CN116113725A - 用于锗种子层的组合物及其使用方法 - Google Patents
用于锗种子层的组合物及其使用方法 Download PDFInfo
- Publication number
- CN116113725A CN116113725A CN202180062806.1A CN202180062806A CN116113725A CN 116113725 A CN116113725 A CN 116113725A CN 202180062806 A CN202180062806 A CN 202180062806A CN 116113725 A CN116113725 A CN 116113725A
- Authority
- CN
- China
- Prior art keywords
- silane
- bis
- allylsilane
- butylamino
- organoamino
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 238000000034 method Methods 0.000 title claims abstract description 92
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229910052732 germanium Inorganic materials 0.000 title claims abstract description 82
- 239000000203 mixture Substances 0.000 title claims description 35
- 239000002243 precursor Substances 0.000 claims abstract description 175
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 96
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 95
- 239000010703 silicon Substances 0.000 claims abstract description 82
- 239000000758 substrate Substances 0.000 claims abstract description 70
- -1 C 1 -C 10 Linear Chemical group 0.000 claims description 170
- 238000010926 purge Methods 0.000 claims description 42
- 239000007789 gas Substances 0.000 claims description 39
- 239000001257 hydrogen Substances 0.000 claims description 39
- 229910052739 hydrogen Inorganic materials 0.000 claims description 39
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 37
- DNAJDTIOMGISDS-UHFFFAOYSA-N prop-2-enylsilane Chemical compound [SiH3]CC=C DNAJDTIOMGISDS-UHFFFAOYSA-N 0.000 claims description 35
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 31
- 238000006243 chemical reaction Methods 0.000 claims description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 28
- 239000007983 Tris buffer Substances 0.000 claims description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 25
- 125000003118 aryl group Chemical group 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- 229910052760 oxygen Inorganic materials 0.000 claims description 20
- 239000001301 oxygen Substances 0.000 claims description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 18
- 125000000753 cycloalkyl group Chemical group 0.000 claims description 17
- 125000000217 alkyl group Chemical group 0.000 claims description 16
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- 238000004873 anchoring Methods 0.000 claims description 14
- 229910000078 germane Inorganic materials 0.000 claims description 14
- 125000004122 cyclic group Chemical group 0.000 claims description 13
- 125000000031 ethylamino group Chemical group [H]C([H])([H])C([H])([H])N([H])[*] 0.000 claims description 13
- 150000002431 hydrogen Chemical class 0.000 claims description 13
- 125000000719 pyrrolidinyl group Chemical group 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 12
- 125000000168 pyrrolyl group Chemical group 0.000 claims description 12
- 125000000008 (C1-C10) alkyl group Chemical group 0.000 claims description 10
- 125000000882 C2-C6 alkenyl group Chemical group 0.000 claims description 10
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 10
- 125000003545 alkoxy group Chemical group 0.000 claims description 10
- 125000003342 alkenyl group Chemical group 0.000 claims description 9
- 238000005137 deposition process Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 125000000304 alkynyl group Chemical group 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- QKXWQSAMRUXIGU-UHFFFAOYSA-N n-[ethenyl-bis(ethylamino)silyl]ethanamine Chemical compound CCN[Si](NCC)(NCC)C=C QKXWQSAMRUXIGU-UHFFFAOYSA-N 0.000 claims description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 6
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 6
- 125000005843 halogen group Chemical group 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- 229910052740 iodine Inorganic materials 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 4
- OPDQOJBKHNWJGO-UHFFFAOYSA-N butylgermane Chemical group CCCC[GeH3] OPDQOJBKHNWJGO-UHFFFAOYSA-N 0.000 claims description 3
- XCLKKWIIZMHQIV-UHFFFAOYSA-N isobutylgermane Chemical compound CC(C)C[Ge] XCLKKWIIZMHQIV-UHFFFAOYSA-N 0.000 claims description 3
- QGBOLMACEVFNFV-UHFFFAOYSA-N phenylgermane Chemical compound [GeH3]C1=CC=CC=C1 QGBOLMACEVFNFV-UHFFFAOYSA-N 0.000 claims description 3
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 3
- MUDDKLJPADVVKF-UHFFFAOYSA-N trichlorogermane Chemical compound Cl[GeH](Cl)Cl MUDDKLJPADVVKF-UHFFFAOYSA-N 0.000 claims description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims 49
- HKILWKSIMZSWQX-UHFFFAOYSA-N tris(prop-2-enyl)silane Chemical compound C=CC[SiH](CC=C)CC=C HKILWKSIMZSWQX-UHFFFAOYSA-N 0.000 claims 24
