通的烷氧基金属化合物的合成方法,可以列举出例如使硅或者铪的卤化物、硝酸盐等无机盐或者其水合物和相应的醇化合物在钠、氢化钠、氨基钠、氢氧化钠、甲醇钠、氨、胺等碱的存在下进行反应的方法;使硅或者铪的卤化物、硝酸盐等无机盐或者其水合物和相应的醇化合物的烷氧基钠、烷氧基锂、烷氧基钾等碱金属烷氧化物进行反应的方法;使硅或者铪的甲氧化物、乙氧化物、异丙氧化物、丁氧化物等低分子醇的烷氧基金属化合物和相应的醇化合物进行交换反应的方法;使硅或者铪的卤化物、硝酸盐等无机盐与给予反应性中间体的衍生物进行反应,获得反应性中间体后,使其与相应的醇化合物进行反应的方法。
作为上述的反应性中间体,可以列举出四(二烷基氨基)硅、四(双(三甲基甲硅烷基)氨基)硅、四(二烷基氨基)铪、四(双(三甲基甲硅烷基)氨基)铪等硅或者铪的酰胺化合物。
本发明的薄膜形成用原料将本发明的烷氧基金属化合物作为薄膜的前体而含有,其形态根据使用该薄膜形成用原料的薄膜制造方法(例如,涂布热解法或溶胶凝胶法等的MOD法、包含ALD法的CVD法)的不同而不同。从烷氧基金属化合物的物性的观点出发,本发明的烷氧基金属化合物即使在薄膜形成用原料中也特别适合用作CVD用原料。
在本发明的薄膜形成用原料为化学气相生长(CVD)用原料时,其形态可以根据所使用的CVD法的输送供给方法等手段而适当地选择。
作为上述输送供给方法,其包括:在原料容器中将CVD用原料加热和/或减压使其气化,与根据需要使用的氩气、氮气和氦等载气一起导入沉积反应部的气体输送法;在液体或溶液状态下,将CVD用原料输送到气化室,通过在气化室中加热和/或减压使其气化,导入沉积反应部的液体输送法。在气体输送法的情况下,以上述通式(1)表示的烷氧基金属化合物本身作为CVD用原料,在液体输送法的情况下,以上述通式(1)表示的烷氧基金属化合物本身或者该化合物溶于有机溶剂后所形成的溶液作为CVD用原料。
另外,在多成分系统的CVD法中,包括:将CVD用原料各成分独立地气化、供给的方法(以下,也记载为单源法);以及预先将多成分原料以所希望的组成混合而形成的混合原料气化、供给的方法(以下,也记载为混合源法)。在混合源法的情况下,只以本发明的烷氧基金属化合物形成的混合物或者混合溶液、或者本发明的烷氧基金属化合物和其它前体的混合物或者混合溶液是CVD用原料。
作为上述CVD用原料中所使用的有机溶剂没有特别的限制,可以使用公知常见的有机溶剂。作为该有机溶剂,例如可以列举出甲醇、乙醇、2-丙醇、正丁醇等醇类,醋酸乙酯、醋酸丁酯、醋酸甲氧基乙酯等醋酸酯类,乙二醇单甲基醚、乙二醇单乙基醚、乙二醇单丁基醚、二甘醇单甲基醚等醚醇类,四氢呋喃、四氢吡喃、乙二醇二甲基醚、二甘醇二甲基醚、三甘醇二甲基醚、二丁基醚、二噁烷等醚类,甲基丁基酮、甲基异丁基酮、乙基丁基酮、二丙基酮、二异丁基酮、甲基戊基酮、环己酮、甲基环己酮等酮类,己烷、环己烷、甲基环己烷、二甲基环己烷、乙基环己烷、庚烷、辛烷、甲苯、二甲苯等烃类,1-氰基丙烷、1-氰基丁烷、1-氰基己烷、氰基环己烷、氰基苯、1,3-二氰基丙烷、1,4-二氰基丁烷、1,6-二氰基己烷、1,4-二氰基环己烷、1,4-二氰基苯等具有氰基的烃类,吡啶、二甲基吡啶,根据溶质的溶解性、使用温度与沸点、闪点的关系等,可以单独使用这些溶剂,或者作为两种或更多种的混合溶剂而使用。在使用这些有机溶剂时,该有机溶剂中的本发明的烷氧基金属化合物和其它前体的总量优选为0.01~2.0mol/L,特别优选为0.05~1.0mol/L。
另外,在为多成分体系的CVD法时,作为可以与本发明的烷氧基金属化合物一起使用的其它前体,没有特别的限制,可以使用CVD用原料中所使用的公知常见的前体。
作为上述其它前体,可以列举出选自醇化合物、二元醇化合物、β-二酮和环戊二烯化合物和有机胺化合物等用作有机配位基的化合物中的1种、2种或更多种和硅或金属形成的化合物。此外,作为前体的金属种,可以列举出镁、钙、锶、钡、钛、锆、铪、钒、铌、钽、锰、铁、钌、钴、铑、铱、镍、钯、铂、铜、银、金、锌、镓、铟、锗、锡、铅、锑、铋、钇、镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱。
