KR101639432B1 - Cvd 전구체 - Google Patents
Cvd 전구체 Download PDFInfo
- Publication number
- KR101639432B1 KR101639432B1 KR1020167005023A KR20167005023A KR101639432B1 KR 101639432 B1 KR101639432 B1 KR 101639432B1 KR 1020167005023 A KR1020167005023 A KR 1020167005023A KR 20167005023 A KR20167005023 A KR 20167005023A KR 101639432 B1 KR101639432 B1 KR 101639432B1
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- KR
- South Korea
- Prior art keywords
- feed gas
- bisaminosilacyclobutane
- silicon
- film
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- Prior art date
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- 239000002243 precursor Substances 0.000 title claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 17
- 239000010703 silicon Substances 0.000 claims abstract description 17
- RWRDLPDLKQPQOW-UHFFFAOYSA-N Pyrrolidine Chemical compound C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 claims description 9
- PASYEMKYRSIVTP-UHFFFAOYSA-N 1,1-dichlorosiletane Chemical compound Cl[Si]1(Cl)CCC1 PASYEMKYRSIVTP-UHFFFAOYSA-N 0.000 claims description 7
- OSYHQGGOLYJONU-UHFFFAOYSA-N 1-(1-pyrrolidin-1-ylsiletan-1-yl)pyrrolidine Chemical compound C1CC[Si]1(N1CCCC1)N1CCCC1 OSYHQGGOLYJONU-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 abstract description 53
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 52
- 239000010408 film Substances 0.000 abstract description 36
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 19
- 239000001301 oxygen Substances 0.000 abstract description 19
- 229910052760 oxygen Inorganic materials 0.000 abstract description 19
- 238000000034 method Methods 0.000 abstract description 13
- 239000000203 mixture Substances 0.000 abstract description 12
- 239000004065 semiconductor Substances 0.000 abstract description 12
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 9
- 239000000377 silicon dioxide Substances 0.000 abstract description 9
- 238000000576 coating method Methods 0.000 abstract description 8
- 229910052581 Si3N4 Inorganic materials 0.000 abstract description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 abstract description 7
- 239000003989 dielectric material Substances 0.000 abstract description 6
- 239000010409 thin film Substances 0.000 abstract description 6
- 230000004888 barrier function Effects 0.000 abstract description 4
- 238000002161 passivation Methods 0.000 abstract description 4
- 125000006850 spacer group Chemical group 0.000 abstract description 3
- 238000012719 thermal polymerization Methods 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 description 11
- INPQQHDZNUWYDS-UHFFFAOYSA-N 1-n,1-n'-ditert-butylsiletane-1,1-diamine Chemical compound CC(C)(C)N[Si]1(NC(C)(C)C)CCC1 INPQQHDZNUWYDS-UHFFFAOYSA-N 0.000 description 10
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 10
- 238000000151 deposition Methods 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 7
- 230000008021 deposition Effects 0.000 description 7
- 239000012528 membrane Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 5
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 5
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 238000005979 thermal decomposition reaction Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 238000005481 NMR spectroscopy Methods 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000000113 differential scanning calorimetry Methods 0.000 description 3
- 125000000031 ethylamino group Chemical group [H]C([H])([H])C([H])([H])N([H])[*] 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000012263 liquid product Substances 0.000 description 3
- 239000012066 reaction slurry Substances 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- DVHMVRMYGHTALQ-UHFFFAOYSA-N silylhydrazine Chemical group NN[SiH3] DVHMVRMYGHTALQ-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 238000000231 atomic layer deposition Methods 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- JUINSXZKUKVTMD-UHFFFAOYSA-N hydrogen azide Chemical compound N=[N+]=[N-] JUINSXZKUKVTMD-UHFFFAOYSA-N 0.000 description 2
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 2