- OYNOOQVZYWROOB-UHFFFAOYSA-N methyl(prop-2-enyl)silane Chemical compound C[SiH2]CC=C OYNOOQVZYWROOB-UHFFFAOYSA-N 0.000 claims 16
- 125000000250 methylamino group Chemical group [H]N(*)C([H])([H])[H] 0.000 claims 13
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 claims 11
- 125000000587 piperidin-1-yl group Chemical group [H]C1([H])N(*)C([H])([H])C([H])([H])C([H])([H])C1([H])[H] 0.000 claims 11
- 125000006318 tert-butyl amino group Chemical group [H]N(*)C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 claims 10
- 125000001664 diethylamino group Chemical group [H]C([H])([H])C([H])([H])N(*)C([H])([H])C([H])([H])[H] 0.000 claims 6
- GSRSOXQVWQFEOV-UHFFFAOYSA-N 2-methylprop-1-enyl(pyrrolidin-1-yl)silane Chemical compound N1(CCCC1)[SiH2]C=C(C)C GSRSOXQVWQFEOV-UHFFFAOYSA-N 0.000 claims 3
- SAUMZHHXEMRHQF-UHFFFAOYSA-N C(C)N[SiH](C=CC)NCC Chemical compound C(C)N[SiH](C=CC)NCC SAUMZHHXEMRHQF-UHFFFAOYSA-N 0.000 claims 3
- ODVDDQFBQGTLIA-UHFFFAOYSA-N n-[bis(ethenyl)-(ethylamino)silyl]ethanamine Chemical compound CCN[Si](C=C)(C=C)NCC ODVDDQFBQGTLIA-UHFFFAOYSA-N 0.000 claims 3
- NTJNMOZFIYDTGH-UHFFFAOYSA-N 2-methyl-N-tris(ethenyl)silylpropan-2-amine Chemical compound CC(C)(C)N[Si](C=C)(C=C)C=C NTJNMOZFIYDTGH-UHFFFAOYSA-N 0.000 claims 2
- UOXRUVMPHHGCKY-UHFFFAOYSA-N 2-methylprop-1-enyl(piperidin-1-yl)silane Chemical compound N1(CCCCC1)[SiH2]C=C(C)C UOXRUVMPHHGCKY-UHFFFAOYSA-N 0.000 claims 2
- NZHWWOPEBOADOJ-UHFFFAOYSA-N C(C)(C)(C)N[SiH](C=CC)NC(C)(C)C Chemical compound C(C)(C)(C)N[SiH](C=CC)NC(C)(C)C NZHWWOPEBOADOJ-UHFFFAOYSA-N 0.000 claims 2
- BSCQDYSKWDRMDV-UHFFFAOYSA-N CC(C)=C[SiH2]N(C)C1=CC=CC=C1 Chemical compound CC(C)=C[SiH2]N(C)C1=CC=CC=C1 BSCQDYSKWDRMDV-UHFFFAOYSA-N 0.000 claims 2
- AKBAFTBHPSTTCX-UHFFFAOYSA-N N-[(butan-2-ylamino)-bis(ethenyl)silyl]butan-2-amine Chemical compound CCC(C)N[Si](C=C)(C=C)NC(C)CC AKBAFTBHPSTTCX-UHFFFAOYSA-N 0.000 claims 2
- UMGCUSXIKFKDGV-UHFFFAOYSA-N N-[[cyclohexyl(methyl)amino]-bis(ethenyl)silyl]-N-methylcyclohexanamine Chemical compound CN(C1CCCCC1)[Si](C=C)(C=C)N(C)C1CCCCC1 UMGCUSXIKFKDGV-UHFFFAOYSA-N 0.000 claims 2
- RHZBDQBCTCXAAY-UHFFFAOYSA-N N-methyl-N-tris(ethenyl)silylcyclohexanamine Chemical compound CN(C1CCCCC1)[Si](C=C)(C=C)C=C RHZBDQBCTCXAAY-UHFFFAOYSA-N 0.000 claims 2
- SFKOLMXZWVVBGN-UHFFFAOYSA-N N-methyl-N-tris(ethenyl)silylethanamine Chemical compound CCN(C)[Si](C=C)(C=C)C=C SFKOLMXZWVVBGN-UHFFFAOYSA-N 0.000 claims 2
- AGSKAUPPLNMACM-UHFFFAOYSA-N N-tris(ethenyl)silylbutan-2-amine Chemical compound CCC(C)N[Si](C=C)(C=C)C=C AGSKAUPPLNMACM-UHFFFAOYSA-N 0.000 claims 2
- OUYCYQTXQGTBHM-UHFFFAOYSA-N N-tris(ethenyl)silylpropan-1-amine Chemical compound CCCN[Si](C=C)(C=C)C=C OUYCYQTXQGTBHM-UHFFFAOYSA-N 0.000 claims 2
- NYWGBOSKMBLDRY-UHFFFAOYSA-N N-tris(ethenyl)silylpropan-2-amine Chemical compound CC(C)N[Si](C=C)(C=C)C=C NYWGBOSKMBLDRY-UHFFFAOYSA-N 0.000 claims 2
- XFXVNEYLBGNECH-UHFFFAOYSA-N N1(CCCCC1)[SiH](C=CC)N1CCCCC1 Chemical compound N1(CCCCC1)[SiH](C=CC)N1CCCCC1 XFXVNEYLBGNECH-UHFFFAOYSA-N 0.000 claims 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims 2
- IQSBKDJPSOMMRZ-UHFFFAOYSA-N ethenyl(methyl)silane Chemical compound C[SiH2]C=C IQSBKDJPSOMMRZ-UHFFFAOYSA-N 0.000 claims 2
- JFCCVNTYPIUJDJ-UHFFFAOYSA-N methyl-tris(prop-2-enyl)silane Chemical compound C=CC[Si](C)(CC=C)CC=C JFCCVNTYPIUJDJ-UHFFFAOYSA-N 0.000 claims 2
- QTEINWXJSZQFQN-UHFFFAOYSA-N n-[bis(ethenyl)-(propylamino)silyl]propan-1-amine Chemical compound CCCN[Si](C=C)(C=C)NCCC QTEINWXJSZQFQN-UHFFFAOYSA-N 0.000 claims 2
- DPNKKXIIBBSUPO-UHFFFAOYSA-N n-[bis(tert-butylamino)-ethenylsilyl]-2-methylpropan-2-amine Chemical compound CC(C)(C)N[Si](NC(C)(C)C)(NC(C)(C)C)C=C DPNKKXIIBBSUPO-UHFFFAOYSA-N 0.000 claims 2
- UTVIFRALDCOELJ-UHFFFAOYSA-N n-[bis[cyclohexyl(methyl)amino]-ethenylsilyl]-n-methylcyclohexanamine Chemical compound C1CCCCC1N(C)[Si](C=C)(N(C)C1CCCCC1)N(C)C1CCCCC1 UTVIFRALDCOELJ-UHFFFAOYSA-N 0.000 claims 2
- FYYCXYLMGPRWLV-UHFFFAOYSA-N n-[diethylamino-bis(ethenyl)silyl]-n-ethylethanamine Chemical compound CCN(CC)[Si](C=C)(C=C)N(CC)CC FYYCXYLMGPRWLV-UHFFFAOYSA-N 0.000 claims 2
- PGNUFNGYXBXBGR-UHFFFAOYSA-N n-[ethenyl-bis(propan-2-ylamino)silyl]propan-2-amine Chemical compound CC(C)N[Si](NC(C)C)(NC(C)C)C=C PGNUFNGYXBXBGR-UHFFFAOYSA-N 0.000 claims 2
- ZRQZPBXNRJHJTF-UHFFFAOYSA-N n-[ethenyl-bis[ethyl(methyl)amino]silyl]-n-methylethanamine Chemical compound CCN(C)[Si](C=C)(N(C)CC)N(C)CC ZRQZPBXNRJHJTF-UHFFFAOYSA-N 0.000 claims 2
- PTTVEOLXVXTTPN-UHFFFAOYSA-N n-ethyl-n-tris(ethenyl)silylethanamine Chemical compound CCN(CC)[Si](C=C)(C=C)C=C PTTVEOLXVXTTPN-UHFFFAOYSA-N 0.000 claims 2
- PTLBSZDLZXSEDD-UHFFFAOYSA-N n-tris(ethenyl)silylethanamine Chemical compound CCN[Si](C=C)(C=C)C=C PTLBSZDLZXSEDD-UHFFFAOYSA-N 0.000 claims 2
- YZYGYNOZNQGQOU-UHFFFAOYSA-N n-tris(ethenyl)silylmethanamine Chemical compound CN[Si](C=C)(C=C)C=C YZYGYNOZNQGQOU-UHFFFAOYSA-N 0.000 claims 2
