TW201806960A - 胺基氯氫二矽烷 - Google Patents
胺基氯氫二矽烷 Download PDFInfo
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- TW201806960A TW201806960A TW106116176A TW106116176A TW201806960A TW 201806960 A TW201806960 A TW 201806960A TW 106116176 A TW106116176 A TW 106116176A TW 106116176 A TW106116176 A TW 106116176A TW 201806960 A TW201806960 A TW 201806960A
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- silicon
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- HKQQUUMRNMOVQK-UHFFFAOYSA-N N[SiH]([SiH3])Cl Chemical class N[SiH]([SiH3])Cl HKQQUUMRNMOVQK-UHFFFAOYSA-N 0.000 title 1
- 150000001875 compounds Chemical class 0.000 claims abstract description 106
- 239000012686 silicon precursor Substances 0.000 claims abstract description 94
- 238000000034 method Methods 0.000 claims abstract description 86
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 67
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 63
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000010703 silicon Substances 0.000 claims abstract description 60
- 239000002243 precursor Substances 0.000 claims abstract description 56
- 230000008021 deposition Effects 0.000 claims abstract description 39
- 239000000203 mixture Substances 0.000 claims abstract description 38
- 239000000758 substrate Substances 0.000 claims abstract description 36
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 33
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000001301 oxygen Substances 0.000 claims abstract description 21
- 239000007833 carbon precursor Substances 0.000 claims abstract description 15
- 125000001309 chloro group Chemical group Cl* 0.000 claims abstract description 10
- 239000011261 inert gas Substances 0.000 claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 125000001145 hydrido group Chemical group *[H] 0.000 claims abstract description 3
- 238000000151 deposition Methods 0.000 claims description 42
- 238000005229 chemical vapour deposition Methods 0.000 claims description 26
- 238000000231 atomic layer deposition Methods 0.000 claims description 25
- 239000000460 chlorine Substances 0.000 claims description 22
- -1 lithium aluminum hydride Chemical compound 0.000 claims description 22
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 21
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 21
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 20
- 229910052799 carbon Inorganic materials 0.000 claims description 19
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- 229930195733 hydrocarbon Natural products 0.000 claims description 15
- 150000002430 hydrocarbons Chemical class 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 13
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 10
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 9
- 125000005265 dialkylamine group Chemical group 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
- 125000004169 (C1-C6) alkyl group Chemical group 0.000 claims description 7
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 claims description 7
- UMVBXBACMIOFDO-UHFFFAOYSA-N [N].[Si] Chemical compound [N].[Si] UMVBXBACMIOFDO-UHFFFAOYSA-N 0.000 claims description 7
- SIPUZPBQZHNSDW-UHFFFAOYSA-N bis(2-methylpropyl)aluminum Chemical compound CC(C)C[Al]CC(C)C SIPUZPBQZHNSDW-UHFFFAOYSA-N 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 6
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 6
