JP6760822B2 - 化合物、薄膜形成用原料、原子層堆積法用の薄膜形成用原料及び薄膜の製造方法 - Google Patents
化合物、薄膜形成用原料、原子層堆積法用の薄膜形成用原料及び薄膜の製造方法 Download PDFInfo
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- JP6760822B2 JP6760822B2 JP2016218054A JP2016218054A JP6760822B2 JP 6760822 B2 JP6760822 B2 JP 6760822B2 JP 2016218054 A JP2016218054 A JP 2016218054A JP 2016218054 A JP2016218054 A JP 2016218054A JP 6760822 B2 JP6760822 B2 JP 6760822B2
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- 239000010409 thin film Substances 0.000 title claims description 202
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- 230000015572 biosynthetic process Effects 0.000 title description 15
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- 238000004519 manufacturing process Methods 0.000 claims description 48
- 239000002243 precursor Substances 0.000 claims description 47
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 33
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- NGAZZOYFWWSOGK-UHFFFAOYSA-N heptan-3-one Chemical compound CCCCC(=O)CC NGAZZOYFWWSOGK-UHFFFAOYSA-N 0.000 description 2
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- DGCTVLNZTFDPDJ-UHFFFAOYSA-N heptane-3,5-dione Chemical compound CCC(=O)CC(=O)CC DGCTVLNZTFDPDJ-UHFFFAOYSA-N 0.000 description 2
- SDAXRHHPNYTELL-UHFFFAOYSA-N heptanenitrile Chemical compound CCCCCCC#N SDAXRHHPNYTELL-UHFFFAOYSA-N 0.000 description 2
- 150000002391 heterocyclic compounds Chemical class 0.000 description 2
- NDOGLIPWGGRQCO-UHFFFAOYSA-N hexane-2,4-dione Chemical compound CCC(=O)CC(C)=O NDOGLIPWGGRQCO-UHFFFAOYSA-N 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 2
- LSHROXHEILXKHM-UHFFFAOYSA-N n'-[2-[2-[2-(2-aminoethylamino)ethylamino]ethylamino]ethyl]ethane-1,2-diamine Chemical compound NCCNCCNCCNCCNCCN LSHROXHEILXKHM-UHFFFAOYSA-N 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 2
- WSGCRAOTEDLMFQ-UHFFFAOYSA-N nonan-5-one Chemical compound CCCCC(=O)CCCC WSGCRAOTEDLMFQ-UHFFFAOYSA-N 0.000 description 2
- 239000012434 nucleophilic reagent Substances 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- BTNXBLUGMAMSSH-UHFFFAOYSA-N octanedinitrile Chemical compound N#CCCCCCCC#N BTNXBLUGMAMSSH-UHFFFAOYSA-N 0.000 description 2
- 125000001181 organosilyl group Chemical group [SiH3]* 0.000 description 2
- OOFGXDQWDNJDIS-UHFFFAOYSA-N oxathiolane Chemical compound C1COSC1 OOFGXDQWDNJDIS-UHFFFAOYSA-N 0.000 description 2
- 238000006864 oxidative decomposition reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000009832 plasma treatment Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 2
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 2
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 2
- 238000000427 thin-film deposition Methods 0.000 description 2
- 125000005270 trialkylamine group Chemical group 0.000 description 2