- JSHASCFKOSDFHY-UHFFFAOYSA-N CCCCN1CCCC1 Chemical compound CCCCN1CCCC1 JSHASCFKOSDFHY-UHFFFAOYSA-N 0.000 description 1
- AVFZOVWCLRSYKC-UHFFFAOYSA-N CN1CCCC1 Chemical compound CN1CCCC1 AVFZOVWCLRSYKC-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- FCLZCOCSZQNREK-UHFFFAOYSA-N Pyrrolidine, hydrochloride Chemical compound Cl.C1CCNC1 FCLZCOCSZQNREK-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 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 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- XWBDWHCCBGMXKG-UHFFFAOYSA-N ethanamine;hydron;chloride Chemical compound Cl.CCN XWBDWHCCBGMXKG-UHFFFAOYSA-N 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- KCWYOFZQRFCIIE-UHFFFAOYSA-N ethylsilane Chemical compound CC[SiH3] KCWYOFZQRFCIIE-UHFFFAOYSA-N 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- -1 fluorine Chemical class 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000003988 headspace gas chromatography Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 125000006038 hexenyl group Chemical group 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- DLDIDQIZPBIVNQ-UHFFFAOYSA-N hydron;2-methylpropan-2-amine;chloride Chemical compound Cl.CC(C)(C)N DLDIDQIZPBIVNQ-UHFFFAOYSA-N 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000005891 transamination reaction Methods 0.000 description 1
- 238000007740 vapor deposition Methods 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
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- 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
- C23C16/401—Oxides containing silicon
- C23C16/402—Silicon dioxide
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- 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
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/62—Plasma-deposition of organic layers
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- 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
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- 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
- C23C16/34—Nitrides
- C23C16/345—Silicon nitride
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- 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
- C23C16/36—Carbonitrides
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- 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
- C23C16/401—Oxides containing silicon
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- 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
- C23C16/42—Silicides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
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- 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
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
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Abstract
비스아미노실라시클로부탄, 및 질소 공급 가스, 산소 공급 가스 및 이들의 혼합물로부터 선택된 공급 가스를 포함하는 반응성 가스 혼합물의 열 중합에 의해 규소 함유 박막을 생성시키는 방법이 기술된다. 증착된 막은, 질화규소, 실리콘 카보니트라이드, 이산화규소 또는 탄소 도핑된 이산화규소일 수 있다. 이들 막은 반도체 장치에서 유전체, 패시베이션 코팅, 배리어 코팅, 스페이서, 라이너 및/또는 스트레서(stressor)로 유용하다.
Description
이산화규소 및 탄소 도핑된 산화규소의 박막은 반도체 장치의 제조에서 사용되는 일반적인 유전체이다. 저온에서 이들 물질의 박막을 증착시키는 것은 전형적으로 플라즈마 증강된 화학적 기상 증착(PECVD) 공정을 이용하여 실시된다. 그러나, 트랜지스터에 대한 잠재적인 플라즈마 손상에 대한 우려 때문에, 몇몇의 환경에서는 저온 공정이 선호된다.
열 질화규소 또는 실리콘 카보니트라이드(silicon carbonitride)는 반도체 장치에서 유전체, 패시베이션 코팅(passivation coating), 배리어 코팅, 스페이서, 라이너 또는 스트레서(stressor)로 사용되어 왔다. 장치 내에서 감열성(heat sensitive) 성분 및 한정된 열적 비용에 의해 제한되기 때문에, 반도체 제작 산업은 감소되는 온도에서 상기한 막을 증착시킬 수 있는 새로운 전구체를 모색하고 있다. 막 증착 온도는 덩어리 생성이 시작되는 경우에 22nm 테크 노드(tech node)에서 400 내지 450℃만큼 낮을 수 있을 것으로 예측된다. 막을 그러한 낮은 온도에서 증착시킬 수 있기 위해서, 전구체는 대략 200℃에서 분해되어야 하면서도, 상기 전구체는 여전히 저장 안정성에 대한 요건을 충족해야 한다. 아마도 지금까지는 그러한 낮은 열 분해 온도 및 양호한 저장성을 갖는 것으로 입증된 유일한 실란 전구체는 에어 프로덕츠(Air Products) 사에 의해 개발된 히드라지노실란이다. 비스(1,1-디메틸히드라지노)에틸실란, HEtSi(NH-NMe2)2가 암모니아 중 370℃에서 15Å/min의 막 성장율을 제공하는 것으로 개시되었다. 약한 N-N 결합을 함유하는 1,1-디메틸히드라지노 리간드는 규소 표면 상에서 200℃ 미만에서 분해되는 것으로 알려져 있다. 그러나, 히드라지노실란으로부터 증착된 실리콘 카보니트라이드 막은 저밀도의 문제점을 지니고 있었다.
비스아미노실라시클로부탄이 규소 함유 막의 저온 증착에 대한 새로운 부류의 전구체로 제안되고 있다. 이들 분자는 저온에서 분해될 수 있는 팽팽한(strained) 4원의 실라시클로부탄 고리를 갖는다. 그러나, 비스아미노실라시클로부탄이 히드라지노실란과는 다른 메커니즘을 통해 분해되기 때문에, 비스아미노실라시클로부탄은 우수한 박막 특성을 제공할 것으로 예측된다. 비스아미노실라시클로부탄은 99+% 순도로 제조되었고, 200 내지 250℃에서 분해되는 것으로 확인되었다.