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 125000005913 (C3-C6) cycloalkyl group Chemical group 0.000 claims description 5
- 125000000882 C2-C6 alkenyl group Chemical group 0.000 claims description 5
- 125000003601 C2-C6 alkynyl group Chemical group 0.000 claims description 5
- 239000001272 nitrous oxide Substances 0.000 claims description 5
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- HJXBDPDUCXORKZ-UHFFFAOYSA-N diethylalumane Chemical compound CC[AlH]CC HJXBDPDUCXORKZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000004065 semiconductor Substances 0.000 claims description 4
- 238000007740 vapor deposition Methods 0.000 claims description 4
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 239000012280 lithium aluminium hydride Substances 0.000 claims description 3
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910001868 water Inorganic materials 0.000 claims description 3
- 125000006557 (C2-C5) alkylene group Chemical group 0.000 claims description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 2
- JEDZLBFUGJTJGQ-UHFFFAOYSA-N [Na].COCCO[AlH]OCCOC Chemical compound [Na].COCCO[AlH]OCCOC JEDZLBFUGJTJGQ-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 229910001882 dioxygen Inorganic materials 0.000 claims description 2
- 239000012419 sodium bis(2-methoxyethoxy)aluminum hydride Substances 0.000 claims description 2
- 229910001148 Al-Li alloy Inorganic materials 0.000 claims 1
- RNJCXDJXPXWMDK-UHFFFAOYSA-N [AlH3].COCCO[Na] Chemical compound [AlH3].COCCO[Na] RNJCXDJXPXWMDK-UHFFFAOYSA-N 0.000 claims 1
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical compound [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 claims 1
- 150000004678 hydrides Chemical class 0.000 claims 1
- 230000002194 synthesizing effect Effects 0.000 abstract description 4
- 125000004663 dialkyl amino group Chemical group 0.000 abstract 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 27
- 238000006243 chemical reaction Methods 0.000 description 22
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 20
- 125000004430 oxygen atom Chemical group O* 0.000 description 20
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 18
- 125000004432 carbon atom Chemical group C* 0.000 description 17
- 238000004817 gas chromatography Methods 0.000 description 17
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 14
- 239000004215 Carbon black (E152) Substances 0.000 description 13
- 239000007789 gas Substances 0.000 description 13
- 238000000576 coating method Methods 0.000 description 11
- 235000012431 wafers Nutrition 0.000 description 11
- 239000011248 coating agent Substances 0.000 description 9
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 9
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 239000011541 reaction mixture Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 125000004429 atom Chemical group 0.000 description 6
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 6
- 239000012159 carrier gas Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 238000005481 NMR spectroscopy Methods 0.000 description 5
- 150000001335 aliphatic alkanes Chemical class 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 5
- 238000004891 communication Methods 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 5
- 229910010271 silicon carbide Inorganic materials 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 4