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- AVFZOVWCLRSYKC-UHFFFAOYSA-N 1-methylpyrrolidine Chemical compound CN1CCCC1 AVFZOVWCLRSYKC-UHFFFAOYSA-N 0.000 description 1
- 229960000549 4-dimethylaminophenol Drugs 0.000 description 1
- 0 CC1(C)OC*(C)(C)C1 Chemical compound CC1(C)OC*(C)(C)C1 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 description 1
- AHVYPIQETPWLSZ-UHFFFAOYSA-N N-methyl-pyrrolidine Natural products CN1CC=CC1 AHVYPIQETPWLSZ-UHFFFAOYSA-N 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052773 Promethium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 125000004183 alkoxy alkyl group Chemical group 0.000 description 1
- 125000005103 alkyl silyl group Chemical group 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 150000001540 azides Chemical class 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 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
- 239000011651 chromium Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 125000004985 dialkyl amino alkyl group Chemical group 0.000 description 1
- 125000004984 dialkylaminoalkoxy group Chemical group 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- VBCSQFQVDXIOJL-UHFFFAOYSA-N diethylazanide;hafnium(4+) Chemical compound [Hf+4].CC[N-]CC.CC[N-]CC.CC[N-]CC.CC[N-]CC VBCSQFQVDXIOJL-UHFFFAOYSA-N 0.000 description 1
- DWCMDRNGBIZOQL-UHFFFAOYSA-N dimethylazanide;zirconium(4+) Chemical compound [Zr+4].C[N-]C.C[N-]C.C[N-]C.C[N-]C DWCMDRNGBIZOQL-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 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
- 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
- 150000004820 halides Chemical class 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 150000004679 hydroxides Chemical class 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
- 230000010354 integration Effects 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
- 239000003446 ligand Substances 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
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- DWFKOMDBEKIATP-UHFFFAOYSA-N n'-[2-[2-(dimethylamino)ethyl-methylamino]ethyl]-n,n,n'-trimethylethane-1,2-diamine Chemical compound CN(C)CCN(C)CCN(C)CCN(C)C DWFKOMDBEKIATP-UHFFFAOYSA-N 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 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
- 239000000047 product Substances 0.000 description 1
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- ASRAWSBMDXVNLX-UHFFFAOYSA-N pyrazolynate Chemical compound C=1C=C(Cl)C=C(Cl)C=1C(=O)C=1C(C)=NN(C)C=1OS(=O)(=O)C1=CC=C(C)C=C1 ASRAWSBMDXVNLX-UHFFFAOYSA-N 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 229910052705 radium Inorganic materials 0.000 description 1
- HCWPIIXVSYCSAN-UHFFFAOYSA-N radium atom Chemical compound [Ra] HCWPIIXVSYCSAN-UHFFFAOYSA-N 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
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 1