- JGYKLVHJPUDFEU-UHFFFAOYSA-N tris(ethenyl)-(1H-pyrrol-2-yl)silane Chemical compound C=C[Si](C=C)(C=C)C1=CC=CN1 JGYKLVHJPUDFEU-UHFFFAOYSA-N 0.000 claims 2
- ZLXQVVMEORAYTI-UHFFFAOYSA-N tris(ethenyl)-piperidin-1-ylsilane Chemical compound C=C[Si](C=C)(C=C)N1CCCCC1 ZLXQVVMEORAYTI-UHFFFAOYSA-N 0.000 claims 2
- 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 1
- VABNYZYGZFRYNP-UHFFFAOYSA-N C=C[SiH](C=C)N1CCCC1 Chemical compound C=C[SiH](C=C)N1CCCC1 VABNYZYGZFRYNP-UHFFFAOYSA-N 0.000 claims 1
- XDGPQXMOEIXOAM-UHFFFAOYSA-N CC(C)(C)N[SiH2]C=C(C)C Chemical compound CC(C)(C)N[SiH2]C=C(C)C XDGPQXMOEIXOAM-UHFFFAOYSA-N 0.000 claims 1
- QNUNQCXYHRSGIO-UHFFFAOYSA-N CC(C)=C[SiH2]C1=CC=CN1 Chemical compound CC(C)=C[SiH2]C1=CC=CN1 QNUNQCXYHRSGIO-UHFFFAOYSA-N 0.000 claims 1
- DLSGFLOESWNCNH-UHFFFAOYSA-N CC(C)=C[SiH2]N(C)C1CCCCC1 Chemical compound CC(C)=C[SiH2]N(C)C1CCCCC1 DLSGFLOESWNCNH-UHFFFAOYSA-N 0.000 claims 1
- UUPHRLOZHBBKIP-UHFFFAOYSA-N CCC(C)N[SiH2]C=C(C)C Chemical compound CCC(C)N[SiH2]C=C(C)C UUPHRLOZHBBKIP-UHFFFAOYSA-N 0.000 claims 1
- BYWHZMZHZXJWCT-UHFFFAOYSA-N CCCN[SiH2]C=C(C)C Chemical compound CCCN[SiH2]C=C(C)C BYWHZMZHZXJWCT-UHFFFAOYSA-N 0.000 claims 1
- OLKFTRIEBIGKIJ-UHFFFAOYSA-N CN[SiH](C=CC)NC Chemical compound CN[SiH](C=CC)NC OLKFTRIEBIGKIJ-UHFFFAOYSA-N 0.000 claims 1
- URLLRCCOOOZVBX-UHFFFAOYSA-N N-[(butan-2-ylamino)-prop-1-enylsilyl]butan-2-amine Chemical compound CC=C[SiH](NC(C)CC)NC(C)CC URLLRCCOOOZVBX-UHFFFAOYSA-N 0.000 claims 1
- VOKVWBFNWOQFKH-UHFFFAOYSA-N N-[(propan-2-ylamino)-prop-1-enylsilyl]propan-2-amine Chemical compound C(C)(C)N[SiH](C=CC)NC(C)C VOKVWBFNWOQFKH-UHFFFAOYSA-N 0.000 claims 1
- UIJZTGYUVYQTGY-UHFFFAOYSA-N N-[bis(ethenyl)-(N-methylanilino)silyl]-N-methylaniline Chemical compound CN(C1=CC=CC=C1)[Si](C=C)(C=C)N(C)C1=CC=CC=C1 UIJZTGYUVYQTGY-UHFFFAOYSA-N 0.000 claims 1
- ZGTQYHJFJJECJZ-UHFFFAOYSA-N N-[prop-1-enyl(propylamino)silyl]propan-1-amine Chemical compound C(CC)N[SiH](C=CC)NCCC ZGTQYHJFJJECJZ-UHFFFAOYSA-N 0.000 claims 1
- KDKMJJRTZITCRZ-UHFFFAOYSA-N N-methyl-N-(2-methylprop-1-enylsilyl)ethanamine Chemical compound C(C)N(C)[SiH2]C=C(C)C KDKMJJRTZITCRZ-UHFFFAOYSA-N 0.000 claims 1
- RZPNHMZPOILSDG-UHFFFAOYSA-N benzylgermanium Chemical compound [Ge]CC1=CC=CC=C1 RZPNHMZPOILSDG-UHFFFAOYSA-N 0.000 claims 1
- YODQWAGGAJVSRC-UHFFFAOYSA-N bis(ethenyl)-bis(1H-pyrrol-2-yl)silane Chemical compound C=C[Si](C=C)(C1=CC=CN1)C1=CC=CN1 YODQWAGGAJVSRC-UHFFFAOYSA-N 0.000 claims 1
- BETODKSPKWVXNX-UHFFFAOYSA-N bis(ethenyl)-di(piperidin-1-yl)silane Chemical compound C1CCCCN1[Si](C=C)(C=C)N1CCCCC1 BETODKSPKWVXNX-UHFFFAOYSA-N 0.000 claims 1
- QIYXRFMWGJJGGK-UHFFFAOYSA-N bis(ethenyl)-dipyrrolidin-1-ylsilane Chemical compound C1CCCN1[Si](C=C)(C=C)N1CCCC1 QIYXRFMWGJJGGK-UHFFFAOYSA-N 0.000 claims 1
- PMSZNCMIJVNSPB-UHFFFAOYSA-N bis(ethenyl)silicon Chemical compound C=C[Si]C=C PMSZNCMIJVNSPB-UHFFFAOYSA-N 0.000 claims 1
- FIRXZHKWFHIBOF-UHFFFAOYSA-N n-(dimethylamino-ethenyl-methylsilyl)-n-methylmethanamine Chemical compound CN(C)[Si](C)(C=C)N(C)C FIRXZHKWFHIBOF-UHFFFAOYSA-N 0.000 claims 1
- GYAFWFQRCYPXHP-UHFFFAOYSA-N n-[(tert-butylamino)-bis(ethenyl)silyl]-2-methylpropan-2-amine Chemical compound CC(C)(C)N[Si](C=C)(C=C)NC(C)(C)C GYAFWFQRCYPXHP-UHFFFAOYSA-N 0.000 claims 1
- ALIGWNJACSYFPX-UHFFFAOYSA-N n-[bis(butan-2-ylamino)-ethenylsilyl]butan-2-amine Chemical compound CCC(C)N[Si](NC(C)CC)(NC(C)CC)C=C ALIGWNJACSYFPX-UHFFFAOYSA-N 0.000 claims 1
- CDQWREDVZBTNEU-UHFFFAOYSA-N n-[bis(diethylamino)-ethenylsilyl]-n-ethylethanamine Chemical compound CCN(CC)[Si](C=C)(N(CC)CC)N(CC)CC CDQWREDVZBTNEU-UHFFFAOYSA-N 0.000 claims 1
- WBVXRXLWILVPMX-UHFFFAOYSA-N n-[bis(dimethylamino)-ethenylsilyl]-n-methylmethanamine Chemical compound CN(C)[Si](C=C)(N(C)C)N(C)C WBVXRXLWILVPMX-UHFFFAOYSA-N 0.000 claims 1
- GWOPLFQULNLCQB-UHFFFAOYSA-N n-[bis(ethenyl)-(methylamino)silyl]methanamine Chemical compound CN[Si](NC)(C=C)C=C GWOPLFQULNLCQB-UHFFFAOYSA-N 0.000 claims 1
- WWDXBDRBEKUZOS-UHFFFAOYSA-N n-[bis(ethenyl)-(propan-2-ylamino)silyl]propan-2-amine Chemical compound CC(C)N[Si](C=C)(C=C)NC(C)C WWDXBDRBEKUZOS-UHFFFAOYSA-N 0.000 claims 1
- YTMGVLAWLCOWNT-UHFFFAOYSA-N n-[bis(ethenyl)-[ethyl(methyl)amino]silyl]-n-methylethanamine Chemical compound CCN(C)[Si](C=C)(C=C)N(C)CC YTMGVLAWLCOWNT-UHFFFAOYSA-N 0.000 claims 1
- DMSOEJVWAVNUGE-UHFFFAOYSA-N n-[dimethylamino-bis(ethenyl)silyl]-n-methylmethanamine Chemical compound CN(C)[Si](C=C)(C=C)N(C)C DMSOEJVWAVNUGE-UHFFFAOYSA-N 0.000 claims 1
- OOQUIPMSLRDFDI-UHFFFAOYSA-N n-[ethenyl(dimethyl)silyl]-n-ethylethanamine Chemical compound CCN(CC)[Si](C)(C)C=C OOQUIPMSLRDFDI-UHFFFAOYSA-N 0.000 claims 1
- GBOKDBXOVRPYTN-UHFFFAOYSA-N n-[ethenyl(dimethyl)silyl]-n-methylethanamine Chemical compound CCN(C)[Si](C)(C)C=C GBOKDBXOVRPYTN-UHFFFAOYSA-N 0.000 claims 1