作为上述用作有机配位基的醇化合物,可以列举出甲醇、乙醇、丙醇、异丙醇、丁醇、2-丁醇、异丁醇、叔丁醇、戊醇、异戊醇、叔戊醇等烷基醇类;2-甲氧基乙醇、2-乙氧基乙醇、2-丁氧基乙醇、2-(2-甲氧基乙氧基)乙醇、2-甲氧基-1-甲基乙醇、2-甲氧基-1,1-二甲基乙醇、2-乙氧基-1,1-二甲基乙醇、2-异丙氧基-1,1-二甲基乙醇、2-丁氧基-1,1-二甲基乙醇、2-(2-甲氧基乙氧基)-1,1-二甲基乙醇、2-丙氧基-1,1-二乙基乙醇、2-仲丁氧基-1,1-二乙基乙醇、3-甲氧基-1,1-二甲基丙醇等醚醇类;供给本发明的烷氧基金属化合物的二烷基氨基醇等。
作为上述用作有机配位基的二元醇化合物,可以列举出1,2-乙二醇、1,2-丙二醇、1,3-丙二醇、2,4-己二醇、2,2-二甲基-1,3-丙二醇、2,2-二乙基-1,3-丙二醇、1,3-丁二醇、2,4-丁二醇、2,2-二乙基-1,3-丁二醇、2-乙基-2-丁基-1,3-丙二醇、2,4-戊二醇、2-甲基-1,3-丙二醇、2-甲基-2,4-戊二醇、2,4-己二醇、2,4-二甲基-2,4-戊二醇等。
作为上述用作有机配位基的β-二酮化合物,可以列举出乙酰丙酮、己烷-2,4-二酮、5-甲基己烷-2,4-二酮、庚烷-2,4-二酮、2-甲基庚烷-3,5-二酮、5-甲基庚烷-2,4-二酮、6-甲基庚烷-2,4-二酮、2,2-二甲基庚烷-3,5-二酮、2,6-二甲基庚烷-3,5-二酮、2,2,6-三甲基庚烷-3,5-二酮、2,2,6,6-四甲基庚烷-3,5-二酮、辛烷-2,4-二酮、2,2,6-三甲基辛烷-3,5-二酮、2,6-二甲基辛烷-3,5-二酮、2,9-二甲基壬烷-4,6-二酮2-甲基-6-乙基癸烷-3,5-二酮、2,2-二甲基-6-乙基癸烷-3,5-二酮等烷基取代β-二酮类;1,1,1-三氟戊烷-2,4-二酮、1,1,1-三氟-5,5-二甲基己烷-2,4-二酮、1,1,1,5,5,5-六氟戊烷-2,4-二酮、1,3-二全氟己基丙烷-1,3-二酮等氟取代烷基β-二酮类;1,1,5,5-四甲基-1-甲氧基己烷-2,4-二酮、2,2,6,6-四甲基-1-甲氧基庚烷-3,5-二酮、2,2,6,6-四甲基-1-(2-甲氧基乙氧基)庚烷-3,5-二酮等醚取代β-二酮类等。
作为上述用作有机配位基的环戊二烯化合物,可以列举出环戊二烯、甲基环戊二烯、乙基环戊二烯、丙基环戊二烯、异丙基环戊二烯、丁基环戊二烯、仲丁基环戊二烯、异丁基环戊二烯、叔丁基环戊二烯、二甲基环戊二烯、四甲基环戊二烯等。另外,作为上述用作有机配位基的有机胺化合物,可以列举出甲胺、乙胺、丙胺、异丙胺、丁胺、仲丁胺、叔丁胺、异丁胺、二甲胺、二乙胺、二丙胺、二异丙胺、乙甲胺、丙甲胺、异丙基甲基胺等。
对于上述其它的前体,在单源法的情况下,优选热和/或氧化分解行为类似的化合物,在混合源法的情况下,优选除了热和/或氧化分解行为类似之外,混合时还不会因化学反应而引起变质的化合物。
作为钛或锆的前体,可以列举出例如与本发明烷氧基金属化合物具有相同配位基的四烷氧基钛和用下述[化学式6]中所示的通式表示的化合物。
[化学式6]
(式中,M1表示钛或者锆,Ra和Rb分别独立地表示可以被卤原子取代、也可以在链中含有氧原子的碳原子数为1~20的烷基,Rc表示碳原子数为1~8的烷基,Rd表示碳原子数为2~18的直链或支链的亚烷基,Re和Rf表示氢原子或者碳原子数为1~3的烷基,Rg表示碳原子数为1~4的烷基,p表示0~4的整数,q表示0或2,r表示0~3的整数。)
