CN103502202B - 醇盐化合物以及薄膜形成用原料 - Google Patents
醇盐化合物以及薄膜形成用原料 Download PDFInfo
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- CN103502202B CN103502202B CN201280022056.6A CN201280022056A CN103502202B CN 103502202 B CN103502202 B CN 103502202B CN 201280022056 A CN201280022056 A CN 201280022056A CN 103502202 B CN103502202 B CN 103502202B
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- 239000002994 raw material Substances 0.000 title claims abstract description 59
- 239000010409 thin film Substances 0.000 title claims abstract description 9
- -1 Alkoxide compound Chemical class 0.000 title abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 88
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 27
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 10
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 9
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims abstract description 8
- 239000010408 film Substances 0.000 claims description 87
- 150000004703 alkoxides Chemical class 0.000 claims description 56
- 230000015572 biosynthetic process Effects 0.000 claims description 38
- 239000002243 precursor Substances 0.000 claims description 37
- 230000008569 process Effects 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 28
- 238000004519 manufacturing process Methods 0.000 claims description 25
- 239000003960 organic solvent Substances 0.000 claims description 10
- 238000012546 transfer Methods 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 69
- 150000001875 compounds Chemical class 0.000 description 49
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 39
- 229910052759 nickel Inorganic materials 0.000 description 38
- 239000007789 gas Substances 0.000 description 26
- 238000006243 chemical reaction Methods 0.000 description 25
- 238000004458 analytical method Methods 0.000 description 16
- 239000000203 mixture Substances 0.000 description 16
- 239000007787 solid Substances 0.000 description 15
- 238000000151 deposition Methods 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 11
- 238000005481 NMR spectroscopy Methods 0.000 description 10
- 230000008021 deposition Effects 0.000 description 10
- 229910052739 hydrogen Inorganic materials 0.000 description 10
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- 230000000052 comparative effect Effects 0.000 description 9
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- 239000002184 metal Substances 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 9
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- UHOVQNZJYSORNB-MZWXYZOWSA-N benzene-d6 Chemical compound [2H]C1=C([2H])C([2H])=C([2H])C([2H])=C1[2H] UHOVQNZJYSORNB-MZWXYZOWSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