본 발명은 비스아미노실라시클로부탄, 및 질소 공급 가스, 산소 공급 가스 및 이의 혼합물로부터 선택된 공급 가스를 포함하는 반응성 가스 혼합물의 열 중합에 의해 규소 함유 박막을 생성시키는 방법에 관한 것이다. 증착된 막은 질화규소, 실리콘 카보니트라이드, 이산화규소 또는 탄소 도핑된 이산화규소일 수 있다. 이들 막은 반도체 장치에서 유전체, 패시베이션 코팅, 배리어 코팅, 스페이서, 라이너 및/또는 스트레서로 유용하다.
도 1은 비스(t-부틸아미노)실라시클로부탄(BTBSCB)을 사용하여 저압 CVD 반응기에서 실리콘 카보니트라이드 막을 증착시키는 공정을 도시한다.
본 발명은 기판 상에서 규소 함유 막을 생성시키는 방법으로서, 상기 막이 질화규소, 실리콘 카보니트라이드, 이산화규소 또는 탄소 도핑된 이산화규소일 수 있는 막 생성 방법에 관한 것이다. 전형적인 기판에는 이들로 제한되지는 않지만, 반도체 기판, 액정 장치, 발광 다이오드 표시 장치, 및 유기 발광 표시 장치가 포함된다. "반도체 기판"은 이들로 제한되는 것은 아니지만, 초점면 어레이, 광-전자 장치, 태양광 전지, 광학 장치, 트랜지스터 유사 장치, 3-D 장치, 규소-온-절연체(silicon-on-insulator), 초 격자(super lattice) 장치 등을 포함하는 반도체 부품의 제작에 사용하도록 의도된 비화갈륨 기재 장치, 및 규소 기재 장치를 포함함을 의미한다. 상기 반도체 기판은 하나 이상의 배선 층을 포함할 수 있다. 상기 반도체 기판은 또한 임의의 배선 층이 형성되기 전의 그러한 기판일 수 있다.
본원에서 유용한 비스아미노실라시클로부탄은 하기 화학식으로 표시되는 화합물 및 이들의 혼합물로부터 선택된다:
상기 식에서, 각각의 R1, R2, R3, R4, R5 및 R6은 독립적으로 수소, 또는 1 내지 6개의 탄소를 갖는 1가 탄화수소(선형, 분지형 또는 고리형; 포화 또는 불포화된) 기로부터 선택되며, m, n은 0 내지 10의 값을 갖는다. 각각의 R1, R2, R3, R4, R5 및 R6은 메틸, 에틸, 프로필, 이소-프로필, n-부틸, 2차-부틸, 3차-부틸, 시클로헥실, 시클로프로필, 페닐, 비닐, 헥세닐 등으로 예시될 수 있으나, 이들로 제한되지 않는다.
본원에서 유용한 비스아미노실라시클로부탄은 하기 화학식으로 표시되는 화합물로 예시될 수 있다:
막을 생성시키는데 사용된 반응성 가스 혼합물은 또한 질소 공급 가스, 산소 공급 가스, 또는 이들의 혼합물로부터 선택된 공급 가스를 조절된 양으로 포함할 수 있다. 공급 가스의 양은 사용된 가스 유형, 또는 막 증착 공정의 조건에 의해 조절될 수 있다.
질소 공급 가스에는 이들로 제한되지 않으나 질소 N2, 암모니아 NH3, 히드라진 N2H4, 히드라조산(hydrazoic acid) HN3, 및 이들의 혼합물이 포함된다. 상기 질소 공급 가스로 전형적인 것은 암모니아지만, 히드라진 및 히드라조산이 저온 증착을 위해 사용될 수 있다. 질소 공급 가스의 양은 전형적으로 비스아미노실라시클로부탄의 용량부(volume part)당 0.1 내지 50 용량부의 질소 공급 가스, 다르게는 비스아미노실라시클로부탄 용량부 당 0.2 내지 7 용량부의 질소 공급 가스이다. 당업자는 질소 공급 가스의 유형 및 증착 조건을 기초로 질소 공급 가스의 양을 용이하게 측정할 수 있을 것이다.