在上述[化学式6]所示的通式中,作为以Ra和Rb表示的可以被卤原子取代、也可以在链中含有氧原子的碳原子数1~20的烷基,可以列举出甲基、乙基、丙基、异丙基、丁基、仲丁基、叔丁基、异丁基、戊基、异戊基、仲戊基、叔戊基、己基、环己基、1-甲基环己基、庚基、3-庚基、异庚基、叔庚基、正辛基、异辛基、叔辛基、2-乙基己基、三氟甲基、全氟己基、2-甲氧基乙基、2-乙氧基乙基、2-丁氧基乙基、2-(2-甲氧基乙氧基)乙基、1-甲氧基-1,1-二甲基甲基、2-甲氧基-1,1-二甲基乙基、2-乙氧基-1,1-二甲基乙基、2-异丙氧基-1,1-二甲基乙基、2-丁氧基-1,1-二甲基乙基、2-(2-甲氧基乙氧基)-1,1-二甲基乙基。另外,作为以Rc表示的碳原子数为1~8的烷基,可以列举出甲基、乙基、丙基、异丙基、丁基、仲丁基、叔丁基、异丁基、戊基、异戊基、仲戊基、叔戊基、己基、1-乙基戊基、环己基、1-甲基环己基、庚基、异庚基、叔庚基、正辛基、异辛基、叔辛基、2-乙基己基。此外,作为Rd表示的碳原子数2~18的直链或支链的亚烷基,其是由二元醇衍生的基团,作为该二元醇,可以列举出1,2-乙二醇、1,2-丙二醇、1,3-丙二醇、1,3-丁二醇、2,4-己二醇、2,2-二甲基-1,3-丙二醇、2,2-二乙基-1,3-丙二醇、2,2-二乙基-1,3-丁二醇、2-乙基-2-丁基-1,3-丙二醇、2,4-戊二醇、2-甲基-1,3-丙二醇、1-甲基-2,4-戊二醇等。另外,作为以Re和Rf表示的碳原子数1~3的烷基,可以列举出甲基、乙基、丙基、2-丙基,作为以Rg表示的碳原子数为1~4的烷基,可以列举出甲基、乙基、丙基、异丙基、丁基、仲丁基、叔丁基、异丁基。
具体地讲,作为钛前体,可以列举出四(乙氧基)钛、四(2-丙氧基)钛、四(丁氧基)钛、四(仲丁氧基)钛、四(异丁氧基)钛、四(叔丁氧基)钛、四(叔戊基)钛、四(1-甲氧基-2-甲基-2-丙氧基)钛等四烷氧基钛类;四(戊烷-2,4-二酮(dionato))钛、(2,6-二甲基庚烷-3,5-二酮)钛、四(2,2,6,6-四甲基庚烷-3,5-二酮)钛等四β-二酮钛类;双(甲氧基)双(戊烷-2,4-二酮)钛、双(乙氧基)双(戊烷-2,4-二酮)钛、双(叔丁氧基)双(戊烷-2,4-二酮)钛、双(甲氧基)双(2,6-二甲基庚烷-3,5-二酮)钛、双(乙氧基)双(2,6-二甲基庚烷-3,5-二酮)钛、双(2-丙氧基)双(2,6-二甲基庚烷-3,5-二酮)钛、双(叔丁氧基)双(2,6-二甲基庚烷-3,5-二酮)钛、双(叔戊氧基)双(2,6-二甲基庚烷-3,5-二酮)钛、双(甲氧基)双(2,2,6,6-四甲基庚烷-3,5-二酮)钛、双(乙氧基)双(2,2,6,6-四甲基庚烷-3,5-二酮)钛、双(2-丙氧基)双(2,6,6,6-四甲基庚烷-3,5-二酮)钛、双(叔丁氧基)双(2,2,6,6-四甲基庚烷-3,5-二酮)钛、双(叔戊氧基)双(2,2,6,6-四甲基庚烷-3,5-二酮)钛等双(烷氧基)双(β二酮)钛类;(2-甲基戊烷二氧)双(2,2,6,6-四甲基庚烷-3,5-二酮)钛、(2-甲基戊烷二氧)双(2,6-二甲基庚烷-3,5-二酮)钛等二醇氧基(glycoxy)双(β二酮)钛类等,作为锆前体,可以列举出将作为上述钛前体所列举的化合物的钛置换为锆的化合物。
作为铝前体,可以列举出例如与本发明烷氧基金属化合物具有相同配位基的三烷氧基铝或用下述[化学式7]中所示的通式表示的化合物。
[化学式7]
(式中,L表示具有氮原子或氧原子的5~6元环的配位性杂环化合物,Ra表示可以被卤原子取代、也可以在链中含有氧原子的碳原子数为1~20的烷基,Rc表示碳原子数为1~8的烷基,Re和Rf表示氢原子或者碳原子数为1~3的烷基,Rg表示碳原子数为1~4的烷基,Rh表示可以被卤原子取代、也可以在链中含有氧原子的碳原子数为1~20的烷基或碳原子数为1~8的烷氧基,Ri表示碳原子数为1~4的烷基,p’表示0~3的整数,q’表示0~2的整数,r’表示0~2的整数。)