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- 239000011734 sodium Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
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- 238000012795 verification Methods 0.000 description 4
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 3
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 3
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 3
- UXFQFBNBSPQBJW-UHFFFAOYSA-N 2-amino-2-methylpropane-1,3-diol Chemical compound OCC(N)(C)CO UXFQFBNBSPQBJW-UHFFFAOYSA-N 0.000 description 3
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- 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
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- 125000004429 atom Chemical group 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 description 3
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- 229910017053 inorganic salt Inorganic materials 0.000 description 3
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
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- 150000004767 nitrides Chemical class 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 239000012048 reactive intermediate Substances 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
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- QEGNUYASOUJEHD-UHFFFAOYSA-N 1,1-dimethylcyclohexane Chemical compound CC1(C)CCCCC1 QEGNUYASOUJEHD-UHFFFAOYSA-N 0.000 description 2
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- 238000005160 1H NMR spectroscopy Methods 0.000 description 2
- OISVCGZHLKNMSJ-UHFFFAOYSA-N 2,6-dimethylpyridine Chemical compound CC1=CC=CC(C)=N1 OISVCGZHLKNMSJ-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
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- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
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- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 description 1
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- 241000534944 Thia Species 0.000 description 1
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- 230000000903 blocking effect Effects 0.000 description 1
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- 229940043232 butyl acetate Drugs 0.000 description 1
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- 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 1
- 229910052804 chromium Inorganic materials 0.000 description 1
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- 229910017052 cobalt Inorganic materials 0.000 description 1
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