- MNWRORMXBIWXCI-UHFFFAOYSA-N tetrakis(dimethylamido)titanium Chemical compound CN(C)[Ti](N(C)C)(N(C)C)N(C)C MNWRORMXBIWXCI-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
-
- 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
- C07F17/00—Metallocenes
-
- 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
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
-
- 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
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/28—Titanium compounds
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Chemical Vapour Deposition (AREA)
- Formation Of Insulating Films (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
また、堆積速度は、原料の供給条件(気化温度、気化圧力)、反応温度、反応圧力によりコントロールすることができる。堆積速度は、大きいと得られる薄膜の特性が悪化する場合があり、小さいと生産性に問題を生じる場合があるので、0.01〜100nm/分が好ましく、1〜50nm/分がより好ましい。また、ALD法の場合は、所望の膜厚が得られるようにサイクルの回数でコントロールされる。
2000mL4つ口フラスコにAr雰囲気下でテトラキス(ジメチルアミノ)ジルコニウム230.0gと脱水トルエン1190gの混合溶液を氷浴した後、シクロペンタジエン113.7gを等圧滴下漏斗より約1時間かけて滴下して反応させた。引き続き、1−(ジメチルアミノ)−2−メチル−2−プロパノール201.5gを等圧滴下漏斗より約2時間かけて滴下して加えて反応させた。滴下終了後、室温まで徐々に昇温し、さらに2時間反応を継続した。引き続き、減圧下で溶媒を留去した後、減圧蒸留67Pa/145〜7℃の留分を分取し、淡黄色液体の化合物No.4を312g得た。
(1)常圧TG−DTA
質量50%減少温度:271℃(Ar流量:100mL/分、昇温:10℃/分、サンプル量:11.491mg)
(2)元素分析(金属分析:ICP−AES、CHN分析:CHN分析装置)
ジルコニウム含有量:20.05質量%(理論値:20.10質量%)
C:58.0質量%(理論値:58.23質量%)、H:7.9質量%(理論値:8.44質量%)、N:5.8質量%(理論値:6.17質量%)
300mL4つ口フラスコにAr雰囲気下でテトラキス(ジメチルアミノ)チタン19.3gと脱水トルエン118.9gの混合溶液を氷浴した後、シクロペンタジエン12.0gを等圧滴下漏斗より約30時間かけて滴下して反応させた。引き続き、1−(ジメチルアミノ)−2−メチル−2−プロパノール20.2gを等圧滴下漏斗より約1時間かけて滴下して加えて反応させた。滴下終了後、室温まで徐々に昇温し、さらに2時間反応を継続した。引き続き、減圧下で溶媒を留去した後、減圧蒸留を行い淡黄色液体の化合物No.22を28.2g得た。
(1)常圧TG−DTA
質量50%減少温度:272℃(Ar流量:100mL/分、昇温:10℃/分、サンプル量:10.421mg)
(2)元素分析(金属分析:ICP−AES、CHN分析:CHN分析装置)
チタン含有量:11.5質量%(理論値:11.67質量%)
C:64.1質量%(理論値:64.38質量%)、H:8.7質量%(理論値:9.33質量%)、N:6.1質量%(理論値:6.83質量%)
300mL4つ口フラスコにAr雰囲気下でテトラキス(ジエチルアミノ)ハフニウム37.4gと脱水トルエン110.6gの混合溶液を氷浴した後、シクロペンタジエン11.1gを等圧滴下漏斗より約30時間かけて滴下して反応させた。引き続き、1−(ジメチルアミノ)−2−メチル−2−プロパノール18.8gを等圧滴下漏斗より約1時間かけて滴下して加えて反応させた。滴下終了後、室温まで徐々に昇温し、さらに2時間反応を継続した。引き続き、減圧下で溶媒を留去した後、減圧蒸留60Pa/145〜7℃の留分を分取し、淡黄色液体の化合物No.40を34.5g得た。
(1)常圧TG−DTA
質量50%減少温度:258℃(Ar流量:100mL/分、昇温:10℃/分、サンプル量:10.421mg)
(2)元素分析(金属分析:ICP−AES、CHN分析:CHN分析装置)
ハフニウム含有量:32.9質量%(理論値:32.99質量%)
C:48.6質量%(理論値:48.84質量%)、H:6.7質量%(理論値:7.08質量%)、N:4.7質量%(理論値:5.18質量%)
化合物No.4、下記に示す比較化合物1及び比較化合物2について、目視によって常圧30℃における各化合物の状態を観察した。また、落球式粘度計(Anton Paar社製、製品名:AMVn)を用いて、30℃における粘度を測定した。また、比較化合物1及び比較化合物2について、TG−DTAを用いて常圧下で重量が50%減少した際の温度を測定した(Ar流量:100mL/分、昇温:10℃/分、比較化合物1のサンプル量:13.064mg、比較化合物2のサンプル量:12.485mg)。また、不活性ガス雰囲気下において100℃〜300℃まで10℃毎の温度で各々1時間加熱処理したサンプルを用意し、上記加熱処理の温度の低いサンプルから常圧条件下でTG−DTA測定(Ar流量:100mL/分、昇温:10℃/分、測定温度範囲:25℃〜600℃)を順次行った。TG−DTA測定後の残渣の量が2質量%以上となった最初のサンプルの上記加熱処理の温度を「熱分解温度」とした。結果を表1に示す。
化合物No.22、下記に示す比較化合物3について、目視によって常圧30℃における各化合物の状態を観察した。固体化合物については微小融点測定装置を用いて融点を測定した。また、比較化合物3について、TG−DTAを用いて常圧下で重量が50%減少した際の温度を測定した(Ar流量:100mL/分、昇温:10℃/分、サンプル量:8.997mg)。結果を表2に示す。