- FHYTZITXNBWWNN-UHFFFAOYSA-N n-[ethenyl(dimethyl)silyl]-n-methylmethanamine Chemical compound CN(C)[Si](C)(C)C=C FHYTZITXNBWWNN-UHFFFAOYSA-N 0.000 claims 1
- MSSPHAUTEGRNOE-UHFFFAOYSA-N n-[ethenyl(dimethyl)silyl]ethanamine Chemical compound CCN[Si](C)(C)C=C MSSPHAUTEGRNOE-UHFFFAOYSA-N 0.000 claims 1
- AXJOMTPYUXBZMU-UHFFFAOYSA-N n-[ethenyl(dimethyl)silyl]methanamine Chemical compound CN[Si](C)(C)C=C AXJOMTPYUXBZMU-UHFFFAOYSA-N 0.000 claims 1
- HBYJSEGJCBTNEW-UHFFFAOYSA-N n-[ethenyl(dimethyl)silyl]propan-2-amine Chemical compound CC(C)N[Si](C)(C)C=C HBYJSEGJCBTNEW-UHFFFAOYSA-N 0.000 claims 1
- ZMWXJYXGBSRKTC-UHFFFAOYSA-N n-[ethenyl-bis(methylamino)silyl]methanamine Chemical compound CN[Si](NC)(NC)C=C ZMWXJYXGBSRKTC-UHFFFAOYSA-N 0.000 claims 1
- PNYNUPZUHYVNDH-UHFFFAOYSA-N n-[ethenyl-bis(propylamino)silyl]propan-1-amine Chemical compound CCCN[Si](NCCC)(NCCC)C=C PNYNUPZUHYVNDH-UHFFFAOYSA-N 0.000 claims 1
- IKUFUNXMBGTURX-UHFFFAOYSA-N n-methyl-n-tris(ethenyl)silylmethanamine Chemical compound CN(C)[Si](C=C)(C=C)C=C IKUFUNXMBGTURX-UHFFFAOYSA-N 0.000 claims 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims 1
- 239000001272 nitrous oxide Substances 0.000 claims 1
- YSWBDPSOTWROFH-UHFFFAOYSA-N prop-1-enyl(dipyrrolidin-1-yl)silane Chemical compound C1CCCN1[SiH](C=CC)N1CCCC1 YSWBDPSOTWROFH-UHFFFAOYSA-N 0.000 claims 1
- 125000002112 pyrrolidino group Chemical group [*]N1C([H])([H])C([H])([H])C([H])([H])C1([H])[H] 0.000 claims 1
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Images
Classifications
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- C07F7/188—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-O linkages
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- 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
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- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
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- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
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- C23C16/14—Deposition of only one other metal element
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- 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
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- C23C16/34—Nitrides
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C—CHEMISTRY; METALLURGY
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- 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
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- C23C16/4408—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber by purging residual gases from the reaction chamber or gas lines
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Abstract
本发明涉及用于(a)形成含硅膜和(b)将衬底表面官能化以形成适用于沉积Ge膜的锗种子层的前体和方法。在一个方面,提供了如本文所描述的式I的前体和/或式II的前体。
Description
背景技术
本发明涉及有机硅化合物,其可用于沉积含硅膜并生成适用于产生锗种子层的乙烯基官能化表面,这有利于在固体衬底表面上生长高质量的还原或金属锗膜。本发明还涉及使用该化合物的方法。
本文描述了新型有机氨基-乙烯基硅烷和有机氨基-烯丙基硅烷前体化合物和包含其的组合物和方法,以通过热原子层沉积(ALD)或等离子体增强原子层沉积(PEALD)工艺或其组合沉积含硅膜,例如但不限于,氧化硅、氧氮化硅、氧碳氮化硅或碳掺杂氧化硅。更具体地,本文描述了用于在约600℃或更低(包括,例如,约25℃至约350℃)的一个或多个沉积温度下形成化学计量或非化学计量的含硅膜或材料的组合物和方法,其中所得的膜用乙烯基官能团封端并适用于形成锗种子层。
使用锗烷和乙锗烷在介电衬底例如氧化硅表面上锗膜的等离子体增强化学气相沉积(PECVD)或热化学气相沉积(CVD)长期存在的问题之一是锗烷化合物与衬底表面羟基的反应性远小于在Ge-Ge键形成中Ge-H键的分解的反应性。该反应性失配的结果是在衬底上形成锗团块岛(islands)而不是平滑膜。为了克服该“岛效应”或“岛生长”(其导致所得锗膜的高水平表面粗糙度),在表面上最初铺设平滑的种子层是必要的,其提供了平滑的起始表面并允许随后锗膜均匀生长。然而,在介电衬底表面上用典型的PECVD或CVD锗前体生长该种子层仍然存在CVD的典型缺点,例如厚度控制、介电表面的低选择性、非自限性反应性和低保形性(conformality)。
已知前体和方法的实例公开于以下公开出版物、专利和专利申请中。
公开号EP1464724A2公开了适用于硅和锗膜的化学气相沉积的具有式MXaHb(NR1R2)cR3 dR4 e的含硅和含锗前体。
Famá,S等人,Appl.Phys.Lett.2002,81,586描述了用于制造p-i-n光电探测器的目的的锗在硅上的外延生长,其首先在350℃下通过化学气相沉积用GeH4沉积薄Ge/Si缓冲层,然后在600℃下化学气相沉积较厚的锗膜。
Hair,M.L.等人,Phys.Chem.1969,73,2372报道了用氯硅烷将二氧化硅官能化,与甲氧基硅烷(100-200℃)相比,其在气相中在300-400℃之间以令人满意的速率发生。
Miao,Q.J.等人,Catal.Commun.2003,4,637描述了用乙烯基三乙氧基硅烷在甲苯中在回流条件下处理气相二氧化硅(fumed silica)48小时,然后与水反应另外48小时以用乙烯基将表面官能化。
Zapilko,C.等人.J.Am.Chem.Soc.2006,128,16266描述了通过用甲苯中的乙烯基取代的三甲硅烷基胺在109℃下处理15小时用氯丙基二甲基甲硅烷基和乙烯基二甲基甲硅烷基将周期性介孔二氧化硅官能化。
美国专利号8,460,753B2描述了通过ALD或CVD沉积二氧化硅或氧化硅膜的前体和方法,其中前体是具有式R1 nR2 mSi(NR3R4)4-n-m的氨基乙烯基硅烷和具有式(R1R2SiNR3)p的环状硅氮烷,其中R1是烯基或芳族的,例如,乙烯基、烯丙基和苯基。
美国公开号20150275355A1描述了使用具有式R1 nSi(NR2R3)mH4-m-n的前体,更具体地使用有机氨基-甲基硅烷前体形成氧化硅膜的组合物和方法。
美国公开号20090162973A1描述了使用具有式GeRx 1(NR2R3)(4-X)的含锗前体在衬底上沉积锗膜或碲化锗锑膜,其中该方法涉及将衬底暴露于单独的或与氧化气体或还原气体结合的含锗前体。
美国公开号20110036289A1描述了一种在低温下使用GeH4前体通过CVD在氢处理的硅衬底上沉积锗种子层,然后在升高的温度下分别在膦或乙硼烷的存在下,使用GeH4前体随后生长n-掺杂或p-掺杂的锗外延膜的方法。
美国公开号20110084308A1公开了一种在图案化的Si衬底上选择性地生长高质量应变或应变弛豫Ge的方法,其涉及首先在350-400℃下用Si2H6和GeH4前体通过CVD生长硅-锗缓冲层,然后在350-400℃下用GeH4前体通过CVD生长Ge种子层,然后在550-600℃下用GeH4前体通过CVD生长Ge外延膜。
美国公开号20130230975A1和20140331928A1均描述了使用基于氨基锗烷的气体在衬底上形成锗种子层,然后使用基于锗烷的气体生长锗薄膜。
先前确定的专利和专利申请的公开内容通过引用并入本文。
在本领域中仍然需要用于在介电衬底表面上沉积平滑、高质量还原或金属锗膜的前体和方法。