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- 239000000039 congener Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- VBWIZSYFQSOUFQ-UHFFFAOYSA-N cyclohexanecarbonitrile Chemical compound N#CC1CCCCC1 VBWIZSYFQSOUFQ-UHFFFAOYSA-N 0.000 description 1
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 125000005265 dialkylamine group Chemical group 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- 229940043279 diisopropylamine Drugs 0.000 description 1
- HPYNZHMRTTWQTB-UHFFFAOYSA-N dimethylpyridine Natural products CC1=CC=CN=C1C HPYNZHMRTTWQTB-UHFFFAOYSA-N 0.000 description 1
- OMBRFUXPXNIUCZ-UHFFFAOYSA-N dioxidonitrogen(1+) Chemical compound O=[N+]=O OMBRFUXPXNIUCZ-UHFFFAOYSA-N 0.000 description 1
- WEHWNAOGRSTTBQ-UHFFFAOYSA-N dipropylamine Chemical compound CCCNCCC WEHWNAOGRSTTBQ-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
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- 238000001704 evaporation Methods 0.000 description 1
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- 230000002349 favourable effect Effects 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- ZTOMUSMDRMJOTH-UHFFFAOYSA-N glutaronitrile Chemical compound N#CCCCC#N ZTOMUSMDRMJOTH-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- CATSNJVOTSVZJV-UHFFFAOYSA-N heptan-2-one Chemical compound CCCCCC(C)=O CATSNJVOTSVZJV-UHFFFAOYSA-N 0.000 description 1
- NGAZZOYFWWSOGK-UHFFFAOYSA-N heptan-3-one Chemical compound CCCCC(=O)CC NGAZZOYFWWSOGK-UHFFFAOYSA-N 0.000 description 1
- SDAXRHHPNYTELL-UHFFFAOYSA-N heptanenitrile Chemical compound CCCCCCC#N SDAXRHHPNYTELL-UHFFFAOYSA-N 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- NDOGLIPWGGRQCO-UHFFFAOYSA-N hexane-2,4-dione Chemical compound CCC(=O)CC(C)=O NDOGLIPWGGRQCO-UHFFFAOYSA-N 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- KHYBPSFKEHXSLX-UHFFFAOYSA-N iminotitanium Chemical compound [Ti]=N KHYBPSFKEHXSLX-UHFFFAOYSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 1
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 1
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 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
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 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
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 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
- 239000012046 mixed solvent Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- QATBRNFTOCXULG-UHFFFAOYSA-N n'-[2-(methylamino)ethyl]ethane-1,2-diamine Chemical compound CNCCNCCN QATBRNFTOCXULG-UHFFFAOYSA-N 0.000 description 1
- VIJMMQUAJQEELS-UHFFFAOYSA-N n,n-bis(ethenyl)ethenamine Chemical compound C=CN(C=C)C=C VIJMMQUAJQEELS-UHFFFAOYSA-N 0.000 description 1