在上述[化学式7]所示的化学式中,作为以L表示的配位性杂环化合物,可以列举出18-冠-6、二环己基-18-冠-6、24-冠-8、二环己基-24-冠-8、二苯并-24-冠-8等冠醚类;环烷烃(cyclam)、四氮杂环十二烷(cyclen)等环状多胺类;吡啶、吡咯烷、哌啶、吗啉、N-甲基吡咯烷、N-甲基哌啶、N-甲基吗啉、四氢呋喃、四氢吡喃、1,4-二噁烷、噁唑、噻唑、氧硫杂戊烷(oxathiolan)等,作为Ra、Rc、Re、Rf和Rg,可以列举出作为上述钛、锆前体所列举的基团,作为以Rh表示的碳原子数为1~8的烷氧基,可以列举出甲氧基、乙氧基、丙氧基、异丙氧基、丁氧基、仲丁氧基、叔丁氧基、异丁氧基、戊氧基、异戊氧基、仲戊氧基、叔戊氧基、己氧基、1-乙基戊氧基、环己氧基、1-甲基环己氧基、庚氧基、异庚氧基、叔庚氧基、正辛氧基、异辛氧基、叔辛氧基、2-乙基己氧基,作为Ri,可以列举出Rg中列举的基团。
作为铋前体,可以列举出三苯基铋、三(o-甲基苯基)铋、三(m-甲基苯基)铋、三(p-甲基苯基)铋等三芳基铋化合物;三甲基铋等三烷基铋化合物;三(2,2,6,6-四甲基庚烷-3,5-二酮)铋等β-二酮类络合物;三(环戊二烯基)铋、三(甲基环戊二烯基)铋等环戊二烯基络合物;三(叔丁氧基)铋、三(叔戊氧基)铋、三(乙氧基)铋等低分子醇的烷氧化物、以下述[化学式8]中所示的通式表示的烷氧基金属化合物、与本发明烷氧基金属化合物具有相同配位基的三烷氧基铋化合物等。
[化学式8]
(式中,Re和Rf表示氢原子或者碳原子数为1~3的烷基,Rg表示碳原子数为1~4的烷基,n表示1或2。)
作为在上述[化学式8]所示的通式中的Re、Rf和Rg,可以列举出在上述的钛前体和锆前体中列举的基团。
作为稀土类前体,可以列举出例如与本发明烷氧基金属化合物具有相同配位基的三烷氧基化合物或以下述[化学式9]中所示的通式表示的化合物。
[化学式9]
(式中,M2表示稀土类原子,Ra和Rb分表示可以被卤原子取代、也可以在链中含有氧原子的碳原子数为1~20的烷基,Rc表示碳原子数为1~8的烷基,Re和Rf表示氢原子或者碳原子数为1~3的烷基,Rg表示碳原子数为1~4的烷基,Rj表示碳原子数为1~4的烷基,p’表示0~3的整数,r’表示0~2的整数。)
在以上述[化学式9]所示的通式表示的稀土类供给源化合物中,作为以M2表示的稀土类原子,可以列举出锶、钇、镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱、钌,作为以Ra、Rb、Rc、Re、Rf和Rg表示的基团,可以列举出作为上述钛前体和锆前体所列举的基团,作为以Rj表示的碳原子数为1~4的烷基,可以列举出在上述的Rg中列举的基团。
另外,为了对本发明的烷氧基金属化合物和其它的前体赋予稳定性,也可以在上述CVD用原料中根据需要含有亲核性试剂。作为该亲核性试剂,可以列举出甘醇二甲醚、二甘醇二甲醚、三甘醇二甲醚、四甘醇二甲醚等乙二醇醚类,18-冠-6、二环己基-18-冠-6、24-冠-8、二环己基-24-冠-8、二苯并-24-冠-8等冠醚类,乙二胺、N,N’-四甲基乙二胺、二亚乙基三胺、三亚乙基四胺、四亚乙基五胺、五亚乙基六胺、1,1,4,7,7-五甲基二亚乙基三胺、1,1,4,7,10,10-六甲基三亚乙基四胺、三乙氧基三亚乙基胺等多胺类,环烷烃(cyclam)、四氮杂环十二烷(cyclen)等环状多胺类,吡啶、吡咯烷、哌啶、吗啉、N-甲基吡咯烷、N-甲基哌啶、N-甲基吗啉、四氢呋喃、四氢吡喃、1,4-二噁烷、噁唑、噻唑、氧硫杂戊烷等杂环化合物类,乙酰乙酸甲酯、乙酰乙酸乙酯、乙酰乙酸2-甲氧基乙基酯等β-酮酯类或乙酰丙酮、2,4-己二酮、2,4-庚二酮、3,5-庚二酮、二叔戊酰基甲烷(dipivaroylmethane)等β-二酮类,相对于1摩尔的前体,作为稳定剂的这些亲核性试剂的用量通常为0.1mol~10mol,优选为1~4mol。
本发明的薄膜制造方法是利CVD法,所述的CVD法是将使本发明的烷氧基金属化合物和根据需要使用的其它前体气化而形成的蒸汽和根据需要使用的反应性气体导入到基板上,然后,使前体在基板上分解和/或进行化学反应而使薄膜在基板上生长、沉积的方法。对原料的输送供给方法、沉积方法、制造条件、制造装置等没有特别的限制,可以使用公知常见的条件、方法等。