- 238000000995 aerosol-assisted chemical vapour deposition Methods 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000010926 purge Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- LUQPSPPZTFJIBE-UHFFFAOYSA-N CCN(CC)[Si](N[SiH3])(N(CC)CC)Cl Chemical compound CCN(CC)[Si](N[SiH3])(N(CC)CC)Cl LUQPSPPZTFJIBE-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 3
- 238000000277 atomic layer chemical vapour deposition Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 description 3
- 125000005843 halogen group Chemical group 0.000 description 3
- 230000000737 periodic effect Effects 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 3
- MNVMAELRKZZCET-UHFFFAOYSA-N Cl[SiH2]N([Si](Cl)(Cl)Cl)Cl Chemical compound Cl[SiH2]N([Si](Cl)(Cl)Cl)Cl MNVMAELRKZZCET-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- LRBZYDDQWIWCGS-UHFFFAOYSA-N [SiH3]N[Si](Cl)(Cl)Cl Chemical compound [SiH3]N[Si](Cl)(Cl)Cl LRBZYDDQWIWCGS-UHFFFAOYSA-N 0.000 description 2
- 239000000443 aerosol Substances 0.000 description 2
- 125000002947 alkylene group Chemical group 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 description 2
- 230000005493 condensed matter Effects 0.000 description 2
- 229910021419 crystalline silicon Inorganic materials 0.000 description 2
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- 150000001983 dialkylethers Chemical class 0.000 description 2
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- 238000002474 experimental method Methods 0.000 description 2
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- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000000259 microwave plasma-assisted chemical vapour deposition Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 238000001289 rapid thermal chemical vapour deposition Methods 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 2
- 238000000038 ultrahigh vacuum chemical vapour deposition Methods 0.000 description 2
- 238000001039 wet etching Methods 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 description 1
- 125000006532 (C3-C5) alkyl group Chemical group 0.000 description 1
- DKPUTCRGYIIWGE-UHFFFAOYSA-N 1-(silylamino)silylbutane Chemical compound C(CCC)[SiH2]N[SiH3] DKPUTCRGYIIWGE-UHFFFAOYSA-N 0.000 description 1
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
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- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 229910007991 Si-N Inorganic materials 0.000 description 1
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- UBMXAAKAFOKSPA-UHFFFAOYSA-N [N].[O].[Si] Chemical compound [N].[O].[Si] UBMXAAKAFOKSPA-UHFFFAOYSA-N 0.000 description 1
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- 150000005215 alkyl ethers Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
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- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical group CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 1
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- GGNALUCSASGNCK-UHFFFAOYSA-N carbon dioxide;propan-2-ol Chemical compound O=C=O.CC(C)O GGNALUCSASGNCK-UHFFFAOYSA-N 0.000 description 1
- 238000000451 chemical ionisation Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical class Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- QMMPBNFUSOIFDC-UHFFFAOYSA-N ctk0b2378 Chemical compound Cl[Si](Cl)(Cl)N[Si](Cl)(Cl)Cl QMMPBNFUSOIFDC-UHFFFAOYSA-N 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
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- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