- DAZXVJBJRMWXJP-UHFFFAOYSA-N n,n-dimethylethylamine Chemical compound CCN(C)C DAZXVJBJRMWXJP-UHFFFAOYSA-N 0.000 description 1
- GVWISOJSERXQBM-UHFFFAOYSA-N n-methylpropan-1-amine Chemical compound CCCNC GVWISOJSERXQBM-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 229910001000 nickel titanium 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
- 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
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
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- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000013618 particulate matter Substances 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
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 1
- 150000003053 piperidines Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 description 1
- OGHBATFHNDZKSO-UHFFFAOYSA-N propan-2-olate Chemical compound CC(C)[O-] OGHBATFHNDZKSO-UHFFFAOYSA-N 0.000 description 1
- DNIAPMSPPWPWGF-UHFFFAOYSA-N propylene glycol Substances CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000003870 refractory metal Substances 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
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 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
- 229910000104 sodium hydride Inorganic materials 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003860 storage 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
- 238000010189 synthetic method Methods 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
- 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
- 238000012360 testing method Methods 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
Classifications
-
- 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
- C07F15/04—Nickel compounds
- C07F15/045—Nickel compounds without a metal-carbon linkage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- 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
-
- 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
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Abstract
本发明涉及一种由下述通式(I)表示的醇盐化合物以及含有该醇盐化合物的薄膜形成用原料。式中,R1表示碳原子数为2~4的直链或支链状烷基,R2、R3表示碳原子数为1~4的直链或支链状烷基。在下述通式(I)中,R1优选为乙基。另外,还优选R2和R3中的任一者或两者为乙基。另外,含有由下述通式(I)表示的醇盐化合物的薄膜形成用原料优选用作化学气相沉积法用原料,
Description
技术领域
本发明涉及一种具有特定的配位基的新型镍醇盐化合物、含有该化合物的薄膜形成用原料。
背景技术
含有镍的薄膜主要用于电阻膜、阻挡膜等电子部件的构件、磁性膜等记录介质用的构件、电极等薄膜太阳电池用构件等。
作为上述的薄膜的制造方法,可以列举出火焰沉积法、溅射法、离子镀法、涂布热分解法以及溶胶凝胶法等MOD法、化学气相沉积法等,由于具有组成控制性、阶梯覆盖性优良,适合于批量生产化,以及能够实现混合集成等诸多优点的缘故,包括ALD(Atomic Layer Deposition,原子层沉积)法在内的化学气相沉积(以下有时也仅记为CVD)法是最适合的制造工艺。
在MOD法或CVD法中,作为对薄膜供给镍原子的前体,一直使用利用了有机配位基的化合物。在专利文献1中报道了镍的3级醇盐(也称为叔醇盐)化合物,在专利文献2中,报道了通过使用了镍的醇盐的CVD法来制造含有镍原子的复合氧化物薄膜的制造方法。另外,在非专利文献1中,报道了通过使用了镍的3级醇盐化合物的ALD法来制作镍氧化膜的技术。
有关镍化合物,对本发明的2级醇盐(也称为仲醇盐)化合物并没有报道,并且对于使用了它的薄膜的制造方法也没有报道。