与现有技术相比,本文所公开的本发明中的种子层前体利用硅-胺官能团作为锚定基团,以将乙烯基或烯丙基连接到表面。该化学性将富含羟基的表面转化为富含乙烯基或烯丙基的表面。然后,将锗烷或乙锗烷或具有至少一个Ge-H键的另一种锗前体引入到反应室,并在氢锗化(hydrogermylation)反应中与乙烯基和/或烯丙基反应和在表面上形成碳键合的甲锗烷基或乙锗烷基。使用锗前体沉积的所得锗膜立即生长在该富含锗烷基的表面上,而不会形成岛。
发明内容
本文描述了包含至少一个乙烯基或烯丙基和至少一个有机氨基锚定基团的有机氨基-乙烯基硅烷和有机氨基-烯丙基硅烷家族的硅前体、包含其的组合物以及使用其沉积含硅膜和形成包含硅和乙烯基的单层膜的方法,其可有助于形成适用于沉积金属薄膜,特别地锗薄膜的种子层。此外,本文描述了包含有机氨基-乙烯基硅烷或有机氨基-烯丙基硅烷的组合物,其基本上不含至少一种选自有机胺、醇、卤化物、较高分子量物质和痕量金属的杂质物质。组合物可另外包含溶剂。本文还公开了在待加工的物体,例如半导体晶片上形成包含硅和乙烯基的膜或涂层的方法。
在本文所描述的方法的一个实施方式中,在用于形成适用于生长锗种子层和随后高质量锗膜的乙烯基封端层的条件下,在沉积室中使用有机氨基-乙烯基硅烷或有机氨基-烯丙基硅烷前体将包含硅和乙烯基的膜沉积到衬底上。
更特别地,通过一种用于形成锗种子层的方法来实现上述目的和其他目的,其包括以下步骤:
a.在反应器中提供衬底;
b.将至少一种由式I和/或II表示的前体引入到所述反应器中;
其中R1选自直链或支链C1至C10烷基、直链或支链C3至C10烯基、直链或支链C3至C10炔基、C3至C10环烷基和C6至C10芳基;R2选自氢、直链或支链C1至C10烷基、直链或支链C2至C6烯基、直链或支链C3至C6炔基、C3至C10环烷基和C6至C10芳基;R3和R4各自独立地选自氢、直链或支链C1-C10烷基、直链或支链C2-C6烯基、直链或支链C3-C6炔基、C3-C10环烷基、C6-C10芳基、C1-C10直链、环状或支链烷氧基,如上所定义的有机氨基(NR1R2)和选自Cl、Br和I的卤基;
c.用吹扫气体吹扫所述反应器;
d.在一定温度下引入至少一种包含至少一个Ge-H键的锗前体以使得所述衬底被至少一个锗单层涂覆;
e.用吹扫气体吹扫所述反应器;
f.任选地引入氢或氢等离子体源;
g.任选地用吹扫气体吹扫所述反应器;
h.在适于生长具有所需厚度的包含锗的膜的温度下,引入与步骤d中相同或不同的锗前体。
在本文所描述的方法的一个实施方式中,具有至少一个Ge-H基团的锗前体包括但不限于,三氯锗烷(ClGeH)、锗烷(GeH4)、乙锗烷(Ge2H6)、叔丁基锗烷(tBuGeH3)、苯基锗烷、仲丁基锗烷、异丁基锗烷和苄基锗烷中的一种或多种。
作为该方法中的步骤,根据一个实施方式,使用式I的有机氨基-乙烯基硅烷前体和/或式II的有机氨基-烯丙基硅烷前体和含氧源,在用于在衬底上形成氧化硅或碳掺杂氧化硅膜的条件下将包含硅和氧的膜沉积到衬底上。作为该方法中的步骤,根据另一个实施方式,使用式I的有机氨基-乙烯基硅烷前体和/或式II的有机氨基-烯丙基硅烷和含氮源,在用于形成氮化硅、碳掺杂氮化硅、氧氮化硅或氧碳氮化硅膜的条件下将包含硅和氮的膜沉积到衬底上。在进一步的实施方式中,根据式I的有机氨基-乙烯基硅烷前体和/或式II的有机氨基-烯丙基硅烷前体用作含金属膜(例如但不限于,金属氧化物膜或金属氮化物膜)的掺杂剂。
在上述方法的某些实施方式中,步骤d和h可以在相同的温度下进行,或步骤d可以在低于步骤h的温度下进行,以避免或限制步骤d中锗膜的CVD,直到形成足够的Ge种子层。在一些实施方式中,步骤d在高于步骤h的温度下进行。在其它实施方式中,在步骤d之后升高温度,以便在步骤g中的后续锗CVD膜沉积之前对至少一个锗单层(称为种子层)进行热退火或在任选的氢或氢等离子体处理期间进行退火。在又另一个实施方式中,包含至少一个Ge-H键的至少一种锗前体与锗CVD前体相同。在其它实施方式中,包含至少一个Ge-H键的至少一种锗前体不与锗CVD前体相同。
在另一个方面,提供了一种用乙烯基和/或烯丙基基团对固体衬底的表面(例如但不限于,二氧化硅、氧化铝、金属氧化物、硅晶片、介电薄膜或金属表面)官能化的方法,所述方法包含以下步骤:
a.在反应器中提供所述衬底;
b.将至少一种由下式I表示的包含连接到至少一个硅原子的至少一个乙烯基和至少一个有机氨基锚定基团的有机氨基-乙烯基硅烷前体,或至少一种由下式II表示的包含连接到至少一个硅原子的至少一个烯丙基和至少一个有机氨基锚定基团的有机氨基-烯丙基硅烷前体引入到所述反应器中;并且
c.用溶剂和/或吹扫气体从所述衬底去除残留的有机氨基-乙烯基硅烷或有机氨基-烯丙基硅烷。
在一些实施方式中,本文公开的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体可以纯净液体的方式、以溶剂中的溶液的方式或以具有或不具有载气的蒸气相的方式在0℃至500℃范围内的温度下引入到固体衬底。
附图说明
图1是描绘一般方案的流程图,其中如本文所公开的具有式I(或替代地式II)的有机氨基-乙烯基硅烷前体用于(a)用乙烯基将衬底表面官能化,使其适用于(b)通过与包含至少一个Ge-H键的锗前体的氢锗化反应形成锗种子层,从而允许(c)随后使用至少一种ALD或CVD Ge前体在该种子层的顶部上生长平滑且均匀的锗膜。
具体实施方式
本文公开了硅前体化合物和使用其用于沉积含硅膜以及将衬底表面官能化以用于随后处理(包括但不限于,锗膜沉积)的方法。
用于形成锗种子层的特定方法包括以下步骤:
a.在反应器中提供衬底;
b.将至少一种由下式I表示的包含连接到至少一个硅原子的至少一个乙烯基和至少一个有机氨基锚定基团的有机氨基-乙烯基硅烷前体,或至少一种由下式II表示的包含连接到至少一个硅原子的至少一个烯丙基和至少一个有机氨基锚定基团的有机氨基-烯丙基硅烷前体引入到所述反应器中;
其中R1选自直链或支链C1至C10烷基、直链或支链C3至C10烯基、直链或支链C3至C10炔基、C3至C10环烷基和C6至C10芳基;R2选自氢、直链或支链C1至C10烷基、直链或支链C2至C6烯基、直链或支链C3至C6炔基、C3至C10环烷基和C6至C10芳基;R3和R4各自独立地选自氢、直链或支链C1-C10烷基、直链或支链C2-C6烯基、直链或支链C3-C6炔基、C3-C10环烷基、C6-C10芳基、C1-C10直链、环状或支链烷氧基,如上所定义的有机氨基(NR1R2)和选自Cl、Br和I的卤基;
c.用吹扫气体吹扫所述反应器;
d.在一定温度下引入包含至少一个Ge-H键的至少一种锗前体以使得所述衬底被至少一个锗单层涂覆;
e.用吹扫气体吹扫所述反应器;
f.任选地引入氢或氢等离子体源;
g.任选地用吹扫气体吹扫所述反应器;并且
h.在适于生长具有所需厚度的包含锗的膜的温度下,引入与步骤d中相同或不同的锗前体。
在一些实施方式中,R1和R2是相同的。在其它实施方式中,R1和R2是不同的。在一些实施方式中,R3和R4是相同的。在其它实施方式中,R3和R4是不同的。
在一些优选的实施方式中,R3和R4独立地选自氢、甲基、乙烯基和烯丙基。
本文所描述的有机氨基-乙烯基硅烷和有机氨基-烯丙基硅烷前体用于形成含有硅加上乙烯基和/或烯丙基的单层膜以及化学计量和非化学计量的含硅膜,例如但不限于,非晶硅、结晶硅、氧化硅、碳掺杂氧化硅、氧碳化硅、氮化硅、氧氮化硅和氧碳氮化硅。这些前体也可用作,例如,含金属膜的掺杂剂。在半导体工艺中使用的有机氨基-乙烯基硅烷和有机氨基-烯丙基硅烷前体通常是高纯度的挥发性液体化学品,其被汽化并以气体递送到沉积室或反应器中,以通过用于半导体装置的CVD或ALD工艺沉积含硅膜,然而,其也可以液体相(纯净或与溶剂一起)引入到衬底。根据所需的最终含硅材料或膜来选择用于沉积的前体材料。例如,前体材料可针对其化学元素的含量、化学元素的化学计量比和/或在CVD下形成的所得的含硅膜或涂层来选择。前体材料也可针对各种其它特性,例如成本、相对低的毒性、操作特性、在室温下保持液体相的能力、挥发性、分子量、热稳定性和/或其它考虑因素来选择。在某些实施方式中,本文所描述的前体可通过多种手段,优选地使用装配有适合的阀和配件的可加压不锈钢容器递送到反应器系统,以允许将液体或蒸气相前体递送到沉积室或反应器。
用于形成锗种子层的另一个特定方法包括以下步骤:
a.在反应器中提供衬底;
b.将至少一种由下式I表示的包含连接到至少一个硅原子的至少一个乙烯基和至少一个有机氨基锚定基团的有机氨基-乙烯基硅烷前体,或至少一种由下式II表示的包含连接到至少一个硅原子的至少一个烯丙基和至少一个有机氨基锚定基团的有机氨基-烯丙基硅烷前体引入到所述反应器中;
其中R1选自直链或支链C1至C10烷基、直链或支链C3至C10烯基、直链或支链C3至C10炔基、C3至C10环烷基和C6至C10芳基;R2选自氢、直链或支链C1至C10烷基、直链或支链C2至C6烯基、直链或支链C3至C6炔基、C3至C10环烷基和C6至C10芳基;R3和R4各自独立地选自氢、直链或支链C1-C10烷基、直链或支链C2-C6烯基、直链或支链C3-C6炔基、C3-C10环烷基、C6-C10芳基、C1-C10直链、环状或支链烷氧基,如上所定义的有机氨基(NR1R2)和选自Cl、Br和I的卤基;
c.用吹扫气体吹扫所述反应器;
d.引入含氧源;
e.用吹扫气体吹扫所述反应器;
f.再引入上述有机氨基-乙烯基硅烷或有机氨基-烯丙基硅烷前体;
g.用吹扫气体吹扫所述反应器;
h.在一定温度下引入至少一种包含至少一个Ge-H键的锗前体以使得所述衬底被至少一个锗单层涂覆;
i.用吹扫气体吹扫所述反应器;
j.任选地引入氢或氢等离子体源;
k.任选地用吹扫气体吹扫所述反应器;并且
l.在适于生长具有所需厚度的包含锗的膜的温度下,引入与步骤d中相同或不同的锗前体;
其中重复步骤b至e,直到在沉积锗种子层和随后的含锗膜之前沉积所需厚度的含硅膜。
在一些实施方式中,R1和R2是相同的。在其它实施方式中,R1和R2是不同的。在一些实施方式中,R3和R4是相同的。在其它实施方式中,R3和R4是不同的。
在一些优选的实施方式中,R3和R4独立地选自氢、甲基、乙烯基和烯丙基。
使用本文所描述的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体沉积的含硅膜,无论是单一单层或多于单一单层,可用作适合于与包含至少一个Ge-H键的锗前体反应的衬底。不受理论的束缚,据信当衬底的表面与本文所描述的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体反应时,其成为被乙烯基和/或烯丙基,或更具体地,乙烯基甲硅烷基和/或烯丙基甲硅烷基官能化。这些基团随后可各自经历与锗前体分子的Ge-H键的氢锗化反应,因此,可将锗原子或锗烷基锚定在表面上存在可用的乙烯基和/或烯丙基的任何位置。该反应中的乙烯基和/或烯丙基被转化成Si和Ge原子之间的亚乙基(ethylene)、乙叉(ethylidene)、亚丙基或甲基亚乙基连接基。一旦衬底的表面被锗烷基均匀地涂覆,则在大多数情况下在升高的温度下,但在一些情况下在相同的温度下,其变成备用于通过ALD、PEALD、CVD、循环CVD或PECVD工艺沉积Ge膜。在一些实施方式中,锚定在表面上的锗烷基必须首先用还原气体(例如但不限于,氢或氢等离子体)还原,以产生-GeHx(x=0、1、2、3)封端的表面。