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- PQPVPZTVJLXQAS-UHFFFAOYSA-N hydroxy-methyl-phenylsilicon Chemical class C[Si](O)C1=CC=CC=C1 PQPVPZTVJLXQAS-UHFFFAOYSA-N 0.000 description 1
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- HTBVGZAVHBZXMS-UHFFFAOYSA-N lithium;tris[(2-methylpropan-2-yl)oxy]alumane Chemical compound [Li].[Al+3].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-] HTBVGZAVHBZXMS-UHFFFAOYSA-N 0.000 description 1
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000000927 vapour-phase epitaxy Methods 0.000 description 1
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Abstract
揭示一種用於沉積之矽前驅物化合物,該矽前驅物化合物包含一種化合物,其係二矽烷且包含至少一個氯基、至少一個二烷基胺基及至少一個氫基;一種用於形成膜的組成物,該組成物包含該矽前驅物化合物,以及下列中之至少一者:惰性氣體、分子氫、碳前驅物、氮前驅物、以及氧前驅物;一種合成該矽前驅物化合物之製程;一種使用該矽前驅物化合物在基材上形成含矽膜的方法;藉以形成的該含矽膜;以及一種形成該矽前驅物化合物之方法。
Description
本發明大致上關於一種用於形成膜的前驅物化合物以及組成物、關於一種合成該前驅物化合物的製程、關於一種用於以該前驅物化合物或組成物經由沉積裝置形成膜的方法、以及關於藉由該方法所形成的膜。
元素矽、及其他矽材料(諸如氧化矽、碳化矽、氮化矽、碳氮化矽、及氧碳氮化矽)具有各種已知的用途。例如,在用於電子或光伏元件的電子電路之製造中,矽膜可用來作為半導體、絕緣層或犧牲層。
已知製備矽材料的方法可以使用一或多種矽前驅物。這些矽前驅物的使用不限於製造用於電子或光伏半導體應用的矽。例如,矽前驅物可用於製備基於矽之潤滑劑、彈性體、及樹脂。
我們在電子和光伏產業中看到對於改良的矽前驅物之長久以來的需求。我們認為改良的前驅物會實現降低沉積溫度及/或製造出更精細的半導體特徵,以得到性能更好的電子和光伏元件。
我們已發現一種改良的矽前驅物。本發明提供下列各種實施例:一種用於沉積之前驅物化合物,該前驅物化合物包含一種化合物,其係二矽烷且包含至少一個氯基、至少一個二烷基胺基及至少一個氫基(hydrido group)(以下稱為「矽前驅物化合物(Silicon Precursor Compound)」)。
一種用於形成膜的組成物,該組成物包含該矽前驅物化合物,以及下列中之至少一者:惰性氣體、分子氫、碳前驅物、氮前驅物、以及氧前驅物。
一種合成該矽前驅物化合物之製程,該方法包含將具有至少二個氯基及至少一個二烷基胺基的二矽烷與氫化鋁接觸。
一種於基材上形成含矽膜之方法,該方法包含在基材存在下,使包含該矽前驅物化合物之矽前驅物之蒸氣經歷沉積條件,以在該基材上形成含矽膜。
一種根據該方法所形成的膜。
發明內容及摘要以引用方式併入本文中。上文概述之本發明實施例、用途及優點將在下文進一步描述。
本發明的態樣在本文使用各種常見慣例來描述。例如,所有的物質狀態都是在25℃和101.3kPa下測定,除非另有指明。所
有的%均按重量計,除非另有說明或指明。除非另有指明,所有的%值都是以所有用以合成或製造該組合物的成分之總量計,所有用以合成或製造該組合物的成分加總為100%。任何包含一個屬及其次屬的馬庫西群組包括該屬中的次屬,例如在「R係烴基或烯基」中,R可以是烯基,或者R可以是烴基,而該烴基除了其他次屬之外還包括烯基。對於美國專利實務,茲以引用方式將本文中引用的所有美國專利申請公開案和專利、或其一部分(若只引用該部分)在以併入的標的物不與本實施方式牴觸下併入本文中,若有任何這樣的牴觸則以本實施方式為準。
本發明的態樣在本文中使用各種專利用語來描述。例如,「可替代地(alternatively)」指示不同且相異的實施例。「比較例(Comparative example)」意指非發明的實驗。「包含(comprise)」及其變型(包含(comprising/comprised of))是開放式的。「由…所組成(Consist of)」及其變型(consisting of)是封閉式的。「接觸(contacting)」表示使進行物理接觸。「可(may)」代表有選擇性,而非必要性。「可選(地)(optionally)」代表存在,可替代地不存在。
本發明的態樣在本文中使用各種化學用語來描述。該等用語之涵義相對應於其由IUPAC發布之定義,除非本文另有定義。為了方便起見,對某些化學用語加以定義。
用語「沉積(deposition)」為在特定位置產生凝態物質的製程。凝態物質在尺寸上可受到限制或不受限制。沉積的實例為形成膜、形成棒、以及形成粒子的沉積。
用語「膜(film)」意指在一個維度受到限制的材料。受限的維度可經表徵為「厚度(thickness)」,且為在所有其他條件皆相同下,隨著沉積該材料以形成膜的製程之時間長度增加而增加的維度。
用語「鹵素(halogen)」是指氟、氯、溴或碘,除非另有定義。
用語「IUPAC」是指國際純化學暨應用化學聯合會。
用語「缺乏(lack)」是指不含或完全不存在。
「元素週期表(Periodic Table of the Elements)」是指由IUPAC在2011年公布的版本。
用語「前驅物(precursor)」意指含有所指元素的原子並且在藉由沉積方法所形成的膜中可用來作為該元素來源的物質或分子。
用語「分離(seperate)」意指造成實體上分開,並因此不再直接接觸。
用語「基材(substrate)」意指具有至少一個表面的物理支撐,另一材料可配置於該至少一個表面上。
本發明提供矽前驅物化合物以及用於形成膜的組成物。矽前驅物化合物特別適合用於形成含矽膜之沉積製程,但是矽前驅物化合物不限於該等應用。例如,可在其他應用中利用矽前驅物化合物,如作為用於製備矽氧烷或矽氮烷材料的反應物。本發明進一步提供形成膜的方法,以及根據該方法所形成的膜。
矽前驅物化合物係二矽烷且包含至少一個氯基、至少一個二烷基胺基及至少一個氫基。當矽前驅物化合物係用於本發明之組成物及方法中時,矽前驅物化合物可具有自99面積%(GC)至99.9999999面積%(GC)的純度。然而,根據設想若用於非電子應用,矽前驅物可具有自95至98%之純度。
在一實施例中,矽前驅物化合物具有式(I):(R1R2N)aClbHcSiSiHdCle(R1R2N)f,其中各R1獨立地係H、(C1-C6)烷基、(C3-C6)環烷基、(C2-C6)烯基、(C2-C6)炔基、或苯基;且各R2獨立地係(C1-C6)烷基、(C3-C6)環烷基、(C2-C6)烯基、(C2-C6)炔基、或苯基;或在相同或不同氮原子上之R1及R2鍵結在一起成為-R1a-R2a-,其中-R1a-R2a-係(C2-C5)伸烷基;且其中a、b、c、d、e及f係整數,其等範圍獨立地自零至三;條件為a及f中之至少一者不是零,b及e中之至少一者不是零,且c及d中之至少一者不是零。
在矽前驅物化合物的一些態樣中,在式(I)中,各R1及R2獨立地係(C1-C6)烷基;可替代地,R1係(C1-C6)烷基且R2係(C3-C5)烷基;可替代地,R1係甲基或乙基且R2係異丙基、二級丁基、異丁基、或三級丁基;可替代地,各R1及R2獨立地係異丙基、二級丁基、異丁基、或三級丁基;可替代地,R1係甲基且R2係三級丁基;可替代地,各R1及R2獨立地係(C3-C4)烷基;可替代地,各R1及R2係異丙基;可替代地,各R1及R2係二級丁基;可替代地,R1係(C3-C6)環烷基;可替代地,R1係(C2-C6)烯基或(C2-C6)炔基;可替代地,R1係H;可替代地,R1係苯基;可替代地,R1係如緊接的前述四個態樣