现有技术文献
专利文献
专利文献1:WO2006/107121A1
专利文献2:WO2006/021850A2
非专利文献
非专利文献1:J.Vac.Sci.Technol.A,Vol.23,No.4,Jul/Aug20051238-1243
发明内容
本发明要解决的问题
对于CVD法等通过使化合物(前体)气化而形成薄膜的方法,该化合物被要求的性质是:熔点较低、能够以液体的状态进行输送,以及蒸汽压较大、容易使其气化。以往的镍化合物并非是在这些方面能够充分满足要求的化合物。
解决问题的手段
本发明者等人反复研究的结果发现,配位基使用了特定的仲氨基醇的镍醇盐化合物能够解决上述问题,从而完成了本发明。
即,本发明提供一种醇盐化合物(alkoxide compound),其由下述通式(I)表示。
(式中,R1表示碳原子数为2~4的直链或支链状烷基,R2、R3表示碳原子数为1~4的直链或支链状烷基。)
另外,本发明提供一种薄膜形成用原料,其含有上述通式(I)表示的醇盐化合物。
发明的效果
根据本发明,能够获得蒸汽压较高,在常温下或通过稍稍加热就成为液体的低熔点的镍醇盐化合物,进而通过将该化合物用作CVD法中的薄膜形成用原料,则在CVD法的含镍薄膜的制造过程中,前体的输送性优良,对基体的供给量的控制容易,并能够稳定地将薄膜形成用原料供给至基体。
附图说明
图1是实施例3中得到的化合物No.4的NMR图。
图2是实施例4中得到的化合物No.7的NMR图。
具体实施方式
下面,根据其优选的实施方式,对本发明的醇盐化合物以及含有该化合物的薄膜形成用材料进行详细说明。
在上述通式(I)中,作为R1所表示的碳原子数为2~4的直链或支链状烷基,可以列举出乙基、丙基、异丙基、丁基、仲丁基、叔丁基、异丁基,作为R2、R3所表示的碳原子数为1~4的的直链或支链状烷基,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。本发明的醇盐化合物有时还具有光学异构体,但不会因其光学异构而区分。
在上述通式(I)中,当在具有使化合物气化的工序的薄膜的制造方法中使用时,R1~R3优选为使化合物在常温常压下是液体状态并且蒸汽压较大的基团,具体地,R1优选为乙基,R2~R3优选其中的任何一者或两者为乙基。另外,当在无气化工序的MOD法的薄膜的制造方法中使用时,R1~R3可以根据在所使用的溶剂中的溶解性以及薄膜形成反应等来任意选择。
将配位基中的末端供体基与金属原子配位而形成环结构的情况示于下述通式(II)中。本发明的醇盐化合物以上述通式(I)作为代表来表示,但不与下述通式(II)区分,是包括两者在内的概念。
(式中,R1表示碳原子数为2~4的直链或支链状烷基,R2、R3表示碳原子数为1~4的直链或支链状烷基。)
作为本发明的醇盐化合物的具体例,可以列举出下述化合物No.1~No.18。不过,本发明不受以下的例示化合物的任何限定。
本发明的醇盐化合物的制造方法没有特别限制,可以应用众所周知的反应来制造。作为制造方法,可以应用使用了对应的氨基醇的众所周知的一般的醇盐化合物的合成方法。例如可以列举出下述方法:使镍的卤化物、硝酸盐等无机盐或其水合物与对应的醇化合物在钠、氢化钠、氨基钠、氢氧化钠、甲氧基钠、氨、胺等碱的存在下反应的方法;使镍的卤化物、硝酸盐等无机盐或其水合物与对应的醇化合物的钠醇盐、锂醇盐、钾醇盐等碱金属醇盐化合物反应的方法;使镍的甲醇盐、乙醇盐、异丙醇盐、丁醇盐等低分子醇的醇盐化合物与对应的醇化合物发生交换反应的方法;使镍的卤素化物、硝酸盐等无机盐与提供反应性中间体的衍生物反应,得到反应性中间体之后,再使其与对应的醇化合物反应的方法。
作为上述的反应性中间体,可以列举出双(二烷基氨基)镍、双(双(三甲基甲硅烷基)氨基)镍等镍的酰胺化合物。
此外,本发明的醇盐化合物的特征是,其是2级醇盐化合物,而且本发明的醇盐化合物显示出特别的性质,与此相对,具有氨基醇盐作为配位基的Cu、Ti、Zr、Hf络合物中,3级醇盐化合物具有优良的特性。
本发明的醇盐化合物除了可以作为制造含有镍的薄膜的前体使用以外,还可以用于有机合成用催化剂、有机合成用原料等用途。
本发明的薄膜形成用原料是指含有上述说明的本发明的醇盐化合物作为薄膜的前体的原料,其形态根据使用该薄膜形成用原料的制造工艺的不同而不同。本发明的醇盐化合物从其物性来看,作为化学气相沉积法用原料是特别有用的。也就是说,本发明的薄膜形成用原料优选是化学气相沉积法用原料。
当本发明的薄膜形成用原料是化学气相沉积法用原料时,其形态可以根据所使用的化学气相沉积法的输送供给方法等手法来适当选择。作为化学气相沉积用原料使用时的本发明的薄膜形成用原料的形态的代表例,可以列举出下述(1)以及(2)。
(1)一种薄膜形成用原料,其由含有本发明的醇盐化合物的前体本身构成,所述醇盐化合物与除了所述醇盐化合物以外的前体的比率是,相对于前者1摩尔,后者为0~10摩尔,在薄膜制造时,通过气体输送法或液体输送法来进行输送供给。
(2)一种薄膜形成用原料,其含有包含本发明的醇盐化合物的前体以及有机溶剂,包含所述醇盐化合物的前体的含量为0.01~2.0摩尔/升,所述醇盐化合物与除了所述醇盐化合物以外的前体的比率是,相对于前者1摩尔,后者为0~10摩尔,在薄膜制造时,通过液体输送法来进行输送供给。
对于作为化学气相沉积法用原料使用时的本发明的薄膜形成用原料,下面进一步详述。
作为上述的输送供给方法,有下述方法:在原料容器中通过将化学气相沉积法用原料加热和/或减压而使其气化,并与根据需要使用的氩气、氮气、氦气等载气一起导入至沉积反应部的气体输送法;将化学气相沉积法用原料以液体或溶液的状态输送至气化室,在气化室通过加热和/或减压而使其气化,然后导入至沉积反应部的液体输送法。在气体输送法中,上述通式(I)表示的醇盐化合物本身成为化学气相沉积用原料,在液体输送法中,上述通式(I)表示的醇盐化合物本身或将该化合物溶解于有机溶剂中而得到的溶液成为化学气相沉积法用原料。