包含至少一个Ge-H键的示例性锗前体包括但不限于,三氯锗烷(Cl3GeH)、锗烷(GeH4)、乙锗烷(Ge2H6)、叔丁基锗烷(tBuGeH3)、苯基锗烷、仲丁基锗烷、异丁基锗烷和苄基锗烷中的一种或多种。
图1描绘了一般方案,其中如本文公开的具有式I的有机氨基-乙烯基硅烷前体用于(a)用乙烯基将衬底表面官能化,使其适用于(b)通过与包含至少一个Ge-H键的锗前体的氢锗化反应形成锗种子层,从而允许(c)随后使用至少一种ALD或CVD Ge前体在该种子层的顶部上生长平滑且均匀的锗膜。相同类型的方案应用于其中在图1的步骤(a)中使用如本文公开的具有式II的有机氨基-烯丙基硅烷前体的方法,不同之处在于衬底用烯丙基而不是用乙烯基来官能化。
据信,当衬底由于预先用本文所公开的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体均匀地处理而被-GeHx(x=0、1、2、3)基团均匀封端时,其用作种子层,这允许具有非常低的非均匀性和低水平的表面粗糙度的无定形或结晶锗膜的后续生长。所得的平滑和均匀的Ge膜被认为是通过消除本领域技术人员已知的在Ge膜沉积开始时的“岛生长”现象而实现的。通过将非反应性的有机、介电、金属或任何其它非反应性表面转化成用锗原子或锗烷基官能化的反应性表面,人们可开始沉积Ge膜而不在表面上形成“岛”。该平滑的、保形的初始层是高质量锗种子层特征的。
本文所描述的有机氨基-乙烯基硅烷和有机氨基-烯丙基硅烷前体表现出反应性和稳定性的平衡,这使其理想地适合作为微电子器件制造工艺中的CVD或ALD前体。关于反应性,本发明中的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷具有至少一个有机氨基(NR1R2),其有助于在ALD工艺期间使有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体与羟基表面反应。尽管本发明中最常提及的羟基表面是介电表面,例如,氧化硅、氮化硅、硅(具有天然氧化物)、金属氧化物、金属氮化物或金属(具有天然氧化物),但是预期可能含有表面羟基的其它材料,例如有机聚合物、硅氧烷、树脂、塑料、珠、吸附剂、无定形碳、活性炭、矿物质、有机物、容器和纺织品,也对本文所描述的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体上的至少一个有机氨基具有反应性。
预期本文所描述的有机氨基-乙烯基硅烷和有机氨基-烯丙基硅烷前体中的有机氨基锚定基团在与-OH封端的表面的反应方面,提供了优于氯-乙烯基硅烷、烷氧基-乙烯基硅烷、乙烯基二硅氮烷、氯-烯丙基硅烷、烷氧基-烯丙基硅烷和烯丙基-二硅氮烷前体的优势,尤其是在低温下和在气相中。例如,在特定温度下用三乙氧基乙烯基硅烷处理衬底可使衬底表面几乎没有或没有被乙烯基官能化,而在相同温度下用有机氨基-乙烯基硅烷处理衬底可提供高得多的官能化水平。类似地,在一定的温度下用三乙氧基烯丙基硅烷处理衬底可使衬底表面几乎没有或没有被烯丙基官能化,而在相同温度下用有机氨基-烯丙基硅烷处理衬底可提供高得多的官能化水平。这使得具有式I和式II的有机氨基-乙烯基硅烷和有机氨基-烯丙基硅烷有利地作为用于除了随后沉积锗膜之外目的的表面改性剂。可受益于表面乙烯基和/或烯丙基的高饱和的当前工艺的实例包括但不限于,(a)将例如催化剂、离子交换官能团、吸附剂或金属清除剂的物质固定到固体载体上;(b)提高衬底的疏水性;(c)改变用于显示应用的衬底的光学性质或折射率;和/或(d)在随后涂层的UV/热退火之后,提供了用于更好粘附的交联位点。
某些前体可能具有太高的沸点而无法汽化并递送到反应器以作为膜沉积在衬底上,因此优选的是选择较小的有机氨基及较小的R-基团以提供具有250℃或更低,优选地200℃或更低的沸点的前体。具有两个或更多个有机氨基可以显著提高沸点;具有较高相对沸点的前体要求递送容器和管线在指定真空下需要加热到或高于前体的沸点,以防止在容器、管线或两者中冷凝或形成颗粒。关于稳定性,其它前体在降解时可能形成甲硅烷(SiH4)或乙硅烷(Si2H6)。硅烷在室温下具有自燃性或其可以自发性地燃烧,这导致安全性和操作问题。此外,甲硅烷或乙硅烷和其它副产物的形成降低了前体的纯度水平,并且对于可靠的半导体制造,小至1-2%的化学纯度变化可能被认为是不可接受的。在某些实施方式中,本文所描述的具有式I和/或II的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体在储存6个月或更长,或1年或更长的时间段后包含2重量%或更少,或1重量%或更少,或0.5重量%或更少的杂质(例如,游离有机胺、醇、氯硅烷、卤化物或较高分子量的歧化产物),其表明是储存稳定的。某些具有Si-H基团的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体(式I和/或II中至少R3和R4之一为氢)可能易于通过分子间氢化硅烷化反应经由聚合而降解。即,如果式I和/或II中R1至R4基团的尺寸不提供足够的空间保护,则一个分子的Si-H基团与另一分子的乙烯基和/或烯丙基之间可发生反应。该氢化硅烷化反应可在储存条件下或在纯化(例如,蒸馏)期间或在沉积工艺期间缓慢地或自发地发生,并且可通过痕量杂质催化。因此,重要的是去除有机氨基-乙烯基硅烷前体中尽可能多的可用作氢化硅烷化/聚合催化剂的杂质。此外,需要仔细选择R1至R4基团以允许有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷在所需条件下与衬底表面容易地反应,同时保持前体的固有稳定性。
在某些优选的实施方式中,式I和/或II中的R3和R4均是有机氨基。在其它优选的实施方式中,式I和/或II中的R3和R4均是甲基。在其它优选的实施方式中,式I和/或II中的R1-4均是甲基。在其它优选的实施方式中,式I和/或II中的R3和R4均是乙烯基。在其它优选的实施方式中,式I和/或II中的R3和R4均是烯丙基。在其它优选的实施方式中,在式I中,R3是有机氨基,R4是乙烯基。在其它优选的实施方式中,在式II中,R3是有机氨基,R4是烯丙基。在其它优选的实施方式中,在式I中,R3是甲基,R4是乙烯基。在其它优选的实施方式中,在式II中,R3是甲基,R4是烯丙基。
在某些实施方式中,例如,对于使用ALD、ALD样、PEALD或CCVD沉积方法沉积氧化硅或氮化硅或其它含硅膜,本文所描述的有机氨基-乙烯基硅烷和有机氨基-烯丙基硅烷前体能够在相对低的沉积温度下沉积高密度材料,例如1000℃或更低、800℃或更低、700℃或更低、500℃或更低、或400℃或更低、300℃或更低、200℃或更低、100℃或更低、或50℃或更低。
在一个实施方式中,本文描述了一种用于形成含硅膜的组合物,其包含:本文所描述的具有式I的有机氨基-乙烯基硅烷和/或具有式II的有机氨基-烯丙基硅烷和溶剂。
不意图受任何特定理论的束缚,据信与现有的硅前体如TEOS、BDEAS、SiCl4相比,本文所描述的组合物可提供一种或多种优势。这些优势包括:有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷在半导体工艺中更好的利用、在长期储存中更好的稳定性、通过闪蒸的更清洁汽化和/或整体上更稳定的直接液体注射(DLI)化学气相沉积工艺,从而允许沉积更高质量的含硅膜,此外允许更优异的后续Ge膜沉积。组合物中有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷的重量百分比范围可以为1至99%,余量为溶剂,其中溶剂不与有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷反应,并且具有与有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷相似的沸点。关于后者,组合物中有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷与溶剂的沸点差异为40℃或更低,更优选地20℃或更低,或10℃或更低。
在一些实施方式中,有利的是使用本发明所描述的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体来沉积含硅膜,例如但不限于,硅、碳化硅、氮化硅、碳掺杂氮化硅、氧化硅、氮氧化硅、碳掺杂氮氧化硅和碳掺杂氧化硅,前提是金属膜如锗膜随后沉积到含硅膜上。不意图受特定理论的束缚,据信当这种含Si膜沉积工艺的最后步骤是有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体暴露时,所得的含硅膜远更易于形成均匀的Ge种子层,并且因此在其后生长平滑的、保形的Ge膜。在一些情况下,也可使用现有技术中已知的各种其它硅前体和沉积方法实现本文所描述的含Si膜的总体组成、物理性质和电学性质。然而,这些膜在沉积还原或金属锗膜之前仍然需要用本文所描述的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体进行官能化,以使这些锗膜具有相同的高质量。因此,如何使用单一硅前体如本文所描述的有机氨基-乙烯基硅烷或有机氨基-烯丙基硅烷来进行含硅膜的沉积以及该膜用乙烯基和/或烯丙基的官能化以用于随后的Ge膜生长将比使用两种不同的硅前体有利得多是清楚的。
在某些实施方式中,式I和/或式II中的取代基R1和R2可以连接到一起以形成环结构。如本领域技术人员将理解的,当R1和R2连接到一起以形成环时,R1包括用于连接到R2的键,反之亦然。在这些实施方式中,环结构可以是不饱和的,例如环状烷基环,或是饱和的,例如芳基环。以类似的方式,式I和/或式II中的R3和R4可以连接到一起以形成环结构。此外,在这些实施方式中,环结构也可以是取代或未取代的。示例性环状环基团包括但不限于,吡咯烷基、2-甲基吡咯烷基、2,5-二甲基吡咯烷基、哌啶子基、2,6-二甲基哌啶子基、吡咯基和咪唑基。然而,在其它实施方式中,取代基R1和R2未连接。又在其它实施方式中,R3和R4未连接。
在该式和整个说明书中,术语“烷基”表示具有1至10个或1至6个碳原子的直链或支链官能团。示例性烷基包括但不限于,甲基、乙基、丙基、异丙基、丁基、异丁基、仲丁基、叔丁基、戊基、异戊基、叔戊基、己基、异己基和新己基。在某些实施方式中,烷基可以具有一个或多个与其连接的官能团,例如但不限于,烷氧基、二烷基氨基或其组合。在其它实施方式中,烷基不具有一个或多个与其连接的官能团。
在该式和整个说明书中,术语“环烷基”表示具有3至10个或4至10个碳原子或5至10个碳原子的环状官能团。示例性环烷基包括但不限于,环丁基、环戊基、环己基和环辛基。