作为根据需要所使用的上述反应性气体,例如作为氧化性的气体,可以列举出氧气、臭氧、二氧化氮、一氧化氮、水蒸气、过氧化氢、甲酸、乙酸、乙酸酐等;作为还原性的气体,可以列举出氢气;另外,作为制造氮化物的气体,可以列举出单烷基胺、二烷基胺、三烷基胺、亚烷基二胺等有机胺化合物、肼、氨等。
另外,作为上述的输送供给方法,可以列举出前述的气体输送方法、液体输送方法、单源法、混合源法等。
另外,作为上述的沉积方法,可以列举出只通过热使原料气体或原料气体与反应性气体反应,并使薄膜沉积的热CVD;使用热和等离子的等离子CVD;使用热和光的光CVD;使用热、光和等离子的光等离子CVD;将CVD的沉积反应划分为基本反应,在分子级别下阶梯地进行沉积的ALD(Atomic Layer Deposition)。
另外,作为上述制造条件,可以列举出反应温度(基板温度)、反应压力、沉积速度等。对于反应温度,其是本发明的烷氧基金属化合物充分反应的温度,优选为160℃或以上,更优选为250℃~800℃。另外,在沉积方法为热CVD和光CVD时,反应压力优选为大气压~10Pa,在使用等离子时,反应压力优选为10~2000Pa。另外,沉积速度可以根据原料的供给条件(气化温度、气化压力)、反应温度和反应压力来控制。如果沉积速度较大,则所得到的薄膜的性质可能恶化,如果较少,则生产性上可能会产生问题,所以沉积速度优选为0.5~5000nm/分钟,更优选为1~1000nm/分钟。另外,在沉积方法为ALD法时,可以通过循环次数来控制膜厚,以得到所希望的膜厚。
另外,在本发明的制造方法中,在薄膜沉积后,也可以在惰性气体氛围下、氧化性气体氛围下或者还原性气体氛围下进行退火处理以得到更好的电特性,在需要阶梯覆盖时,可以设置回流(reflow)工序。此时的温度通常为400~1200℃,优选为500~800℃。
根据使用本发明的薄膜形成用原料的本发明的薄膜的制造方法所制造的薄膜,可以通过适当选择其它成分的前体、反应性气体和制造条件,形成氧化物陶瓷、氮化物陶瓷、玻璃等所希望的种类的薄膜。作为这些薄膜的组成,例如,可以列举出氧化硅、氧化铪、硅-钛复合氧化物、硅-锆复合氧化物、硅-铪复合氧化物、硅-铋复合氧化物、铪-铝复合氧化物、铪-稀土类元素复合氧化物、硅-铋-钛复合氧化物、硅-铪-铝复合氧化物、硅-铪-稀土类元素复合氧化物、氮化硅、氮化铪,作为这些薄膜的用途,可以列举出例如高介电电容器膜、栅绝缘膜、栅电路膜、强介电电容器膜、电容器膜、阻挡膜等电子元件构件、光纤、光波导、光放大器、光学开关等光学玻璃构件等。
实施例
以下,举出制造例、评价例、实施例等对本发明进行更详细地说明,但是,本发明不受到以下实施例等的任何限定。
另外,下述制造例1-3表示本发明的烷氧基金属化合物的实施例,在评价例1和2中,进行本发明的烷氧基金属化合物和比较化合物的热氧化分解性评价,在评价例3和4中,进行本发明的烷氧基金属化合物和比较化合物的挥发特性评价。此外,下述实施例1~3表示本发明的薄膜形成用材料的实施例和本发明的薄膜的制造方法的实施例,下述比较例1表示使用了并非是本发明的烷氧基金属化合物的化合物的薄膜形成用原料的实施例和薄膜的制造方法的实施例。
[制造例1]化合物No.1的制造
在干燥的氩气氛围气体下,向反应烧瓶中加入1-二甲基氨基-2-丙醇0.687摩尔、进行了脱水处理的甲苯500ml和钠0.481摩尔,进行搅拌直到固体钠消失。使体系内的温度为4℃后,向其中滴加干燥甲苯50ml和四氯化硅0.1145摩尔的混合液。此时,将体系内的温度控制为30℃或以下。滴加结束后,在120℃下回流27小时。将反应液用0.2μm的过滤器进行过滤,然后将通过减压蒸馏除去了溶剂和未反应的醇的浓缩液进行减压蒸馏。由25~30Pa、塔顶温度108~109℃的馏分以46%的收率获得无色液体。对该液体进一步通过减压蒸馏进行精制,从而获得无色透明液体。利用该精制的回收率是95%。获得的无色透明液体被鉴定为是作为目标物的化合物No.1。以下表示所得到的无色透明液体的分析值。