另外,在多成分体系的化学气相沉积法中,包括以各成分独立的方式将化学气相沉积法用原料进行气化、供给的方法(以下有时也记为单源法);以及预先以期望的组成混合多成分原料,并将得到的混合原料进行气化、供给的方法(以下有时也记为混合源法)。在混合源法中,仅由二种以上的本发明的醇盐化合物形成的混合物或混合溶液、一种以上的本发明的镍醇盐化合物与一种以上的其它前体形成的混合物或混合溶液是化学气相沉积法用原料。将本发明的醇盐化合物与其它前体形成的混合物或混合溶液制成化学气相沉积法用原料时,两者的混合比率可以根据所期望的薄膜组成来适当选择,但一般是相对于本发明的醇盐化合物1摩尔,其它前体优选从0.01~10摩尔的范围内选择,更优选从0.1~5摩尔的范围内选择。
作为上述的CVD用原料所使用的有机溶剂,可以不受特别限制地使用众所周知的一般的有机溶剂。作为该有机溶剂,可以列举出例如乙酸乙酯、乙酸丁酯、乙酸甲氧基乙酯等乙酸酯类;乙二醇单甲醚、乙二醇单乙醚、乙二醇单丁基醚、二甘醇单甲醚等醚醇类;四氢呋喃、四氢吡喃、乙二醇二甲醚、二甘醇二甲醚、三甘醇二甲醚、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,它们可以根据溶质的溶解性、使用温度与沸点、闪点的关系等,单独使用或作为二种以上的混合溶剂使用。使用这些有机溶剂时,该有机溶剂中的本发明的醇盐化合物和其它的前体的总量优选为0.01~2.0摩尔/升,特别优选为0.05~1.0摩尔/升。
另外,在使用多成分体系的CVD法的情况下,作为与本发明的醇盐化合物一起使用的其它的前体,没有特别限制,可以使用在CVD用原料中使用的众所周知的一般的前体。
作为上述的其它的前体,可以列举出选自醇化合物、二醇化合物、β-二酮化合物、环戊二烯化合物以及有机胺化合物等中的一种或二种以上的有机配位化合物与硅或金属形成的化合物。另外,作为前体的金属种,可以列举出镁、钙、锶、钡、钛、锆、铪、钒、铌、钽、铬、钼、钨、锰、铁、钌、钴、铑、铱、镍、钯、铂、铜、银、金、锌、铝、镓、铟、锗、锡、铅、锑、铋、钇、镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱。
作为上述的有机配位化合物使用的醇化合物,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;提供本发明的醇盐化合物的二烷基氨基醇。
作为上述的有机配位化合物使用的二醇化合物,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。
作为上述的有机配位化合物使用的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。
作为上述的有机配位化合物使用的环戊二烯化合物,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,作为有机配位化合物使用的有机胺化合物,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、乙基甲胺、丙基甲胺、异丙基甲胺等。
在使用单源法的情况下,上述的其它的前体优选为与本发明的醇盐化合物的热和/或氧化分解的行为相类似的化合物,在使用混合源法的情况下,优选除了热和/或氧化分解的行为相类似以外,混合时还不会因化学反应而变质的化合物。
另外,本发明的薄膜形成用原料中,根据需要为了赋予本发明的醇盐化合物以及其它前体的稳定性,还可以含有亲核性试剂。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-冠醚-6、二环己基-18-冠醚-6、24-冠醚-8、二环己基-24-冠醚-8、二苯并-24-冠醚-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,四氮杂环十四烷(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,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,这些作为稳定剂的亲核性试剂的使用量是,相对于前体1摩尔优选为0.1摩尔~10摩尔的范围,更优选为1~4摩尔。
本发明的薄膜形成用原料中,要尽量避免含有构成其的成分以外的杂质金属元素成分、杂质氯等杂质卤素成分以及杂质有机成分。杂质金属元素成分优选每种元素为100ppb以下,更优选为10ppb以下,总量优选为1ppm以下,更优选为100ppb以下。特别是,作为LSI的栅极绝缘膜、栅极膜、阻挡层使用时,必须减少对所得到的薄膜的电特性有影响的碱金属元素、碱土类金属元素、以及同族元素的含量。杂质卤素成分优选为100ppm以下,更优选为10ppm以下,进一步优选为1ppm以下。杂质有机成分的总量优选为500ppm以下,更优选为50ppm以下,进一步优选为10ppm以下。另外,水分会引起化学气相沉积用原料中的粒子发生、以及薄膜形成中的粒子发生,所以对于金属化合物、有机溶剂以及亲核性试剂,为了减少各自的水分,在使用时最好预先尽可能地除去水分。金属化合物、有机溶剂以及亲核性试剂各自的水分量优选为10ppm以下,更优选为1ppm以下。
另外,本发明的薄膜形成用原料优选尽量不含粒子,以减少或防止所形成的薄膜的粒子污染。具体地,在液相中的利用光散射式液中粒子检测器进行的粒子测定中,优选大于0.3μm的粒子的数量在液相1ml中为100个以下,更优选大于0.2μm的粒子的数量在液相1ml中为1000个以下,进一步优选大于0.2μm的粒子的数量在液相1ml中为100个以下。
下面对使用本发明的薄膜形成用原料作为化学气相沉积法用原料使用时的使用方法(薄膜制造方法)进行具体说明。该薄膜制造方法基于下述的化学气相沉积法来进行:将使本发明的醇盐化合物和根据需要使用的其它前体气化而得到的蒸汽、以及根据需要使用的反应性气体导入至基板上,然后,使前体在基板上发生分解和/或反应,从而使薄膜在基板上生长、沉积。在化学气相沉积法的过程中,可以使用催化剂,有关原料的输送供给方法、沉积方法、制造条件、制造装置等,不受特别限制,可以使用众所周知的一般的条件、方法。
作为上述的根据需要使用的反应性气体,例如作为氧化性的气体,可以列举出氧、臭氧、二氧化氮、一氧化氮、水蒸汽、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、氨或有机金属化合物等,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,作为上述催化剂,可以列举出钨等高熔点金属。