中之任一者所定義且R2係(C1-C6)烷基或R2係與R1相同;可替代地,R1及R2鍵結在一起成為-R1a-R2a-,其中-R1a-R2a-係(C3-C5)伸烷基;可替代地,在相同氮上之R1及R2鍵結在一起成為-R1a-R2a-,其中-R1a-R2a-係(C4或C5)伸烷基。
在矽前驅物化合物的一些態樣中,在式(I)中,a及f中只有一者係一,且另一者係零。
在矽前驅物化合物的一些態樣中,在式(I)中,b及e獨立地係零、1、或2,可替代地0、可替代地1、可替代地2、可替代地3、可替代地0或1、可替代地1或2。
在矽前驅物化合物的一些態樣中,在式(I)中,b+e係自1至4、可替代地1、可替代地2、可替代地3、可替代地4、可替代地自2至4、可替代地自3或4、可替代地1至3、可替代地自1或2、可替代地2或3、可替代地3或4。
在一些態樣中,矽前驅物化合物係[(CH3)2CH]2NSiCl2SiH3、[(CH3)2CH]2NSiH2SiH2Cl、[(CH3CH2)2N]2SiClSiH3、[(CH3CH2)(CH3)N]2SiClSiH3、HSiClN[CH(CH3)2]2SiCl3、HSiCl2SiCl2N[CH(CH3)2]2、或HSiClN[CH(CH3)2]2SiCl2N[CH(CH3)2]2,可替代地[(CH3)2CH]2NSiCl2SiH3、[(CH3)2CH]2NSiH2SiH2Cl、[(CH3CH2)2N]2SiClSiH3或[(CH3CH2)(CH3)N]2SiClSiH3。
矽前驅物化合物可以任何方式提供。例如,矽前驅物化合物可藉由合成或以其他方式獲得以用於該方法中。在一實施例中,
矽前驅物化合物係藉由下列製成合成。在第一步驟中,2 HSiCl3+熱->HSiCl2SiCl3+HCl,其可諸如經由蒸發或汽提來自其中分離。在(正式)第二步驟中,2n HNR1R2+HSiCl2SiCl3->HSi2(NR1R2)nCl5-n,其中n係1至4,且R1及R2係如上定義。當NR1R2基團的來源係HNR1R2時,會形成反應副產物H2NR1R2Cl。當NR1R2基團的來源係MANR1R2時,會形成反應副產物MA(Cl)m。H2NR1R2Cl及MA(Cl)m鹽可經由諸如過濾或傾析來自其中分離。製程的第二步驟可包含在烴媒劑中,使五氯二矽烷(HSiCl2SiCl3)與NR1R2基團的來源接觸,以給出矽前驅物化合物;其中NR1R2基團的來源係金屬R1R2醯胺[(R1R2N]mMA,其中下標m係1或2,其中當m係1時,MA係元素週期表I族的元素,且當m係2時,MA係元素週期表II族的元素,或者NR1R2基團的來源係HNR1R2。
合成矽前驅物化合物的製程的第二步驟可在烴媒劑或醚媒劑中實行。醚媒劑可包含二矽基醚、二烴基醚、或烷二醇二烷基醚、或其任二或更多者之混合物。二烴基醚可以是直鏈醚、環醚、或二芳基醚、或其任二或更多者之混合物。醚媒劑的實例為二乙基醚、二甲基醚、四氫呋喃、1,2-二甲氧基乙烷、四乙二醇二甲基醚。烷二醇二烷基醚可為伸丁二醇二(C1-C4)烷基醚、丙二醇二(C2-C4)烷基醚、乙二醇二(C3或C4)烷基醚、或其任二或更多者之混合物。烴媒劑可包含具有至少5個碳原子之烷烴、具有至少5個碳原子之環烷、具有至少6個碳原子之芳烴、或其任二或更多者之混合物。烴媒劑可包含戊
烷、己烷、環己烷、庚烷、苯、甲苯、二甲苯、或其任二或更多者之混合物。
烴媒劑的組成物可經設想以優化接觸步驟(例如,選擇具有用於達到所欲反應溫度的沸點的烴媒劑或缺乏溶解反應副產物的能力的烴媒劑)。除此之外或可替代地,烴媒劑的組成物可經設想以優化可選的分離步驟(例如,選擇具有所欲沸點的烴媒劑,使得能夠在不蒸發矽前驅物化合物的情况下實現其蒸發)。烴媒劑可由碳和氫原子組成或可為由碳、氫和鹵素原子組成的鹵化烴媒劑。由C和H原子組成的烴媒劑可為烷烴、芳烴、及其任二或更多者之混合物。烷烴可為己烷、環己烷、庚烷、異烷烴、或其任二者或更多者之混合物。芳烴可為甲苯、二甲苯、或其任二者或更多者之混合物。鹵化烴媒劑可為二氯甲烷。具有不同烴媒劑組成物的製程可以在至少一種結果、性質、功能、及/或用途中彼此不同。烴媒劑的不同組成物可為矽前驅物化合物、NR1R2基團的來源、反應副產物、或其任二或更多者之組合提供不同的溶解性。
本發明進一步關於一種用於生產化合物之方法,該化合物係二矽烷且包含至少一個氯基、至少一個二烷基胺基及至少一個氫基。該方法包含將具有至少二個氯基及至少一個二烷基胺基的二矽烷與氫化鋁接觸。較佳地,二矽烷僅具有氯基及二烷基胺基。氫化鋁係具有至少一個氫基與鋁原子鍵結之化合物。氫化鋁之實例包括例如氫化二異丁基鋁、氫化二乙基鋁、氫化三-三級丁氧基鋁鋰、氫化參[(3-乙基-3-戊基)氧基]鋁鋰、氫化雙(2-甲氧基乙氧基)鋁鈉、氫化鋁鋰、氫
化鋁鈉及氫化鋁。較佳的氫化鋁係氫化二異丁基鋁及氫化二乙基鋁,較佳的是氫化二異丁基鋁。較佳地,二矽烷對氫化鋁之莫耳比係自0.1:1至0:1,可替代地自0.2:1至3.5:1,可替代地0.3:1至3:1,可替代地1:1至4:1,可替代地1:1至3.5:1,可替代地2:1至3:1。較佳地,反應溫度係自-30℃至40℃,可替代地自-30℃至20℃,可替代地自-25℃至15℃。較佳地,反應係在無溶劑下實行。
如上所述,用於形成膜的組成物包含矽前驅物化合物,以及下列中之至少一者:惰性氣體、分子氫、碳前驅物、氮前驅物、以及氧前驅物。分子氫可與矽前驅物化合物一起使用於組成物中,以用於形成元素矽膜。於本文中,分子氫、碳前驅物、氮前驅物、或氧前驅物的蒸氣或氣體狀態通常稱作額外反應物氣體。
碳前驅物可與矽前驅物化合物一起使用於組成物中,以用於根據本方法的實施例形成矽碳膜。矽碳膜含有Si及C原子,且可包含碳化矽。碳前驅物可包含下列、可替代地基本上由下列所組成、可替代地由下列所組成:C、H、及可選地Si原子。當包含C、H、及可選地Si原子的碳前驅物係在用於形成碳氮化矽膜或氧碳化矽膜之方法中使用時,該碳前驅物可進一步分別包含N或O原子,或當該碳前驅物係在用於形成氧碳氮化矽膜之方法中使用時,該碳前驅物可進一步包含N及O原子。基本上由C、H、及可選地Si原子所組成之碳前驅物缺乏N及O原子,但可選地可具有一或多個鹵素原子(例如,Cl)。由C及H原子所組成之碳前驅物的實例係烴,諸如烷。由C、
H、及Si原子所組成之碳前驅物的實例係烴基矽烷,諸如丁基二矽烷或四甲基矽烷。
氮前驅物可與矽前驅物化合物一起使用於組成物中,以用於根據本方法的實施例形成矽氮膜。氮前驅物與矽前驅物化合物不同。矽氮膜含有Si及N原子以及可選地C及/或O原子,且可包含氮化矽、氧氮化矽、或氧碳氮化矽。氮化矽可以是SixNy,其中下標x係1、2或3,可替代地自1至4之整數,且下標y係自1至5之整數。氮前驅物可包含N原子以及可選地H原子;可替代地,氮前驅物可基本上由N原子以及可選地H原子所組成;可替代地,氮前驅物可由N以及可選地H原子所組成。當包含N以及可選地H原子的氮前驅物係在用於形成碳氮化矽膜或氧氮化矽膜之方法中使用時,該氮前驅物可進一步分別包含C或O原子,或當該氮前驅物係在用於形成氧碳氮化矽膜之方法中使用時,該氮前驅物可進一步包含C及O原子。基本上由N原子以及可選地H原子所組成之氮前驅物缺乏C及O原子,但可選地可具有一或多個鹵素原子(例如,Cl)。由N原子所組成之氮前驅物的一實例係分子氮。由N及H原子所組成之氮前驅物的實例係氨及肼。由O及N原子所組成之氮前驅物的一實例係一氧化氮(N2O)及二氧化氮(NO2)。
氧前驅物可與矽前驅物化合物一起使用於組成物中,以用於根據本方法的實施例形成矽氧膜。矽氧膜含有Si及O原子以及可選地C及/或N原子,且可包含氧化矽、氧碳化矽、氧氮化矽、或氧碳氮化矽。氧化矽可以是SiO或SiO2。氧前驅物可包含O原子以及可選