在该式和整个说明书中,术语“芳基”表示具有5至12个碳原子或6至10个碳原子的芳族环状官能团。示例性芳基包括但不限于,苯基、苄基、氯苄基、甲苯基和邻二甲苯基。
在该式和整个说明书中,术语“烯基”表示具有一个或多个碳-碳双键,并且具有3至10个或3至6个或3至4个碳原子的基团。示例性烯基包括但不限于,乙烯基和烯丙基。
在该式和整个说明书中,术语“炔基”表示具有一个或多个碳-碳三键,并且具有3至10个或3至6个或3至4个碳原子的基团。
在该式和整个说明书中,术语“有机氨基”表示具有至少一个连接到氮原子的烷基或另外地烃基,并且具有1至10个或2至6个或2至4个碳原子的基团。示例性有机氨基包括但不限于,甲基氨基、乙基氨基、正丙基氨基、异丙基氨基、正丁基氨基、异丁基氨基、仲丁基氨基、叔丁基氨基、环戊基氨基、环己基氨基、苯基氨基、二甲基氨基、N-乙基甲基氨基、二乙基氨基、二异丙基氨基。
在该式和整个说明书中,术语“二烷基氨基”表示具有两个连接到氮原子的烷基的基团,其中每个烷基具有例如1至10个、2至6个或2至4个碳原子。示例性二烷基氨基包括但不限于,二甲基氨基、二乙基氨基、乙基甲基氨基、二-正丙基氨基、二-异丙基氨基、二-正丁基氨基、二-异丁基氨基、二-仲丁基氨基、二-叔丁基氨基。
在某些实施方式中,式I和式II中烷基、烯基、炔基或芳基中的一个或多个可被取代或具有替代例如氢原子而取代的一个或多个原子或原子团。示例性取代基包括但不限于,氧、硫、卤素原子(例如,F、Cl、I或Br)、氮和磷。
在某些实施方式中,至少一种具有式I的有机氨基-乙烯基硅烷前体和/或至少一种具有式II的有机氨基-烯丙基硅烷前体具有一个或多个包含氧或氮原子的取代基。
据信,本文所描述的式I和II前体的独特结构允许在1000℃或更低、700℃或更低、500℃或更低、400℃或更低、300℃或更低、200℃或更低、100℃或更低,或25℃或更低的温度下沉积含硅膜和/或固体衬底的表面官能化。
表1列出了根据式I的具有连接到至少一个硅原子的至少一个乙烯基和至少一个有机氨基锚定基团的硅前体的实例。
表1.示例性有机氨基-乙烯基硅烷前体。
表2列出了根据式II的具有连接到至少一个硅原子的至少一个烯丙基和至少一个有机氨基锚定基团的硅前体的实例。
表2.示例性有机氨基烯丙基硅烷前体。
根据本发明的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体和包含根据本发明的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体的组合物优选地基本上不含有机胺或卤离子。如本文所使用,术语“基本上不含”当涉及卤离子(或卤化物)如氯化物和氟化物、溴化物和碘化物时,意旨小于5ppm(按重量计),优选地小于3ppm,更优选地小于1ppm,和最优选地0ppm。如本文所使用,术语“不含”当其涉及卤离子或其它杂质时,意指0ppm。已知氯化物用作用于有机氨基-乙烯基硅烷和有机氨基-烯丙基硅烷的分解催化剂。最终产物中的显著水平的氯化物可导致有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体降解。有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷的逐渐降解可直接影响膜沉积工艺或表面官能化处理,从而使得半导体制造商难以满足膜标准。此外,有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷的较高降解速率对保质期或稳定性有负面影响,从而使得其难以保证1-2年的保质期。因此,有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷的加速分解呈现出与这些易燃和/或自燃性气态副产物(有机胺,包括但不限于,C1至C10有机胺、有机二胺)的形成相关的安全性和性能问题。具有式I和式II的硅前体化合物优选地基本上不含金属离子,例如,Li+、Na+、K+、Mg2+、Ca2+、Al3+、Fe2+、Fe2+、Fe3+、Ni2+、Cr3+。如本文所使用,当涉及Li、Na、K、Mg、Ca、Al、Fe、Ni、Cr、贵金属,如来自合成中使用的钌或铂催化剂的挥发性Ru或Pt络合物时,术语“基本上不含”意指通过ICP-MS或用于测量痕量金属的其它分析方法测量的,小于5ppm(按重量计),优选地小于3ppm,并且更优选地小于1ppm,和最优选地0.1ppm。
用于形成含硅膜或涂层的方法是沉积工艺。用于本文所公开的方法的适合的沉积工艺的实例包括但不限于,循环CVD(CCVD)、MOCVD(金属有机CVD)、热化学气相沉积、等离子体增强化学气相沉积(“PECVD”)、高密度PECVD、光子辅助CVD、等离子体-光子辅助(“PPECVD”)、低温化学气相沉积、化学辅助气相沉积、热丝化学气相沉积、液体聚合物前体的CVD、由超临界流体的沉积和低能CVD(LECVD)。在某些实施方式中,含金属膜通过原子层沉积(ALD)、等离子体增强ALD(PEALD)或等离子体增强循环CVD(PECCVD)工艺沉积。如本文所使用,术语“化学气相沉积工艺”是指其中将衬底暴露于一种或多种挥发性前体(其在衬底表面上反应和/或分解以产生所需的沉积)的任何工艺。如本文所使用,术语“原子层沉积工艺”是指将材料膜沉积到不同组成的衬底上的自限性(例如,在每个反应循环中沉积的膜材料的量是恒定的)、连续表面化学。尽管本文所用的前体、试剂和来源有时可描述为“气态”,但应理解,前体可为液体或固体,其在存在或不存在惰性气体的情况下通过直接汽化、鼓泡或升华运输到反应器中。在一些情况下,汽化的前体可以通过等离子体发生器。在一个实施方式中,使用ALD工艺沉积含硅膜。在另一个实施方式中,使用CCVD工艺沉积含硅膜。在另一个实施方式中,使用热CVD工艺沉积含硅膜。本文所用的术语“反应器”包括但不限于,反应室或沉积室。
在某些实施方式中,本文所公开的方法通过使用在前体引入到反应器之前和/或期间分隔前体的ALD或CCVD方法避免了前体的预反应。对此,沉积技术如ALD或CCVD工艺用于沉积含硅膜。在一个实施方式中,膜通过将衬底表面交替地暴露于含硅前体、含氧源、含氮源或其它前体或试剂中的一种或多种经由ALD工艺来沉积。膜的生长通过表面反应的自限性控制、每种前体或试剂的脉冲长度和沉积温度来进行。然而,一旦衬底表面饱和,膜生长停止。
在某些实施方式中,本文所描述的方法还包括除了具有上述式I和/或II的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体以外的一种或多种另外的含硅前体。另外的含硅前体的实例包括但不限于,单氨基硅烷(例如,二异丙基氨基硅烷、二仲丁基氨基硅烷、苯基甲基氨基硅烷;有机硅化合物,例如,三甲硅烷基胺(TSA);单氨基硅烷(二异丙基氨基硅烷、二仲丁基氨基硅烷、苯基甲基氨基硅烷);硅氧烷(例如,六甲基二硅氧烷(HMDSO)和二甲基硅氧烷(DMSO),及六氯二硅氧烷(HCDSO));有机硅烷(例如,甲基硅烷、二甲基硅烷、二乙基硅烷、乙烯基三甲基硅烷、三甲基硅烷、四甲基硅烷、乙基硅烷、二甲硅烷基甲烷、2,4-二硅杂戊烷、1,4-二硅杂丁烷、2,5-二硅杂己烷、2,2-二甲硅烷基丙烷、1,3,5-三硅杂环己烷及这些化合物的氟化衍生物);含苯基的有机硅化合物(例如,二甲基苯基硅烷和二苯基甲基硅烷);含氧的有机硅化合物,例如,二甲基二甲氧基硅烷;1,3,5,7-四甲基环四硅氧烷;1,1,3,3-四甲基二硅氧烷;1,3,5,7-四硅杂-4-氧代-庚烷;2,4,6,8-四硅杂-3,7-二氧代-壬烷;2,2-二甲基-2,4,6,8-四硅杂-3,7-二氧代-壬烷;八甲基环四硅氧烷;[1,3,5,7,9]-五甲基环戊硅氧烷;1,3,5,7-四硅杂-2,6-二氧代-环辛烷;六甲基环三硅氧烷;1,3-二甲基二硅氧烷;1,3,5,7,9-五甲基环戊硅氧烷;六甲氧基二硅氧烷及这些化合物的氟化衍生物。
在某些实施方式中,根据沉积方法,一种或多种含硅前体可以预定的摩尔量或约0.1至约1000微摩尔引入到反应器中。在该实施方式或其它实施方式中,含硅和/或有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体引入到反应器中预定的时间段。在某些实施方式中,该时间段在约0.001至约500秒的范围内。
在某些实施方式中,使用本文所描述的方法沉积的含硅膜在氧的存在下使用含氧源、试剂或包含氧的前体形成。含氧源可以至少一种含氧源的形式引入到反应器中和/或可附带地存在于沉积工艺中使用的其它前体中。合适的含氧源气体可包括,例如,水(H2O)(例如,去离子水、纯化水和/或蒸馏水)、过氧化氢(H2O2)、氧气(O2)、氧等离子体、臭氧(O3)、NO、N2O、NO2、一氧化碳(CO)、二氧化碳(CO2)及其组合。在某些实施方式中,含氧源包含在约1到约2000标准立方厘米(sccm)或约1到约1000sccm的范围内的流速下引入到反应器中的含氧源气体。含氧源可引入约0.1至约100秒的范围内的时间。在一个特定的实施方式中,含氧源包含具有温度10℃或更高的水。在其中膜通过ALD或循环CVD工艺沉积的实施方式中,前体脉冲可具有大于0.01秒的脉冲持续时间,并且含氧源可具有小于0.01秒的脉冲持续时间,而水脉冲持续时间可具有小于0.01秒的脉冲持续时间。在又另一个实施方式中,脉冲之间的吹扫持续时间可以低至0秒或连续地脉冲而在期间没有吹扫。含氧源或试剂以相对于硅前体小于1:1比率的分子的量提供,使得至少一些碳保留在原样沉积的含硅膜中。
在某些实施方式中,含硅膜包含硅和氮。在这些实施方式中,使用本文所描述的方法沉积的含硅膜在含氮源的存在下形成。含氮源可以至少一种含氮源的形式引入到反应器中和/或可附带地存在于沉积工艺中使用的其它前体中。合适的含氮源气体可包括,例如,氨、肼、单烷基肼、二烷基肼、氮、氮/氢、氨等离子体、氮等离子体、氮/氢等离子体及其混合物。在某些实施方式中,含氮源包含氨等离子体或氢/氮等离子体源气体,其在约1到约2000标准立方厘米(sccm)或约1到约1000sccm的范围内的流速下引入到反应器中。含氮源可引入约0.1至约100秒的范围内的时间。在其中膜通过ALD或循环CVD工艺沉积的实施方式中,前体脉冲可具有大于0.01秒的脉冲持续时间,并且含氮源可具有小于0.01秒的脉冲持续时间,而水脉冲持续时间可具有小于0.01秒的脉冲持续时间。在又另一个实施方式中,脉冲之间的吹扫持续时间可以低至0秒或连续地脉冲而在期间没有吹扫。
本文所公开的沉积方法可涉及一种或多种吹扫气体。用于吹扫去除未消耗的反应物和/或反应副产物的吹扫气体是不与前体反应的惰性气体。示例性吹扫气体包括但不限于,氩(Ar)、氮(N2)、氦(He)、氖、氢(H2)及其混合物。在某些实施方式中,吹扫气体例如Ar在约10至约2000sccm的范围内的流速下供给到反应器中持续约0.1至1000秒,从而吹扫未反应的材料和可能留在反应器中的任何副产物。
供给前体、含氧源、含氮源,和/或其它前体、源气体和/或试剂的相应步骤可通过改变其供给时间来进行,以改变所得的含硅膜的化学计量组成。