化合物No.4を化学気相成長用原料とし、図1に示す化学気相成長用装置を用いて以下の条件のALD法により、シリコン基板上に酸化ジルコニウム薄膜を製造した。得られた薄膜について、X線反射率法による膜厚測定、X線回折法及びX線光電子分光法による薄膜構造及び薄膜組成の確認を行ったところ、膜厚は2〜4nmであり、膜組成は酸化ジルコニウム(XPS分析によるZr4dピークで確認)であり、薄膜中の残留炭素含有量は検出下限である0.1atom%よりも少なかった。1サイクル当たりに得られる膜厚は、0.02〜0.04nmであった。
反応温度(基板温度);250℃、反応性ガス;オゾン
(工程)
下記(1)〜(4)からなる一連の工程を1サイクルとして、100サイクル繰り返した。
(1)原料容器加熱温度:150℃、原料容器内圧力:80Pa以下の条件で気化させた化学気相成長用原料を成膜チャンバーに導入し、系圧力:80Paで10秒間堆積させる。
(2)10秒間のアルゴンパージにより、未反応原料及び副生ガスを除去する。
(3)反応性ガスを成膜チャンバーに導入し、系圧力:80Paで10秒間反応させる。
(4)10秒間のアルゴンパージにより、未反応原料及び副生ガスを除去する。
比較化合物2(Zr(DMAMP)4)を化学気相成長用原料とし、図1に示す化学気相成長用装置を用いて以下の条件のALD法により、シリコン基板上に酸化ジルコニウム薄膜を製造した。得られた薄膜について、X線反射率法による膜厚測定、X線回折法及びX線光電子分光法による薄膜構造及び薄膜組成の確認を行ったところ、膜厚は1nmであり、膜組成は酸化ジルコニウム(XPS分析によるZr4dピークで確認)であり、薄膜中の残留炭素含有量は5atom%であった。1サイクル当たりに得られる膜厚は、0.01nmであった。
反応温度(基板温度);280℃、反応性ガス;オゾン
(工程)
下記(1)〜(4)からなる一連の工程を1サイクルとして、100サイクル繰り返した。
(1)原料容器加熱温度:150℃、原料容器内圧力:80Pa以下の条件で気化させた化学気相成長用原料を成膜チャンバーに導入し、系圧力:80Paで10秒間堆積させる。
(2)10秒間のアルゴンパージにより、未反応原料及び副生ガスを除去する。
(3)反応性ガスを成膜チャンバーに導入し、系圧力:80Paで10秒間反応させる。
(4)10秒間のアルゴンパージにより、未反応原料及び副生ガスを除去する。
化合物No.22を化学気相成長用原料とし、図1に示す化学気相成長用装置を用いて以下の条件のALD法により、シリコン基板上に酸化チタン薄膜を製造した。得られた薄膜について、X線反射率法による膜厚測定、X線回折法及びX線光電子分光法による薄膜構造及び薄膜組成の確認を行ったところ、膜厚は3〜4nmであり、膜組成は酸化チタン(XPS分析によるTi3dピークで確認)であり、薄膜中の残留炭素含有量は検出下限である0.1atom%よりも少なかった。1サイクル当たりに得られる膜厚は、0.03〜0.04nmであった。
反応温度(基板温度);300℃、反応性ガス;オゾン
(工程)
下記(1)〜(4)からなる一連の工程を1サイクルとして、100サイクル繰り返した。
(1)原料容器加熱温度:160℃、原料容器内圧力:80Pa以下の条件で気化させた化学気相成長用原料を成膜チャンバーに導入し、系圧力:80Paで10秒間堆積させる。
(2)10秒間のアルゴンパージにより、未反応原料及び副生ガスを除去する。
(3)反応性ガスを成膜チャンバーに導入し、系圧力:80Paで10秒間反応させる。
(4)10秒間のアルゴンパージにより、未反応原料及び副生ガスを除去する。
化合物No.40を化学気相成長用原料とし、図1に示す化学気相成長用装置を用いて以下の条件のALD法により、シリコン基板上に酸化ハフニウム薄膜を製造した。得られた薄膜について、X線反射率法による膜厚測定、X線回折法及びX線光電子分光法による薄膜構造及び薄膜組成の確認を行ったところ、膜厚は2〜4nmであり、膜組成は酸化ハフニウム(XPS分析によるHf4fピークで確認)であり、薄膜中の残留炭素含有量は検出下限である0.1atom%よりも少なかった。1サイクル当たりに得られる膜厚は、0.02〜0.04nmであった。
反応温度(基板温度);300℃、反応性ガス;オゾン
(工程)
下記(1)〜(4)からなる一連の工程を1サイクルとして、100サイクル繰り返した。
(1)原料容器加熱温度:150℃、原料容器内圧力:80Pa以下の条件で気化させた化学気相成長用原料を成膜チャンバーに導入し、系圧力:80Paで10秒間堆積させる。
(2)10秒間のアルゴンパージにより、未反応原料及び副生ガスを除去する。
(3)反応性ガスを成膜チャンバーに導入し、系圧力:80Paで10秒間反応させる。
(4)10秒間のアルゴンパージにより、未反応原料及び副生ガスを除去する。
Claims (8)
- 前記一般式(1)において、R 1 〜R 5 のすべてが水素であるか又はR 1 〜R 5 のうち1つがメチル基であり且つ残りの4つが水素であり、R 6 及びR 7 はメチル基又はエチル基であり、R 8 及びR 9 はメチル基又はエチル基である請求項1に記載の化合物。
- 請求項1又は2に記載の化合物を含有してなる薄膜形成用原料。
- 請求項3に記載の薄膜形成用原料を気化させて得られる化合物を含有する蒸気を、基体が設置された成膜チャンバー内に導入し、該化合物を分解及び/又は化学反応させて該基体の表面にジルコニウム原子又はチタン原子を含有する薄膜を形成する薄膜の製造方法。
- 前記一般式(2)において、R 11 〜R 15 のすべてが水素であるか又はR 11 〜R 15 のうち1つがメチル基であり且つ残りの4つが水素であり、R 16 及びR 17 はメチル基又はエチル基であり、R 18 及びR 19 はメチル基又はエチル基である請求項5に記載の薄膜形成用原料。
- 原子層堆積法による、ジルコニウム原子、ハフニウム原子及びチタン原子から選ばれる少なくとも1種の原子を含有する薄膜の製造方法であって、
請求項5又は6に記載の薄膜形成用原料を気化させて得られる化合物を含有する蒸気を、基体が設置された成膜チャンバー内に導入し、該基体の表面に前駆体薄膜を形成する工程と、
未反応の化合物ガス及び副生したガスを該成膜チャンバーから排気する工程と、
反応性ガスを該成膜チャンバー内に導入し、該前駆体薄膜を該反応性ガスと反応させて該基体の表面にジルコニウム原子、ハフニウム原子及びチタン原子から選ばれる少なくとも1種の原子を含有する薄膜を形成する工程と
を有する薄膜の製造方法。 - 前記反応性ガスがオゾンであり、前記基体が150〜350℃に加熱されている請求項7に記載の薄膜の製造方法。
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