地H原子;可替代地,可基本上由O原子以及可選地H原子所組成;可替代地,可由O原子以及可選地H原子所組成。當包含O原子以及可選地H原子的氧前驅物係在用於形成氧碳化矽膜或氧氮化矽膜之方法中使用時,該氧前驅物可進一步分別包含C或N原子,或當該氧前驅物係在用於形成氧碳氮化矽膜之方法中使用時,該氧前驅物可進一步包含C及N原子。由O原子所組成之氧前驅物的實例係分子氧及臭氧。由O及H原子所組成之氧前驅物的實例係水及過氧化氫。由O及N原子所組成之氧前驅物的一實例係一氧化氮、一氧化二氮、及二氧化氮。
惰性氣體可與前述前驅物之任一者以及組成物或方法的任一實施例組合使用。惰性氣體的實例係氦、氬、及其混合物。例如,在其中所形成之含矽膜係元素矽膜之方法的實施例中,氦可與矽前驅物化合物及分子氫組合使用。可替代地,氦可與矽前驅物化合物及碳前驅物、氮前驅物、及氧前驅物中之任一者一起使用於其中所形成之含矽膜分別係矽碳膜、矽氮膜、或矽氧膜之方法的實施例中。
本方法所形成之膜係含有Si且在一個維度受到限制的材料,該維度可稱作該材料的厚度。含矽膜可以是元素矽膜、矽碳膜、矽氮膜、或矽氧膜(例如氧化矽、氮化矽、碳氮化矽、氧氮化矽、或氧碳氮化矽膜。本方法所形成之元素矽膜缺乏C、N、及O原子,且可以是非晶形或結晶Si材料。本方法所形成之矽碳膜含有Si及C原子以及可選地N及/或O原子。本方法所形成之矽氮膜含有Si
及N原子以及可選地C及/或O原子。本方法所形成之矽氧膜含有Si及O原子以及可選地C及/或N原子。
該膜可有用於電子或光伏應用。例如,氮化矽膜可形成作為絕緣層、鈍化層、或在電容器中之多晶矽層之間的介電層。
本形成膜之方法使用沉積裝置。本方法中所利用之沉積裝置通常係基於所欲之形成膜之方法而選擇,且可以是所屬技術領域中具有通常知識者已知之任何沉積裝置。
在某些實施例中,沉積裝置包含物理氣相沉積裝置。在這些實施例中,沉積裝置一般而言係選自濺鍍裝置及直流電(DC)磁控管濺鍍裝置。這些物理氣相沉積裝置之各者的最佳操作參數係基於本方法中所利用之矽前驅物化合物以及經由該沉積裝置所形成之膜的所欲應用而定。在某些實施例中,沉積裝置包含濺鍍裝置。濺鍍裝置可以是例如離子束濺鍍裝置、反應性濺鍍裝置、或離子輔助濺鍍裝置。
然而更一般而言,沉積裝置包含原子層沉積裝置或化學氣相沉積裝置。在使用原子層沉積裝置的實施例中,形成膜之方法可稱作原子層沉積法。同樣地,在使用化學氣相沉積裝置的實施例中,形成膜之方法可稱作化學氣相沉積法。原子層沉積和化學氣相沉積之裝置與方法大致上係所屬技術領域中所熟知。本方法在下文中藉由提及使用原子層沉積裝置來例示,然而本方法可輕易地經調適以使用化學氣相沉積裝置。
在使用原子層沉積裝置之方法的實施例中,原子層沉積裝置可選自例如熱原子層沉積裝置、電漿增強原子層沉積裝置、及空
間原子層沉積裝置。這些原子層沉積裝置之各者的最佳操作參數係基於本方法中所利用之矽前驅物化合物以及經由該沉積裝置所形成之膜的所欲應用而定。所屬技術領域中具有通常知識者將知道如何最佳化所採用之特定裝置的操作參數。
在原子層沉積中,用於形成膜之氣體一般而言係在一系列循環中經引入沉積艙中並在沉積艙中反應,其中循環包含用矽前驅物化合物填充反應艙(第一半反應)、用惰性氣體吹掃反應器、用另一反應氣體填充反應艙(第二半反應)、接著用惰性氣體吹掃反應器。一系列的二個半反應(第一及第二)循環在基材表面上形成適當膜元素或分子原子層沉積通常需要對系統添加能量,諸如加熱沉積艙及基材。
在使用化學氣相沉積裝置之方法的實施例中,化學氣相沉積裝置可選自,例如可流動化學氣相沉積裝置、熱化學氣相沉積裝置、電漿增強化學氣相沉積裝置、光化學氣相沉積裝置、電子迴旋共振裝置、感應耦合電漿裝置、磁約束電漿裝置、低壓化學氣相沉積裝置、以及噴射氣相沉積裝置。這些化學氣相沉積裝置之各者的最佳操作參數係基於本方法中所利用之矽前驅物化合物以及經由該沉積裝置所形成之膜的所欲應用而定。在某些實施例中,沉積裝置包含電漿增強化學氣相沉積裝置。在其他實施例中,沉積裝置包含低壓化學氣相沉積裝置。
在化學氣相沉積中,用於形成膜之氣體一般係在沉積艙中混合與反應。該反應形成蒸氣狀態之適當膜元素或分子。然後元素
或分子沉積在基材(或晶圓)上且積累以形成膜。化學氣相沉積通常需要對系統添加能量,諸如加熱沉積艙及基材。
氣體物種之反應通常係所屬技術領域中眾所周知的,且可經由本發明之方法實行任何習知化學氣相沉積(CVD)技術。例如,可使用諸如以下方法:簡單熱氣相沉積、電漿增強化學氣相沉積(PECVD)、電子迴旋共振(ECRCVD)、大氣壓化學氣相沉積(APCVD)、低壓化學氣相沉積(LPCVD)、超高真空化學氣相沉積(UHVCVD)、氣溶膠輔助化學氣相沉積(AACVD)、直接液體注入化學氣相沉積(DLICVD)、微波電漿輔助化學氣相沉積(MPCVD)、遠端電漿增強化學氣相沉積(RPECVD)、原子層化學氣相沉積(ALCVD或ALD)、熱絲化學氣相沉積(HWCVD)、混合物理化學氣相沉積(HPCVD)、快速熱化學氣相沉積(RTCVD)、及氣相磊晶化學氣相沉積(vapor-phase epitaxy chemical vapor,VPECVD)、光輔助化學氣相沉積(photo-assisted chemical vapor disposition,PACVD)、火焰輔助化學氣相沉積(FACVD)、或任何相似的技術。
可利用化學氣相沉積或原子層沉積來形成具有多種厚度之膜,該等厚度將視膜的所欲最終用途而定。舉例來說,膜可具有數奈米之厚度或數微米之厚度、或更大或更小之厚度(或落在這些值之間的厚度)。這些膜可以可選地被塗層覆蓋,諸如SiO2塗層、SiO2/改質陶瓷氧化物層、含矽塗層、含矽碳塗層、含碳化矽塗層、含矽氮塗層、含氮化矽塗層、含矽氮碳塗層、含矽氧氮塗層、及/或類鑽石碳塗層。此等塗層及其沉積方法通常係所屬技術領域中已知。
本方法中所利用之基材不受限制。在某些實施例中,基材僅受限於在沉積艙的溫度以及環境中之熱及化學安定性的需求。因此,基材可以是,例如玻璃、金屬、塑膠、陶瓷、以及矽(如單晶矽、多晶矽、非晶矽等)。
本方法的實施例可包括包含一氧化二氮(N2O)之反應性環境。此等反應性環境通常係所屬技術領域中已知的。在這些實施例中,該方法通常涉及在一氧化二氮存在下分解矽前驅物化合物。該方法的一實例描述於美國專利第US 5,310,583號。利用一氧化二氮可修飾在化學氣相沉積方法中形成之所得膜之組成。
化學氣相沉積裝置及原子層沉積裝置以及因此所利用之化學氣相沉積及原子層沉積方法通常係藉由平衡若干因子而選擇,該等因子包括但不限於矽前驅物化合物、所欲的膜純度、基材的幾何組態、以及經濟考量。
化學氣相沉積以及原子層沉積中所控制之主要操作變數包括但不限於溫度、基材溫度、壓力、矽前驅物化合物在氣相中的濃度、任何額外的反應物氣體濃度(例如,任何碳前驅物、氮前驅物、及/或氧前驅物之氣體的濃度)、以及總氣體流。化學氣相沉積或原子層沉積係自包括但不限於熱解、氧化、還原、水解、及其組合之化學反應而產生。選擇化學氣相沉積或原子層沉積之最佳溫度需要有對矽前驅物化合物以及所選化學反應之動力學與熱力學之了解。
習知化學氣相沉積方法通常需要顯著高溫,諸如大於600℃,例如600℃至1000℃。然而,咸信矽前驅物化合物可以大幅
較低的溫度在化學氣相沉積或原子層沉積中利用。例如,本方法可在自25℃至700℃、可替代地自100至700℃、可替代地自200℃至700℃、可替代地自200℃至600℃、可替代地自200℃至500℃、可替代地自200℃至400℃、可替代地自100℃至300℃的溫度下實行。實行該方法之溫度可以是恆溫的或動態的。
化學氣相沉積或原子層沉積製程一般涉及產生前驅物、運輸前驅物至反應艙中、以及將前驅物吸附至經加熱基材上,或前驅物之化學反應且後續吸附至基材上。以下列舉化學氣相沉積或原子層沉積方法的概略調查以說明大量可用選項中的一些。
在熱CVD或ALD中,膜係藉由使矽前驅物化合物之蒸氣形式氣流通過經加熱基材上而沉積。當矽前驅物化合物之蒸氣形式接觸經加熱基材時,矽前驅物化合物通常會反應及/或分解以形成膜。
在PECVD中,矽前驅物化合物之蒸氣形式係藉由通過電漿域而反應以形成反應性物種。然後反應性物種會集中並沉積在基材上以形成膜。大致上,PECVD優於熱CVD的優點是可以使用較低的基材溫度。PECVD中所利用之電漿包含衍生自各種來源之能量,諸如放電、在射頻或微波範圍的電磁場、雷射、或粒子束。大致上,PECVD利用於中等功率密度(每平方公分0.1至5瓦特(W/cm2))之射頻(10千赫茲(kHz)至102百萬赫茲(MHz))或微波能量(0.1至10千兆赫茲(GHz)),但這些變數的任一者皆可修改。然而,具體頻率、功率、以及壓力通常係依沉積裝置而量身打造。