(分析值)
(1)元素分析(金属分析:ICP-AES)
硅:6.49质量%(理论值6.43%)、Na:低于1ppm、Cl:低于5ppm
(2)1H-NMR(溶剂∶重苯)(化学位移∶多重性∶H数)
(1.46∶d∶12)(2.18∶s∶24)(2.27∶m∶4)(2.53∶m∶4)(4.44∶m∶4)
(3)TG-DTA(Ar100ml/min、10℃/min升温、试样量为7.762mg)
减少50质量%的温度为217℃
[制造例2]化合物No.2的制造
在干燥的氩气氛围气体下,向反应烧瓶中加入1-二甲基氨基-2-甲基-2-丙醇0.687摩尔、进行了脱水处理的甲苯500ml和钠0.481摩尔,进行搅拌直到固体钠消失。使体系内的温度为4℃后,向其中滴加干燥甲苯50ml和四氯化硅0.1145摩尔的混合液。此时,将体系内的温度控制为30℃或以下。滴加结束后,在120℃下回流27小时。将反应液用0.2μm的过滤器进行过滤,然后将通过减压蒸馏除去了溶剂和未反应醇的浓缩液进行减压蒸馏。由25~30Pa、塔顶温度115~118℃的馏分以52%的收率获得无色液体。对该液体进一步通过减压蒸馏进行精制,从而获得无色透明液体。利用该精制的回收率是95%。获得的无色透明液体被鉴定为是作为目标物的化合物No.2。以下表示所得到的无色透明液体的分析值。
(分析值)
(1)元素分析(金属分析:ICP-AES)
硅:6.10质量%(理论值6.04%)、Na:低于1ppm、Cl:低于5ppm
(2)1H-NMR(溶剂∶重苯)(化学位移∶多重性∶H数)
(1.56∶s∶24)(2.32∶s∶24)(2.44∶s∶8)
(3)TG-DTA(Ar100ml/min、10℃/min升温、试样量为9.199mg)
减少50质量%的温度为233℃
[制造例3]化合物No.13的制造
在干燥的氩气氛围气体下,向反应烧瓶中加入四(2-丙氧基)铪·2-丙醇0.100摩尔、进行了脱水处理的二甲苯60ml和1-二甲基氨基-2-甲基-2-丙醇0.600摩尔,一边馏去副产生的2-丙醇,一边在140℃下进行反应8小时。对馏去二甲苯后得到的残渣进行减压蒸馏。由25~28Pa、塔顶温度154~150℃的馏分以32%的收率获得无色液体。对该液体进一步通过减压蒸馏进行精制,从而获得无色透明液体。利用该精制的回收率是93%。获得的无色透明液体被鉴定为是作为目标物的化合物No.13。以下表示所得到的无色透明液体的分析值。
(分析值)
(1)元素分析(金属分析:ICP-AES)
铪:28.2质量%(理论值27.7%)
(2)1H-NMR(溶剂∶重苯)(化学位移∶多重性∶H数)
(1.45∶s∶24)(2.36∶s∶24)(2.53∶s∶8)
(3)TG-DTA(Ar100ml/min、10℃/min升温、试样量为7.695mg)
减少50质量%的温度为250℃
[评价例1]硅化合物的热氧化分解性评价
对由上述制造例1获得的化合物No.1、四乙氧基硅烷(TEOS)和以下所示的比较化合物1进行热氧化分解性的评价。对于化合物No.1和比较化合物1,从30℃开始以10℃/分钟的升温速度、在干燥氧(100ml/分钟)气流下的测量条件进行差示热分析(TG-DTA),通过测量DTA的放热峰顶温度和450℃的残留成分进行评价。结果示于表1。
此外,对于TEOS,由于不能用上述方法进行测量,所以在密闭容器中与氧混合,在500℃下加热1分钟,确认有无氧化分解。其结果,确认没有氧化分解。
[化合物10]
比较化合物1
[表1]
化合物 | 放热峰顶 | 450℃残留成分 | 作为SiO2的理论值 |
化合物No.1 | 205℃ | 12.8质量% | 13.8质量% |
比较化合物1 | 217℃ | 5.0质量% | 13.5质量% |
TEOS | - | 0质量% | 26.3质量% |