산소 공급 가스에는 이들로 제한되지 않지만 산소, 공기, 일산화질소, 산화질소, 일산화탄소, 과산화물, 이산화황 및 이들의 혼합물이 포함된다. 산소 공급 가스의 양은 전형적으로 비스아미노실라시클로부탄의 용량부 당 0.1 내지 50 용량부의 산소 공급 가스, 다르게는 비스아미노실라시클로부탄 용량부 당 0.2 내지 7 용량부의 산소 공급 가스이다. 당업자는 산소 공급 가스의 유형 및 증착 조건을 기초로 산소 공급 가스의 양을 용이하게 측정할 수 있을 것이다.
다른 물질들이 반응성 가스 혼합물 중에 존재할 수 있다. 예를 들어, 캐리어 가스, 예컨대 헬륨, 질소, 또는 아르곤, 도펀트(dopant), 예컨대 포스핀 또는 디보란, 할로겐, 예컨대 불소, 할로겐 함유 가스, 예컨대 SiF4, CF4, C3F6 및 C4F8, 또는 막에 부가적인 바람직한 특성을 제공하는 임의의 다른 물질이 존재할 수 있다.
상기 반응성 가스 혼합물이 기판, 바람직하게는 반도체 기판을 포함하는 증착 챔버 내로 도입되는데, 여기서 비스아미노실라시클로부탄의 중합이 이루어져서 기판 상에 막이 증착되게 된다. 열 화학적 기상 증착, 예컨대 저압 화학적 기상 증착(LPCVD) 또는 원자층 증착(ALD)이, 사용될 수 있는 저온 및 산업에서의 광범위한 용도 때문에 바람직하다. 플라즈마 보조된 CVD가 또한, 산소 공급 가스를 사용하거나 사용하지 않고 비스아미노실라시클로부탄으로부터 이산화규소 또는 탄소 도핑된 산화규소 막을 증착시키는데, 또는 질소 공급 가스를 사용하거나 사용하지 않고 비스아미노실라시클로부탄으로부터 질화규소 또는 실리콘 카보니트라이드 막을 증착시키는데 사용될 수 있다.
PECVD에서, 가스 혼합물은 플라즈마 장을 통과함으로써 반응한다. 이 공정에 사용된 플라즈마는 다양한 공급원, 예컨대 전기적 방전, 라디오 주파수 또는 극초단파 범위에서의 전자기장, 레이저 또는 입자 빔으로부터 유래한 에너지를 포함한다. 플라즈마 증착 공정에서는 중간 전력 밀도(0.1 내지 5 watt/㎠)에서의 극초단파(1.0 내지 10 GHz) 에너지, 또는 라디오 주파수(10 kHz 내지 102 MHz)를 사용하는 것이 일반적으로 바람직하다. 그러나 특정 주파수, 전력 및 압력은 일반적으로 장치에 대해 조정된다. 바람직하게는 상기 막은 20 내지 1000W의 전력; 0.13 내지 1333Pa의 압력; 및 25 내지 500℃의 온도에서 PECVD를 사용하여 증착된다. 종종 고밀도 플라즈마로도 칭해지는 한정된, 저압(0.13 내지 0.65 Pa) 극초단파 주파수 플라즈마는 CVD 성장 동안에 다양한 표면 지형의 평탄화를 돕는 공정에서 RF 주파수 여기와 조합될 수 있다.
본원에서 증착될 수 있는 막의 한 유형은 실리콘 카보니트라이드 막이다. 이들 막은 전형적으로 화학식 SiwCxHyNz로 표시되고, 여기서 C:Si의 비는 약 0:1 내지 약 10:1의 범위 내일 수 있고, N:Si의 비는 약 0:1 내지 약 1.5:1의 범위 내일 수 있으며, 잔여량은 수소이다. 실리콘 카보니트라이드 막을 증착시키기 위해서, 공동-반응물은 질소 공급 가스이다. 막이 비스아미노실라시클로부탄 및 질소 공급 가스로부터 증착되는 경우에, 아미노 기는 트랜스아미노화를 통해 질소 공급 가스로 대체되고, 상기 실라시클로부탄 기는 분해되어 유기 가스 종을 방출시키는 것으로 이론화되어 있다. 따라서, 막 중의 C:Si의 비는 전구체 중의 C:Si의 비와는 매우 다를 것으로 예상된다. 질소 공급 가스에 대한 비스아미노실라시클로부탄의 양은 100 부의 질소 공급 가스에 대해 1 부의 비스아미노실라시클로부탄, 다르게는 10 부의 질소 공급 가스에 대해 1 부의 비스아미노실라시클로부탄의 범위 내이다.