在AACVD中,矽前驅物化合物係溶解在化學介質中以形成混合物。將包含矽前驅物化合物與化學介質之混合物封裝於傳統氣溶膠中。氣溶膠將矽前驅物化合物原子化並引入至經加熱艙中,在該經加熱艙中,矽前驅物化合物經歷分解及/或化學反應。AACVD的一個優點係無需真空就能形成膜之能力。
所選沉積製程以及操作參數將對膜之結構與性質有所影響。通常,控制膜結構的定向、膜聚結之方式、膜的均勻性、以及膜的結晶/非結晶結構係可能的。
應注意的是,也可在沉積艙中使用促進所欲沉積之環境。舉例來說,於本文中,諸如空氣、氧、氧電漿、氨、胺、肼等之反應性環境或惰性環境皆可使用。
額外地,本發明提供一種根據本方法所形成之膜。膜的組成及結構不僅隨沉積裝置及其參數而變動,亦隨所利用的矽前驅物化合物以及於本方法期間存在或不存在任何反應性環境而變動。矽前驅物化合物可與任何其他已知前驅物化合物組合利用,或可在沒有任何其他前驅物化合物之本方法中利用。
由於矽前驅物化合物含有至少一個Si-N鍵,因此矽前驅物化合物可在未使用氮前驅物的條件下用來形成氮化矽膜,但是若有需要亦可使用氮前驅物。亦即,可能沒有必要添加氮前驅物(例如第二蒸氣),以形成氮化矽膜。沉積條件可經最佳化以控制本發明之方法形成的是元素Si膜或SiN膜。若有需要,氮前驅物可用於第二蒸氣中以富集SiN膜的氮含量。
可替代地,矽前驅物化合物可與傳統上用來形成包含結晶矽或氮化矽之矽膜的其他基於矽之前驅物化合物一起使用。在此等實施例中,膜可以是例如結晶的或磊晶的。視在本方法期間之反應性環境的存在而定,除了包含矽及氮外,膜可進一步包含氧及/或碳。
矽前驅物化合物之純度可以藉由29Si-NMR、逆相液相層析術、或更可能的是藉由如後所述的氣相層析術(GC)來測定。例如,由GC測定的純度可以從60面積%至100面積%(GC)、可替代地從70面積%至100面積%(GC)、可替代地從80面積%至100面積%(GC)、可替代地從90面積%至100面積%(GC)、可替代地從93面積%至100面積%(GC)、可替代地從95面積%至100面積%(GC)、可替代地從97面積%至100面積%(GC)、可替代地從99.0面積%至100面積%(GC)。各100面積%(GC)可獨立地如先前所定義。
藉由以下的非限制性實例來進一步說明本發明,並且本發明實施例可以包括以下限制性實例之特徵和限制的任意組合。環境溫度係約23℃,除非另有指明。
氣相層析術-火焰離子化偵測器(GC-FID)條件:長度30公尺、內徑0.32mm的毛細管柱,並且在該毛細管柱的內表面上含有塗層形式的0.25μm厚固定相,其中該固定相由苯基甲基矽氧烷所組成。載氣是以每分鐘105mL的流速使用的氦氣。GC儀器是Agilent型號7890A氣相層析儀。入口溫度係200℃。GC實驗溫度曲線係由
下列所組成:在50℃持溫(保持)2分鐘、以15℃/分鐘的速率升溫到250℃、並在250℃持溫(保持)10分鐘。
GC-MS儀器和條件:藉由電子撞擊離子化及化學離子化氣相層析-質譜法(EI GC-MS及CI GC-MS)分析樣本。Agilent 6890 GC條件包括具有30公尺(m)×0.25毫米(mm)×0.50微米(μm)膜組態之DB-1管柱、入口溫度200℃、烘箱程式為在50℃持溫2分鐘、以15℃/分鐘升溫至250℃、並在250℃持溫10分鐘。氦載氣流量為1mL/分鐘的恆定流速和50:1的分離噴射。Agilent 5973 MSD條件包括15至800道耳頓之MS掃描範圍、EI離子化、及CI離子化(使用5% NH3及95% CH4之訂製CI氣體混合)。
29Si-NMR儀器及溶劑:使用Varian 400MHz汞光譜儀。使用C6D6做為溶劑。
1H-NMR儀器及溶劑:使用Varian 400MHz汞光譜儀。使用C6D6做為溶劑。
在15mL閃爍小瓶中,將0.20g(0.7mmol)之1,2-雙(二異丙基胺)二矽烷(BisDPDS)稀釋於2mL之戊烷中並使用磁攪拌棒攪拌。添加0.21g(0.7mmol)之六氯二矽烷並攪拌30分鐘。GC-MS分析顯示幾乎消耗掉所有BisDPDS以給出作為唯一主要產物之產物DPDCH4(>90%轉化率)。
將二異丙基胺基五氯二矽烷(DPDC,0.52g,1.6mmol)添加至配備有磁攪拌棒之30-mL閃爍小瓶中。將熱電偶絲夾置於小瓶底部與陶瓷攪拌板頂部之間,以監測反應溫度。將氫化二異丁基鋁(DiBAH,0.23g,1.6mmol)逐滴添加至攪拌中之DPDC中,其中觀察到放熱。使用GC-FID及GC-MS分析反應混合物發現下列組成物:2.00%(i-Pr2-N)SiCl2H、1.45%(i-Pr2-N)SiCl3、22.50%(i-Pr2-N)Si2Cl2H3(DPDCH3)、微量(i-Pr2-N)Si2Cl3H2(DPDCH2)、3.15%(i-Pr2-N)Si2Cl4H(DPDCH)、68.83%(i-Pr2-N)Si2Cl5(DPDC)、及2.07%其他氯矽烷。
在填充氬之手套箱中,將配備有磁攪拌器之1-L包有外套之圓底燒瓶裝填66.8%純的二異丙基胺基五氯二矽烷(DPDC,268.6g,約0.54mol)並冷卻至-15℃。將氫化二異丁基鋁(DiBAH,229.1g,1.61mol)在3小時期間使用大的塑膠吸量管以每次30g等分添加至劇烈攪拌中之DPDC中,以保持反應溫度在10℃以下。在添加結束時,以每次增加10℃之方式調高冷卻器設定,使反應混合物回到室溫(可能觀察到二次放熱)。一旦反應混合物達到溫度,將燒瓶之內容物轉移至(未包有外套之)配備有熱電偶、磁攪拌棒及蒸餾塔之1-
L三頸圓底燒瓶中。藉由在全主動真空下在74至82℃之鍋溫度下汽提蒸餾,自高沸點副產物中單離出80%粗製1-二異丙基胺基-1,1-二氯二矽烷(DPDCH3)。產量:129.0g(83.0%)。
在500ml圓底燒瓶中添加11.1g(47.4mmol)之五氯二矽烷(PCDS)及110ml之無水己烷。將燒瓶在乾冰-異丙醇浴中冷卻至-10℃。在攪拌下,在15分鐘內在-10℃下添加含有9.60g(94.9mmol)之二異丙基胺及20ml之無水己烷之溶液。形成黃白色漿液。在添加後,將反應混合物溫熱至室溫並在室溫下持續攪拌2小時。接著將漿液過濾通過覆蓋0.5英吋厚之乾燥矽藻土的D型玻料。將鹽餅用20ml之無水己烷洗滌二次。將130ml透明濾液在真空下(低至1托)在高至室溫下汽提,直到去除所有低沸溶劑。單離出呈透明無色液體產物之鍋殘餘物(6.70g)。將產物用GC-TCD、GC-MS及1H NMR分析。產物含有76.2%之胺基氯氫二矽烷,其包括44.3%之1-二異丙基胺基-1,2,2,2-四氯二矽烷iPr2N-SiClH-SiCl3、17.1%之1-二異丙基胺基-1,1,2,2-四氯二矽烷HCl2Si-SiCl2-NPri 2及14.8%之雙(二異丙基胺基)三氯二矽烷異構物HSi2(NPri 2)2Cl3。
在15分鐘內在-5℃下,將1.80g(10.9mmol)之1,1,1-三氯二矽烷(3CDS)於5ml之己烷中之溶液添加至在250ml圓底燒瓶中之2.12g(35.9mmol)之乙基甲基胺及3.63g(35.9mmol)之三乙胺於90ml之己烷中之溶液中。在添加後,將反應混合物(漿液)在室溫至40℃下攪拌30分鐘。接著將反應混合物過濾以給出透明液體。將液體中之揮發性內容物在真空低至1托下去除。單離出透明液體(0.96g)。據GC-FID估計,液體含有約30wt%之1,1-雙(乙基甲基胺基)-1-氯二矽烷。1,1-雙(乙基甲基胺基)-1-氯二矽烷之結構係由GC-MS及1H NMR表徵。