另外,作为上述的输送供给方法,可以列举出前面记载的气体输送法、液体输送法、单源法、混合源法等。
另外,作为上述的沉积方法,可以列举出仅通过热使原料气体或原料气体和反应性气体反应并使薄膜沉积的热CVD法、使用热和等离子体的等离子体CVD法、使用热和光的光CVD法、使用热、光以及等离子体的光等离子体CVD法、将CVD法的沉积反应分为基本反应,以分子水平阶段性地进行沉积的ALD。
另外,作为上述的制造条件,可以列举出反应温度(基板温度)、反应压力、沉积速度等。有关反应温度,优选为本发明的醇盐化合物能够充分反应的温度即100℃以上,更优选为150℃~300℃。另外,反应压力在热CVD、光CVD的情况下,优选为大气压~10Pa,使用等离子体的情况下,优选为2000Pa~10Pa。
另外,沉积速度可以通过原料的供给条件(气化温度、气化压力)、反应温度、反应压力来控制。沉积速度如果大的话,得到的薄膜的特性有可能恶化,如果小的话,生产率有可能发生问题,所以优选为0.01~5000nm/分钟,更优选为0.1~1000nm/分钟。另外,使用ALD时,可以以获得所期望的膜厚的方式通过循环的次数来进行控制。
例如,当使用CVD法来形成镍薄膜时,首先,如上所述,使本发明的醇盐化合物和根据需要使用的其它前体气化,将得到的蒸汽、以及根据需要使用的反应性气体导入至基板上(原料导入工序)。本发明的醇盐化合物优选在室温~200℃下蒸发。另外,使本发明的醇盐化合物蒸发时的压力优选为0.01~300Pa。在前面说明的原料导入工序的下面,使导入至沉积反应部的镍醇盐化合物在基体上形成前体薄膜(前体薄膜成膜工序)。此时,可以通过加热基体或加热沉积反应部来施加热。在该工序中成膜的前体薄膜是镍薄膜、或一部分镍醇盐化合物分解和/或反应而生成的薄膜,与目标的镍薄膜具有不同的组成。本工序进行的温度优选为室温~400℃,更优选为150~300℃。
接着,从沉积反应部排出未反应的镍醇盐化合物气体以及副生成的气体(排气工序)。未反应的镍醇盐化合物气体以及副生成的气体从沉积反应部完全排出是理想的情况,但也未必需要完全排出。作为排气方法,可以列举出用氦气、氩气等惰性气体来吹扫体系内的方法、通过将体系内减压来进行排气的方法、将它们组合的方法等。减压时的减压度优选为0.01~300Pa,更优选为0.1~100Pa。
接着,将还原性气体导入至沉积反应部,通过该还原性气体、或氧化性气体和热的作用,由在前面的前体薄膜成膜工序中而得到前体薄膜形成镍薄膜(镍薄膜形成工序)。在本工序中,使热作用时的温度优选为室温~400℃,更优选为150~300℃。本发明的醇盐化合物与还原性气体的反应性良好,可以得到镍薄膜。
将由上述的原料导入工序、前体薄膜成膜工序、排气工序、以及镍薄膜形成工序构成的一连串操作的薄膜沉积设定为1个循环,可以反复进行多次该循环,直到得到所需膜厚的薄膜为止(ALD法)。此时,进行1个循环后,优选与上述排气工序同样地从沉积反应部排出未反应的镍醇盐化合物气体和还原性气体、以及副生成的气体之后,再进行下一个循环。
另外,在利用ALD法进行镍薄膜的形成中,也可以施加等离子体、光、电压等能量。施加这些能量的时期没有特别限定,例如,可以是在原料导入工序的镍醇盐化合物气体导入时、前体薄膜成膜工序或镍薄膜形成工序的加温时、排气工序的体系内的排气时、镍薄膜形成工序的还原性气体导入时,也可以是上述的各工序之间。
另外,使用本发明的薄膜形成用原料制作薄膜时,薄膜沉积后,为了获得更良好的电特性,可以在惰性气氛下、氧化性气氛下或还原性气氛下进行退火处理,需要阶梯覆盖时,还可以设置回流工序。此时的温度为250~1000℃,优选为300~500℃。
使用本发明的薄膜形成用原料制造的薄膜通过适当选择其它成分的前体、反应性气体以及制造条件,由此可以制成金属、氧化物陶瓷、氮化物陶瓷、玻璃等所期望的种类的薄膜。作为制造的薄膜的组成,可以列举出例如金属镍、镍系氧化物、镍系氮化物、以及Ni-Ti、Ni-Cr、Ni-V、Ni-Cu、Ni-Cr-Si、Ni-Cr-Al、Ni-W、AuGeNi和NiP2等镍系合金等,作为它们的用途,可以列举出电极膜、阻挡膜、电阻膜、磁性膜、液晶用阻挡金属膜、薄膜太阳电池用构件、半导体装置用构件、纳米结构体、储氢合金以及微小电气机械传动装置等。
实施例
下面,通过实施例更详细地说明本发明。但是,本发明不受以下实施例等的任何限制。
[实施例1]化合物No.1的制造
在氩气气氛下,向反应烧瓶中加入六氨合镍(II)氯化物12.77g、脱水处理后的甲苯40.37g,在室温下搅拌。在室温下向其中缓慢加入在脱水处理后的甲苯68.70g中溶解有1-(N,N-二甲基氨基)-2-丁氧基钠15.17g而得到的溶液。然后,回流大约8小时后进行过滤。从得到的滤液中除去甲苯,得到固体残渣。使该固体残渣在150Pa的减压下于120℃升华,得到绿色固体。该精制的回收率为60%。得到的绿色固体的熔点为84℃,元素分析和1H-NMR分析的结果确认是目标化合物的化合物No.1。上述的分析结果如下所示。以下,TG-DTA的结果也一并表示。
(分析值)
(1)元素分析(金属分析:ICP-AES、氯分析:TOX)
镍:17.1质量%(理论值20.2%)、Na:低于1ppm、Cl:低于1ppm
C:45.2质量%、H:9.1质量%、N:9.0质量%(理论值:C:49.5%、H:9.7%、N:9.6%)
(2)1H-NMR(溶剂:氘代苯)(化学位移:多重态:H数)
(0.99:t:3)(1.28:m:2)(1.42:m:1)(2.0:m:4)(2.53:d:3)(3.32:m:1)
(3)TG-DTA(Ar100ml/min、10℃/min升温、样品量9.172mg)
50质量%减少温度为183℃
[实施例2]化合物No.3的制造
在氩气气氛下,向反应烧瓶中加入六氨合镍(II)氯化物12.54g、脱水处理后的甲苯36.27g,在室温下搅拌。在室温下向其中缓慢加入在脱水处理后的甲苯52.46g中溶解有1-(N,N-二甲基氨基)-2-六氧化钠18.06g而得到的溶液。然后,回流大约8小时后进行过滤。从得到的滤液中除去甲苯,得到固体残渣。使该固体残渣在150Pa的减压下于140℃升华,得到绿色固体。该精制的回收率为68%。得到的绿色固体的熔点为96℃,元素分析和1H-NMR分析的结果确认是目标化合物的化合物No.3。上述的分析结果如下所示。以下,TG-DTA的结果也一并表示。