본원에서 증착될 수 있는 다른 유형의 막은 질화규소 막이다. 이들 막은 전형적으로 화학식 SibHcNd로 표시될 수 있고, 여기서 H:Si의 비는 약 0:1 내지 약 5:1의 범위 내일 수 있고, N:Si의 비는 약 0:1 내지 약 1.5:1의 범위 내일 수 있다. 이러한 막은 전형적으로 공동-반응물로서 질소 공급 가스를 사용하여 증착된다. 질소 공급 가스에 대한 비스아미노실라시클로부탄의 양은 100 부의 질소 공급 가스에 대해 1 부의 비스아미노실라시클로부탄, 다르게는 10 부의 질소 공급 가스에 대해 1 부의 비스아미노실라시클로부탄의 범위 내이다.
본원에서 증착될 수 있는 다른 유형의 막은 산화규소 막이다. 이들 막은 전형적으로 화학식 SiOx로 표시될 수 있고, 여기서 x는 0 내지 3이다. 이러한 막은 전형적으로 공동-반응물로서 산소 공급 가스를 사용하여 증착된다. 산소 공급 가스에 대한 비스아미노실라시클로부탄의 양은 100 부의 산소 공급 가스에 대해 1 부의 비스아미노실라시클로부탄, 다르게는 10 부의 산소 공급 가스에 대해 1 부의 비스아미노실라시클로부탄의 범위 내이다.
본원에서 증착될 수 있는 제 4 유형의 막은 탄소 도핑된 이산화규소 막이다. 이들 막은 전형적으로 화학식 SieCfOgHh로 표시될 수 있고, 여기서 e는 10 내지 33, 다르게는 18 내지 20 원자%의 값이고, f는 1 내지 66, 다르게는 18 내지 21 원자%의 값이고, g는 1 내지 66, 다르게는 31 내지 38 원자%이고, h는 0.1 내지 60, 다르게는 25 내지 32 원자%이고; e + f + g + h = 100 원자%이다. 이들 막은 전형적으로 공동-반응물로 산소 공급 가스를 사용하여 증착된다. 산소 공급 가스에 대한 비스아미노실라시클로부탄의 양은 100 부의 산소 공급 가스에 대해 1 부의 비스아미노실라시클로부탄, 다르게는 10 부의 산소 공급 가스에 대해 1 부의 비스아미노실라시클로부탄의 범위 내이다.
*본원에서 증착된 막은 변화되는 두께를 지닐 수 있다. 0.01 내지 10 ㎛의 두께를 갖는 막이 본 발명의 방법으로 증착될 수 있다. 다르게는, 상기 막은 0.5 내지 3.0 ㎛의 두께를 갖는다.
본원에서 증착된 막은 이들로 제한되지 않지만 게이트 유전체, 프리메탈(premetal) 및 금속간(intermetal) 유전체, 및 패시베이션 코팅을 포함하는, 반도체 집적 회로 제작에서의 유전체 또는 배리어 금속 코팅으로서 특히 적합하다.
도 1은 비스아미노실라시클로부탄으로부터 질화규소 또는 실리콘 카보니트라이드 박막을 증착하는 전형적인 공정을 도시하고 있다. 이 공정에서, 웨이퍼 기판이 저압 CVD(LPCVD) 반응기 내로 로딩되고, LPCVD 반응기는 목표 온도로 가열되어 10-4 torr 아래에서 배기된다. 암모니아 가스는 희석용 질소 가스와 혼합되고, 혼합된 NH3-N2 가스가 그 후 LPCVD 반응기 내로 계량된다. 질소 캐리어 가스는 액체 BTBSCB를 함유하는 샘플 실린더를 통해 유동한다. 질소 중에 운반된 BTBSCB의 증기는 LPCVD 반응기 내로 계량된다. 막이 증착된 후에, LPCVD 반응기는 냉각되고 대기압의 압력까지 질소로 다시 채워진다. 종국적으로 코팅된 웨이퍼가 LPCVD 반응기로부터 제거된다.
하기 실시예는 본 발명의 구체예를 설명하기 위해 포함된 것이다. 당업자는, 하기 실시예에 개시된 기술이 본 발명의 실시에서 잘 작용하기 위해 발명자에 의해 발견된 기술을 나타냄을 이해해야 한다. 그러나, 당업자는 본원의 개시 내용의 견지에서 많은 변형이, 개시되고 본 발명의 사상 및 범주를 벗어나지 않고 계속하여 유사한 결과를 나타내는 특정 구체예에서 이루어질 수 있음을 이해해야 한다. 모든 퍼센트는 중량%로 표시된다.