在15分鐘內在-5℃下,將1.84g(11.1mmol)之1,1,1-三氯二矽烷(3CDS)於10ml之己烷中之溶液添加至在250ml圓底燒瓶中之5.35g(73.2mmol)之二乙胺於100ml之己烷中之溶液中。在添加後,將反應混合物(漿液)在室溫下攪拌1.5小時。接著將反應混合物過濾以給出透明液體。將液體中之揮發性內容物在真空低至1托下去除。單離出透明液體(1.35g)。據GC-FID估計,液體含有約59wt%之1,1-雙(二乙基胺基)-1-氯二矽烷。1,1-雙(二乙基胺基)-1-氯二矽烷之結構係由GC-MS及1H NMR表徵。
使用PEALD反應器、及含有DPDCH3且與PEALD反應器流體連通之小圓筒,加熱含有DPDCH3之圓筒至77℃。將PEALD反應器用氮(N2)吹掃,其中PEALD反應器含有在350℃(設定點)下加熱的複數個水平定向並間隔開的矽晶圓。接著按下列順序,用DPDCH3來生長PEALD SiN膜:DPDCH3劑量1至10sec/N2吹掃30sec/含N2或NH3+N2之電漿15sec/N2吹掃30sec。重複前述步驟順序直到在晶圓上形成具有所欲厚度之適形氮化矽膜。
氮化矽膜之厚度及折射率(在波長632nm下)係使用光譜分析橢圓偏光計(M-2000DI,J.A.Woollam)來表徵。收集在波長範圍375nm至1690nm之橢圓偏光計資料,並使用Tauc-Lorentz振盪器模型與J.A.Woollam提供之軟體來分析。使用以D.I.水稀釋之500:1 HF溶液,在室溫下對PEALD製程生長之薄膜進行濕式蝕刻速率測試。濕式蝕刻速率係自在稀釋HF溶液中蝕刻之前及之後的厚度差異計算。結果呈現在下表中。
實例8(預示):使用矽前驅物化合物與氨(NH3)以及LPCVD來形成氮化矽膜:使用LPCVD反應器、及含有矽前驅物化合物且與LPCVD反應器流體連通之鼓泡器,加熱含有矽前驅物化合物之鼓泡器至70℃以增加該矽前驅物化合物之蒸氣壓。然後使He載氣流過鼓泡器,以攜帶矽前驅物化合物的蒸氣進入LPCVD反應器,其中LPCVD反應器含有蒸氣氨及經加熱到500℃的複數個垂直定向並間隔開的矽晶圓,以在晶圓上形成適形氮化矽膜。
實例9(預示):使用矽前驅物化合物與氨以及PECVD來形成氮化矽膜:使用PECVD反應器、及與PECVD反應器流體連通之鼓泡器,加熱含有矽前驅物化合物之鼓泡器至70℃以增加該矽前驅物化合物之蒸氣壓。然後使He載氣流過鼓泡器,以攜帶矽前驅物化合物的蒸氣進入PECVD反應器,其中PECVD反應器具有衍生自氨的電漿並含有經加熱到500℃的複數個水平定向並間隔開的矽晶圓,以在晶圓上形成適形氮化矽膜。
實例10(預示):使用矽前驅物化合物以及LPCVD來形成氧化矽膜:使用LPCVD反應器、及與LPCVD反應器流體連通之鼓泡器,加熱含有矽前驅物化合物之鼓泡器至70℃以增加該矽前驅物化合物之蒸氣壓。然後使He載氣流過鼓泡器,以攜帶矽前驅物化合物的蒸氣進入LPCVD反應器,其中LPCVD反應器具有氧氣氛並含有經加熱到500℃的複數個垂直定向並間隔開的矽晶圓,從而在晶圓上形成適形氧化矽膜。
實例11(預示):使用矽前驅物化合物與甲烷以及PECVD來形成碳化矽膜:使用PECVD反應器、及與PECVD反應器流體連通之鼓泡器,加熱含有矽前驅物化合物之鼓泡器至70℃以增加該矽前驅物化合物之蒸氣壓。然後使He載氣流過鼓泡器,以攜帶矽前驅物化合物的蒸氣進入PECVD反應器,其中PECVD反應器具有衍生自甲烷的電漿並含有經加熱到500℃的複數個水平定向並間隔開的矽晶圓,以在晶圓上形成適形碳化矽膜。
以下的申請專利範圍係以引用方式併入本文中,並且用語「請求項(claim)」可以用語「態樣(aspect)」取代。本發明之實施例也包括這些產生的有編號態樣。
Claims (15)
- 一種化合物,其係二矽烷且包含至少一個氯基、至少一個二烷基胺基及至少一個氫基(hydrido group)。
- 如請求項1之化合物,其中該化合物具有式(R1R2N)aClbHcSiSiHdCle(R1R2N)f,其中各R1獨立地係H、(C1-C6)烷基、(C3-C6)環烷基、(C2-C6)烯基、(C2-C6)炔基、或苯基;且各R2獨立地係(C1-C6)烷基、(C3-C6)環烷基、(C2-C6)烯基、(C2-C6)炔基、或苯基;或在相同或不同氮原子上之R1及R2鍵結在一起成為-R1a-R2a-,其中-R1a-R2a-係(C2-C5)伸烷基;且其中a、b、c、d、e及f係整數,其等範圍獨立地自零至三;條件為a及f中至少一者不是零,b及e中至少一者不是零,且c及d中至少一者不是零。
- 如請求項2之化合物,其包括限制a)、b)、c)及d)中之一或多者:a)R1及R2獨立地係C2-C6烷基;b)a及f中只有一者係一,且另一者係零;c)b及e獨立地係零、一或二;d)b+e係自一至四。
- 如請求項3之化合物,其中R1及R2獨立地係C3-C4烷基。
- 如請求項1之化合物,其係[(CH3)2CH]2NSiCl2SiH3、[(CH3)2CH]2NSiH2SiH2Cl、[(CH3CH2)2N]2SiClSiH3、[(CH3CH2)(CH3)N]2SiClSiH3、HSiClN[CH(CH3)2]2SiCl3、HSiCl2SiCl2N[CH(CH3)2]2、或HSi2Cl3[N(CH(CH3)2)2]2。
- 一種用於生產化合物之方法,該化合物係二矽烷且包含至少一個氯基、至少一個二烷基胺基及至少一個氫基;該方法包含將具有至少二個氯基及至少一個二烷基胺基的二矽烷與氫化鋁接觸。
- 如請求項6之方法,其中該氫化鋁包含氫化鋁鋰、氫化三-三級丁氧基鋁鋰、氫化參[(3-乙基-3-戊基)氧基]鋁鋰、氫化雙(2-甲氧基乙氧基)鋁鈉、氫化二異丁基鋁、氫化二乙基鋁、或者氫化鋁鋰、氫化三-三級丁氧基鋁鋰、氫化參[(3-乙基-3-戊基)氧基]鋁鋰、氫化雙(2-甲氧基乙氧基)鋁鈉、氫化二異丁基鋁、及氫化二乙基鋁中之二或更多者之組合。
- 一種於基材上形成含矽膜之方法,該方法包含在該基材存在下,使包含如前述請求項中任一項之化合物之矽前驅物之蒸氣經歷沉積條件,以在該基材上形成含矽膜。
- 如請求項8之方法,其包括限制e)、f)、g)、h)及i)中之一或多者:e)其中該含矽膜係元素矽膜、矽碳膜、矽氮膜、或矽氧膜;f)包含在該基材存在下,使包含如請求項1至6中任一項之化合物之矽前驅物之第一蒸氣與包含氦或氫的第二蒸氣經歷沉積條件,以在該基材上形成含矽膜,其中該含矽膜係元素矽膜;g)包含在該基材存在下,使包含如請求項1至6中任一項之化合物之矽前驅物之第一蒸氣與包含烴、烴基矽烷、或其任兩者之組合之碳前驅物之第二蒸氣經歷沉積條件,以在該基材上形成含矽膜,其中該含矽膜係矽碳膜; h)包含在該基材存在下,使包含如請求項1至6中任一項之化合物之矽前驅物之第一蒸氣與包含分子氮、氨、肼、胺、或其任二或三者之組合之氮前驅物之第二蒸氣經歷沉積條件,以在該基材上形成含矽膜,其中該含矽膜係矽氮膜;i)包含在該基材存在下,使包含如請求項1至6中任一項之化合物之矽前驅物之第一蒸氣與包含分子氧、臭氧、一氧化氮、二氧化氮、一氧化二氮、水、過氧化氫、或其任二或三者之組合之氧前驅物之第二蒸氣經歷沉積條件,以在該基材上形成含矽膜,其中該含矽膜係矽氧膜。
- 如請求項8至9中任一項之方法,其中該基材係經加熱及設置於經組態用於原子層沉積之沉積反應器中,該方法包含重覆地饋送包含如請求項1至6中任一項之化合物之矽前驅物之該第一蒸氣;以惰性氣體吹掃;饋送該第二蒸氣至該沉積反應器中;以及以惰性氣體吹掃,以利用原子層沉積在該經加熱基材上形成該含矽膜,其中該等饋送可相同或不同。
- 如請求項8至9中任一項之方法,其中該基材係經加熱及設置於經組態用於化學氣相沉積之沉積反應器中,該方法包含饋送包含如請求項1至6中任一項之化合物之矽前驅物之該第一蒸氣;以及饋送該第二蒸氣至該沉積反應器中,以利用化學氣相沉積在該經加熱基材上形成該含矽膜,其中該等饋送可相同或不同。
- 如請求項10或11之方法,其中該等氣相沉積條件缺乏碳和氧,且該矽氮膜包含氮化矽膜。
- 如前述請求項中任一項之方法,其中該基材係半導體材料。
- 一種用於形成矽氮膜之組成物,該組成物包含:包含如請求項1至6中任一項之化合物之矽前驅物、以及氮前驅物。
- 一種如請求項1至6中任一項之組成物用於形成矽氮膜的方法中之用途。
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