由上述表1可知,如果将化合物No.1和比较化合物1进行比较,则对于放热峰顶来说,化合物No.1比比较化合物1的温度还低。对于450℃的残留量而言,化合物No.1是接近于SiO2的理论值的值,比较化合物1是比理论值还小得多的值。这是因为化合物No.1与TEOS和比较化合物1相比,由于热氧化分解反应在低温下进行,因而可以确认:其是优异的向薄膜供给氧化硅的前体。
[评价例2]铪化合物的热氧化分解性评价
对于由上述制造例3所得到的化合物No.13和以下所示的比较化合物2,与上述评价例1相同地进行热氧化分解性的评价。结果示于表2。
[化合物11]
比较化合物2
[表2]
化合物 | 放热峰顶 | 450℃残留成分 | 作为HfO2的理论值 |
化合物No.13 | 256℃ | 30.1质量% | 32.7质量% |
比较化合物2 | 271℃ | 18.2质量% | 30.2质量% |
由上述表2可知,如果将化合物No.13和比较化合物2进行比较,则对于放热峰顶来说,化合物No.13比比较化合物2的温度还低。对于450℃的残留量而言,化合物No.13是接近于作为HfO2的理论值的值,比较化合物2是比理论值还小的值。这是因为化合物No.13与比较化合物2相比,热氧化分解反应在低温下进行,因而可以确认:其是优异的向薄膜供给氧化铪的前体。
[评价例3]硅化合物的挥发特性评价
对化合物No.1和2以及以下所示的比较化合物3,通过蒸气压测量评价挥发特性。通过将体系固定在恒定的压力下测量液面附近的蒸汽温度的方法来进行蒸气压测量。通过改变体系的压力来测量3~4点的蒸汽温度,根据克劳修斯-克拉珀龙曲线,使用蒸气压的式子计算出120℃和150℃下的蒸气压。结果示于表3。
[化合物12]
比较化合物3
[表3]
化合物 | 蒸气压的式子 | 120℃的蒸汽压(Torr) | 150℃的蒸汽压(Torr) |
化合物No.1 | LogP(Torr)=12.97-5302/T(K) | 0.301 | 2.73 |
化合物No.2 | LogP(Torr)=18.65-7562/T(K) | 0.256 | 5.93 |
比较化合物3 | LogP(Torr)=13.93-5842/T(K) | 0.116 | 1.32 |
由上述的表3可以确认,通过(I)中的M是硅的本发明的烷氧基金属化合物比比较化合物3的蒸气压还大,挥发特性优异。
[评价例4]铪化合物的挥发特性评价
对化合物No.13以及以下所示的比较化合物4,用与上述评价例3相同的方法,进行蒸气压测量,计算出150℃和200℃下的蒸气压,评价挥发特性。
此外,由于比较化合物4即使在210℃下也不会挥发,所以不能获得蒸汽相,不可能测量蒸气压。对于比较化合物4,在干燥氩气流下进行差示热分析(TG-DTA),结果可以确认只通过热慢慢地产生分解。
对于化合物No.13的结果示于表4。
[化合物13]
比较化合物4
[表4]
化合物 | 蒸气压的式子 | 150℃的蒸气压(Torr) | 200℃的蒸气压(Torr) |
化合物No.13 | LogP(Torr)=13.46-5963/T(K) | 0.231 | 7.13 |
由上述的表4可以确认,通过(I)中的M是铪的本发明的烷氧基金属化合物作为CVD用原料表现出了足够的蒸气压。与此相反,比较化合物4不能成为蒸汽的状态,不适合作为CVD用原料。
[实施例1]
将乙基环己烷在金属钠线中干燥后,在氩气流下,分馏前馏分10质量%和釜残留馏分10质量%,进行蒸馏精制,获得水分量低于1ppm的溶剂。在该溶剂500ml中在氩气流下混合0.02摩尔化合物No.2、0.1摩尔化合物No.13,从而获得硅-铪的混合源。使用图1中所示的CVD装置和上述混合源,在硅晶片上以下述条件制造铪硅复合氧化物薄膜。对于所制造的薄膜,使用荧光X射线进行膜厚和组成的测量。以下表示这些结果。
(条件)