실시예 1
비스(t-부틸아미노)실라시클로부탄(BTBSCB)을 1,1-디클로로실라시클로부탄과 과량의 t-부틸아민을 반응시켜서 합성하였다(반응식 1). 이렇게 하기 위해서, 19.7 ml(0.166 mol)의 1,1-디클로로실라시클로부탄을 0℃에서 1L 헥산 중의 105 ml(0.999 mol)의 t-부틸아민에 첨가하였다. 실온에서 3일 동안 반응시킨 후에, t-부틸아민 염화물 염이 제거되도록 반응 슬러리를 여과하였다. 여과물을 진공 건조하여 미정제 액체 생성물을 수득하고 이것을 진공 증류시켰다. 16 g의 생성물을 50 torr 압력 하 71℃에서 45% 수율로 99.2%의 순도로 분리하였다. 1H, 13C 및 29Si NMR, FT-IR 및 GC-MS로 분석된 생성물의 구조는 비스(t-부틸아미노)실라시클로부탄과 일치하였다:
실시예 2
비스(에틸아미노)실라시클로부탄을 1,1-디클로로실라시클로부탄과 과량의 에틸아민을 반응시켜서 합성하였다(반응식 2). 이렇게 하기 위해서, 20.0 ml(0.169 mol)의 1,1-디클로로실라시클로부탄을 -10℃에서 1L 펜탄 중의 66.2 ml(1.01 mol)의 에틸아민에 첨가하였다. 실온에서 하루 동안 반응시킨 후에, 에틸아민 히드로염화물 염이 제거되도록 반응 슬러리를 여과하였다. 여과물을 진공 건조하여 미정제 액체 생성물을 수득하고 이것을 진공 증류시켰다. 9.8 g의 생성물을 30 torr 압력 하 42℃에서 36% 수율로 적어도 99%의 순도로 분리하였다. 1H, 13C 및 29Si NMR, FT-IR 및 GC-MS로 분석된 생성물의 구조는 비스(에틸아미노)실라시클로부탄과 일치하였다:
실시예 3
비스(피롤리디노)실라시클로부탄을 1,1-디클로로실라시클로부탄과 과량의 피롤리딘을 반응시켜서 합성하였다(반응식 3). 이렇게 하기 위해서, 23.7 ml(0.200 mol)의 1,1-디클로로실라시클로부탄을 -10℃에서 1L 헥산 중의 100.0 ml(1.20 mol)의 피롤리딘에 첨가하였다. 실온에서 2일 동안 반응시킨 후에, 피롤리딘 염화물 염이 제거되도록 반응 슬러리를 여과하였다. 여과물을 진공 건조하여 미정제 액체 생성물을 수득하고 이것을 진공 증류시켰다. 15.4 g의 생성물을 1 torr 압력 하 51℃에서 34% 수율로 99.7%의 순도로 분리하였다. 1H, 13C 및 29Si NMR, FT-IR 및 GC-MS로 분석된 생성물의 구조는 비스(피롤리디노)실라시클로부탄과 일치하였다:
실시예 4: 비스아미노실라시클로부탄의 열 분해 온도의 측정
실시예 1 내지 3에서 생성된 비스아미노실라시클로부탄을 시차 주사 열량계(DSC)로 분석하였다. 분자의 열 분해는, 발열 곡선이 DSC 스펙트럼 상에서 경사지기 시작하는 온도에서 시작한다. 열 분해 온도는 각각 비스(t-부틸아미노)실라시클로부탄(BTBSCB), 비스(에틸아미노)실라시클로부탄 및 비스(피롤리디노)실라시클로부탄에 대해 200℃, 200℃ 및 250℃인 것으로 측정되었다. 열 처리가 실시된 DSC 샘플을 이들 물질의 분해를 확인하기 위해 GC-MS로 분석하였다. BTBSCB의 분해를 200℃ 및 295℃에서 실행된 헤드스페이스(headspace) GC를 사용하여 추가로 확인하였다.
Claims (25)
- 비스(피롤리디노)실라시클로부탄을 포함하는 조성물.
- 1,1-디클로로실라시클로부탄을 피롤리딘과 반응시키는 단계를 포함하는, 비스(피롤리디노)실라시클로부탄을 제조하는 방법.
- 비스(피롤리디노)실라시클로부탄을 전구체로서 사용하여, 규소 함유 막을 저온 증착하는 방법.
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