(分析值)
(1)元素分析(金属分析:ICP-AES、氯分析:TOX)
镍:15.5质量%(理论值16.9%)、Na:低于1ppm、Cl:低于1ppm
C:50.2质量%、H:9.9质量%、N:9.5质量%(理论值:C:55.4%、H:10.5%、N:8.1%)
(2)1H-NMR(溶剂:氘代苯)(化学位移:多重态:H数)
(0.95:t:3)(1.39:m:6)(1.55:m:3)(1.99:m:1)(2.24:m:4)(2.54:d:3)(3.40:m:1)
(3)TG-DTA(Ar100ml/min、10℃/min升温、样品量9.439mg)
50质量%减少温度为223℃
[实施例3]化合物No.4的制造
在氩气气氛下,向反应烧瓶中加入六氨合镍(II)氯化物125.13g、脱水处理后的甲苯638g,在室温下搅拌。在室温下向其中缓慢加入在脱水处理后的甲苯241.5g中溶解有1-(N,N-乙基甲基氨基)-2-丁氧基钠165.30g而得到的溶液。然后,回流大约8小时后进行过滤。从得到的滤液中除去甲苯,得到液体残渣。减压蒸馏该液体残渣,分级100Pa、塔顶温度为105~106℃的馏分,得到深绿色液体。该精制的回收率为80%。元素分析和1H-NMR分析的结果确认得到的深绿色液体是目标化合物的化合物No.4。上述的分析结果如下所示。以下,TG-DTA的结果也一并表示。
(分析值)
(1)元素分析(金属分析:ICP-AES、氯分析:TOX)
C:46.5质量%、H:9.6质量%、N:8.5质量%(理论值:C:52.7%、H:10.1%、N:8.8%)
Ni:17.8质量%(理论值18.4%)
(2)1H-NMR(溶剂:氘代苯)(化学位移:多重态:H数)
得到的NMR图示于图1中。
(3)TG-DTA(Ar100ml/min、10℃/min升温、样品量10.796mg)
50质量%减少温度为195℃
[实施例4]化合物No.7的制造
在氩气气氛下,向反应烧瓶中加入六氨合镍(II)氯化物12.55g、脱水处理后的甲苯42.64g,在室温下搅拌。在室温下向其中缓慢加入在脱水处理后的甲苯61.2g中溶解有1-(N,N-二乙基氨基)-2-丁氧基钠18.06g而得到的溶液。然后,回流大约8小时后进行过滤。从得到的滤液中除去甲苯,得到液体残渣。减压蒸馏该液体残渣,分级120Pa、塔顶温度为102~103℃的馏分,得到深绿色液体。该精制的回收率为66%。元素分析和1H-NMR分析的结果确认得到的深绿色液体是目标化合物的No.7。上述的分析结果如下所示。以下,TG-DTA的结果也一并表示。
(分析值)
(1)元素分析(金属分析:ICP-AES、氯分析:TOX)
C:45.5质量%、H:9.1质量%、N:6.5质量%(理论值:C:55.4%、H:10.5%、N:8.1%)
Ni:16.4质量%(理论值:16.9%)
(2)1H-NMR(溶剂:氘代苯)(化学位移:多重态:H数)
得到的NMR图示于图2中。
(3)TG-DTA(Ar100ml/min、10℃/min升温、样品量10.568mg)
50质量%减少温度为206℃
镍化合物的物性评价
对上述实施例1~4中分别得到的化合物No.1(实施例1)、No.3(实施例2)、No.4(实施例3)、No.7(实施例4)以及下述所示的比较化合物1(比较例1)、2(比较例2),通过目视观察常温常压下的化合物的状态,对于固体化合物,使用微小熔点测定装置测定熔点,并且测定各化合物的沸点。结果示于表1中。
[表1]
化合物 | 状态 | 熔点 | 沸点 | |
实施例1 | 化合物No.1 | 固体 | 84℃ | 120℃/150Pa |
实施例2 | 化合物No.3 | 固体 | 96℃ | 140℃/150Pa |
实施例3 | 化合物No.4 | 液体 | — | 105℃/100Pa |
实施例4 | 化合物No.7 | 液体 | — | 102℃/120Pa |
比较例1 | 比较化合物1 | 固体 | 118~119℃ | 100℃/100Pa※1 |
比较例2 | 比较化合物2 | 固体 | 147℃ | 100℃/80Pa※1 |
※1尝试了试验,但无法经由液体状态,发生了升华。
由上述表1确认了:比较例1、2是熔点超过100℃的固体,与此相对,实施例1、2、3、4是液体或通过稍稍加热就成为液体的低熔点的化合物。
另外可知,比较例1、2的固体化合物的升华性较高,作为化学气相沉积用原料使用时,难以稳定地以液体状态供给原料。这种升华性较高的化合物在化学气相沉积法中的向基体导入化学气相沉积用原料的导入工序中,该原料向基材的供给量的控制明显困难。本发明的醇盐化合物由于在常温下是液体或通过稍稍加热就成为液体,所以在化学气相沉积法中的向基体导入化学气相沉积用原料的导入工序中,能够将该原料稳定地供给至基体以及供给量的控制性容易,在这些方面是有利的。
由上述结果确认了:本发明的醇盐化合物适合用作薄膜形成用原料。
Claims (6)
1.一种醇盐化合物,其由下述通式(I)表示,
式中,R1表示乙基,R2、R3表示碳原子数为1~4的直链或支链状烷基,且R2和R3中的任一者或两者为乙基。
2.根据权利要求1所述的醇盐化合物,其是薄膜形成用原料。
3.一种薄膜形成用原料,其含有权利要求1所述的醇盐化合物。
4.根据权利要求3所述的薄膜形成用原料,其用作化学气相沉积法用原料。
5.根据权利要求4所述的薄膜形成用原料,其中,所述薄膜形成用原料由含有所述醇盐化合物的前体本身构成,所述醇盐化合物与除了所述醇盐化合物以外的前体的比率是,相对于前者1摩尔,后者为0~10摩尔,在薄膜制造时,通过气体输送法或液体输送法来输送供给所述薄膜形成用原料。
6.根据权利要求4所述的薄膜形成用原料,其中,所述薄膜形成用原料含有包含所述醇盐化合物的前体以及有机溶剂,包含所述醇盐化合物的前体的含量为0.01~2.0摩尔/升,所述醇盐化合物与除了所述醇盐化合物以外的前体的比率是,相对于前者1摩尔,后者为0~10摩尔,在薄膜制造时,通过液体输送法来输送供给所述薄膜形成用原料。
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