气化室温度:170℃、原料流量:20mg/分钟、反应压力:667Pa、反应时间:20分钟、基板温度:450℃、载气Ar:200sccm、沉积后的退火条件:氧流量100sccm中600℃下10分钟
(结果)
膜厚:63nm、组成比(摩尔):Hf/Si=1.00∶0.17
[实施例2]
将乙基环己烷在金属钠线中干燥后,在氩气流下,分馏前馏分10质量%和釜残留馏分10质量%,进行蒸馏精制,获得水分量低于1ppm的溶剂。在该溶剂500ml中在氩气流下混合0.02摩尔化合物No.1、0.1摩尔四(1-甲氧基-2-甲基-2-丙氧基)铪,从而获得硅-铪的混合源。使用图1中所示的CVD装置,在硅晶片上以下述条件使用上述混合源来制造铪硅复合氧化物薄膜。对于所制造的薄膜,与上述实施例1相同地进行膜厚和组成的测量。以下表示这些结果。
(条件)
气化室温度:170℃、原料流量:20mg/分钟、反应压力:667Pa、反应时间:30分钟、基板温度:450℃、载气Ar:200sccm、沉积后的退火条件:氧流量100sccm中600℃下10分钟
(结果)
膜厚:98nm、组成比(摩尔):Hf/Si=1.00∶0.22
[比较例1]
将乙基环己烷在金属钠线中干燥后,在氩气流下,分馏前馏分10质量%和釜残留馏分10质量%,进行蒸馏精制,获得水分量低于1ppm的溶剂。在该溶剂500ml中在氩气流下混合0.1摩尔四(1-甲氧基-2-甲基-2-丙氧基)硅、0.1摩尔四(1-甲氧基-2-甲基-2-丙氧基)铪,从而获得硅-铪的比较用混合源。使用图1中所示的CVD装置,在硅晶片上以下述条件使用上述比较用混合源制造铪硅复合氧化物薄膜。对于所制造的薄膜,与上述实施例1相同地进行膜厚和组成的测量。以下表示这些结果。
(条件)
气化室温度:170℃、原料流量:20mg/分钟、反应压力:667Pa、反应时间:30分钟、基板温度:450℃、载气Ar:200sccm、沉积后的退火条件:氧流量100sccm中600℃下10分钟
(结果)
膜厚:87nm、组成比(摩尔):Hf/Si=1.00∶0.05
[实施例3]
将乙基环己烷在金属钠线中干燥后,在氩气流下,分馏前馏分10质量%和釜残留馏分10质量%,进行蒸馏精制,获得水分量低于1ppm的溶剂。在该溶剂500ml中在氩气流下混合0.1摩尔化合物No.13、0.03摩尔三(1-甲基氨基-2-甲基-2-丙氧基)钇化合物,从而获得铪-钇的混合源。使用图1中所示的CVD装置,在硅晶片上以下述条件使用上述混合源制造铪-钇复合氧化物薄膜。对于所制造的薄膜,使用荧光X射线进行膜厚和组成的测量。以下表示这些结果。
(条件)
气化室温度:170℃、原料流量:20mg/分钟、反应压力:667Pa、反应时间:30分钟、基板温度:450℃、载气:氩200sccm、氧化气体:氧300sccm
(结果)
膜厚:100nm、组成比(摩尔):Hf/Y=1.00∶0.25
就上述实施例1~3而言,薄膜形成原料的组成和所获得的薄膜的组成非常一致。与此相反,在比较例1中,薄膜形成原料的组成和所获得的薄膜的组成不一致。这表示本发明的烷氧基金属化合物可以赋予良好的组成控制。
工业上的可利用性
如果使用含有本发明烷氧基金属化合物的本发明的薄膜形成用原料,则可以实现组成控制性等优异的薄膜的制造,特别是在通过CVD法制造多成分薄膜时表现出优异的效果。
Claims (6)
2、根据权利要求1记载的烷氧基金属化合物,在上述通式(1)中,A是亚甲基。
3、根据权利要求1或2记载的烷氧基金属化合物,在上述通式(1)中,M是硅原子。
4、根据权利要求1或2记载的烷氧基金属化合物,在上述通式(1)中,M是铪原子。
5、薄膜形成用原料,其含有权利要求1~4任一项所记载的烷氧基金属化合物。
6、薄膜的制造方法,其中将含有使权利要求5所记载的薄膜形成用原料气化而得到的烷氧基金属化合物的蒸汽引入到基材上,使蒸汽分解和/或进行化学反应而在基材上形成薄膜。
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