将能量施加到前体、含氧源、含氮源、还原剂、其它前体或其组合中的至少一种以引发反应,并在衬底上形成含硅膜或涂层。此类能量可通过但不限于,热、等离子体、脉冲等离子体、螺旋波等离子体、高密度等离子体、电感耦合等离子体、X射线、电子束、光子、远程等离子体方法及其组合来提供。在某些实施方式中,次级RF频率源可用于改变衬底表面处的等离子体特性。在其中沉积涉及等离子体的实施方式中,等离子体发生过程可包括其中在反应器中直接生成等离子体的直接等离子体发生过程,或替代地,其中在反应器外部生成等离子体并将其供给到反应器中的远程等离子体发生过程。
有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体、其它含硅前体和/或锗前体可以各种方式递送到反应室,例如CVD或ALD反应器。在一个实施方式中,可利用液体递送系统。在替代的实施方式中,可采用组合液体递送和闪蒸气化工艺单元,诸如,例如由明尼苏达州肖维尔的MSP公司制造的涡轮汽化器,以使低挥发性材料能够定量地递送,其导致可再现的运输和沉积而不会使前体热分解。在液体递送方式中,本文所描述的前体可以纯净液体形式递送,或替代地,可以在包含其的溶剂制剂或组合物中递送。因此,在某些实施方式中,前体制剂可包括具有可能期望和在给定最终用途应用中有利的合适特性的溶剂组分以将膜在衬底上形成。
对于其中包含溶剂和本文所描述的具有式I和/或II的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体的组合物中使用具有式I和/或式II的前体的那些实施方式,所选择的溶剂或其混合物不与有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷反应。在组合物中按重量百分比计的溶剂量在0.5重量%至99.5重量%或10重量%至75重量%的范围内。在该实施方式或其他实施方式中,溶剂具有类似于具有式I和/或II的前体的沸点(b.p.)的b.p.或者溶剂的b.p.与具有式I或II的前体的b.p.之间的差异为40℃或更低、30℃或更低,或20℃或更低,或10℃。可选地,沸点的差异在任何一个或多个以下端点的范围内:0℃、10℃、20℃、30℃或40℃。b.p.差异的适合范围的实例包括但不限于,0至40℃、20至30℃或10至30℃。组合物中合适溶剂的实例包括但不限于,醚(例如,1,4-二噁烷、二丁基醚)、叔胺(例如,吡啶、1-甲基哌啶、1-乙基哌啶、N,N’-二甲基哌嗪、N,N,N’,N’-四甲基乙二胺)、腈(例如,苄腈)、烷基烃(例如,辛烷、壬烷、十二烷、乙基环己烷)、芳香烃(例如,甲苯、均三甲苯)、叔氨基醚(例如,双(2-二甲基氨基乙基)醚)或其混合物。
在另一个实施方式中,本文描述了包含一种或多种具有式I或II的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体的用于沉积含硅膜的容器。在一个特定的实施方式中,容器包含至少一个装配适合的阀和配件的可加压容器(优选地不锈钢的),以允许将一种或多种前体递送到用于CVD或ALD工艺的反应器。在该实施方式或其它实施方式中,在由不锈钢构成的可加压容器中提供具有式I和/或II的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体,并且前体的纯度为98重量%或更大或者99.5%或更大,其适用于大多数半导体应用。在某些实施方式中,此类容器还可具有用于将前体与一种或多种另外的前体混合(如果需要)的装置。在这些或其它实施方式中,容器的内容物可以与另外的前体预混合。可选地,可将有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体和/或其它前体维持在单独的容器中或在具有分离装置的单一容器中,其用于在储存过程中保持有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体和其它前体分离。
在本文所描述的方法的一个实施方式中,可采用循环沉积工艺如CCVD、ALD或PEALD,其中使用至少一种选自具有本文所描述的式的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体的含硅前体和任选地含氮源,例如氨、肼、单烷基肼、二烷基肼、氮、氮/氢、氨等离子体、氮等离子体、氮/氢等离子体。
在某些实施方式中,根据工艺要求,将从前体罐连接到反应室的气体管线加热到一个或多个温度,并且将具有本文所描述的式I和/或II的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体的容器保持在一个或多个温度下用于鼓泡。在其它实施方式中,将包含至少一种具有本文所描述的式的含硅前体的溶液注入保持在一个或多个温度下的汽化器中用于直接液体注射。
氩气和/或其它气体流可用作载气以在前体脉冲期间帮助将至少一种有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体的蒸气递送到反应室。在某些实施方式中,反应室工艺压力为约10托或更小。在另外的实施方式中,反应室工艺压力为约5托或更小。
对于多组分含硅膜,可将其他前体如含硅前体、含氮前体、还原剂或其它试剂交替地引入到反应室中。
在本文所描述的方法的一个实施方式中,使用热ALD工艺和包含氢的等离子体沉积氧化硅或碳含量在0原子%至20原子%的范围内的碳掺杂的氧化硅膜以改善膜性能。在该实施方式中,该方法包括:
a.将一个或多个包含表面特征的衬底放置于反应器中,并将反应器加热到环境温度至约550℃范围内的一个或多个温度,和任选地将所述反应器维持在100托或更低的压力下;
b.将至少一种由式I和/或II表示的包含连接于至少一个硅原子的至少一个乙烯基和/或烯丙基和至少一个有机氨基锚定基团的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体引入到反应器中;
c.用惰性气体吹扫所述反应器,从而去除未反应的硅前体,并形成包含吹扫气体和硅前体的组合物;
d.向所述反应器中提供含氧源以与表面反应,从而形成含硅和氧的膜;
g.用惰性气体吹扫以去除反应副产物;
f.重复步骤b至e以提供所需厚度的氧化硅或碳掺杂氧化硅;
在该实施方式或其它实施方式中,UV暴露步骤可以在膜沉积期间或一旦沉积完成就进行。在另一个实施方式中,可使用如本文所描述的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷,以与上述相同的步骤(除了使用含氮源替代含氧源)沉积含硅和氮的膜,例如,氮化硅或碳氮化硅。
在一个实施方式中,衬底包括至少一个特征,其中该特征包括具有1:9或更高的深宽比和/或180nm或更小的开口的图案沟槽。
在其中用等离子体处理膜的实施方式中,等离子体源选自氢等离子体、包含氢和氦的等离子体和包含氢和氩的等离子体。氢等离子体使膜的介电常数降低,并提高了对随后的等离子体灰化工艺的损伤抗性,同时仍然保持总体的碳含量几乎不变。
在整个说明书中,术语“ALD或ALD样”是指包括但不限于以下过程的工艺:a)将包括硅前体和反应性气体的每种反应物依次引入到反应器中,例如单晶片ALD反应器、半批式ALD反应器或批式炉ALD反应器;b)通过将衬底移动或旋转到反应器的不同区段而将包括硅前体和反应性气体的每种反应物暴露于衬底,并且每个区段通过惰性气体帘幕分隔(即,空间ALD反应器或卷对卷ALD反应器)。
在整个说明书中,术语“灰化”是指在半导体制造工艺中使用包含氧源的等离子体(例如,O2/惰性气体等离子体、O2等离子体、CO2等离子体、CO等离子体、H2/O2等离子体或其组合)去除光致抗蚀剂或碳硬掩模的工艺。
在整个说明书中,术语“损伤抗性”是指在氧灰化处理之后的膜性能。良好的或高的损伤抗性定义为在氧灰化后的以下膜性能:膜介电常数低于4.5;总体中碳含量(在膜超过深度处)为灰化前的5原子%之内;通过膜表面附近(小于深度)和膜主体(大于深度)之间的稀HF蚀刻速率差异观察的,小于的膜受到损伤。
在某些实施方式中,本文所描述的具有式I和/或II的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体也可用作含金属膜,例如但不限于,金属氧化物膜或金属氮化物膜,的掺杂剂。在这些实施方式中,使用ALD或CVD工艺,例如本文所描述的使用金属醇盐、金属酰胺或挥发性有机金属前体的那些工艺来沉积含金属膜。可与本文所公开的方法一起使用的适合金属醇盐前体的实例包括但不限于,第3至6族金属醇盐、具有烷氧基和烷基取代的环戊二烯基配体的第3至6族金属络合物、具有烷氧基和烷基取代的吡咯基配体的第3至6族金属络合物、具有烷氧基和二酮配体的第3至6族金属络合物;具有烷氧基和酮酯配体的第3-6族金属配合物。可与本文所公开的方法一起使用的适合的金属酰胺前体的实例包括但不限于,四(二甲基氨基)锆(TDMAZ)、四(二乙基氨基)锆(TDEAZ)、四(乙基甲基氨基)锆(TEMAZ)、四(二甲基氨基)铪(TDMAH)、四(二乙基氨基)铪(TDEAH)和四(乙基甲基氨基)铪(TEMAH)、四(二甲基氨基)钛(TDMAT)、四(二乙基氨基)钛(TDEAT)、四(乙基甲基氨基)钛(TEMAT)、叔丁基亚氨基三(二乙基氨基)钽(TBTDET)、叔丁基亚氨基三(二甲基氨基)钽(TBTDMT)、叔丁基亚氨基三(乙基甲基氨基)钽(TBTEMT)、乙基亚氨基三(二乙基氨基)钽(EITDET)、乙基亚氨基三(二甲基氨基)钽(EITDMT)、乙基亚氨基三(乙基甲基氨基)钽(EITEMT)、叔戊基亚氨基三(二甲基氨基)钽(TAIMAT)、叔戊基亚氨基三(二乙基氨基)钽、五(二甲基氨基)钽、叔戊基亚氨基三(乙基甲基氨基)钽、双(叔丁基亚氨基)双(二甲基氨基)钨(BTBMW)、双(叔丁基亚氨基)双(二乙基氨基)钨、双(叔丁基亚氨基)双(乙基甲基氨基)钨及其组合。可与本文所公开的方法一起使用的适合的有机金属前体的实例包括但不限于,环戊二烯基或烷基环戊二烯基3族金属。本文中的示例性第3至6族金属包括但不限于,Y、La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Er、Yb、Lu、Ti、Hf、Zr、V、Nb、Ta、Cr、Mo和W。
在某些实施方式中,所得的含硅膜或涂层可暴露于沉积后处理,例如但不限于,等离子体处理、化学处理、紫外线暴露、电子束暴露和/或其它处理,以实现膜的一种或多种性能。
在某些实施方式中,本文所描述的含硅膜具有6或更低的介电常数。在这些或其它实施方式中,膜可具有约5或更低、或约4或更低、或约3.5或更低的介电常数。然而,可以预见,可以根据膜的所需最终用途形成具有其它介电常数(例如,更高或更低)的膜。使用本文所描述的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体和方法所形成的含硅或含硅膜的实例具有配方SixOyCzNvHw,其中如通过例如XPS或其它手段测定的,按原子重量百分%计,Si在约10%至约40%的范围内;O在约0%至约65%的范围内;C在约0%至约75%或约0%至约50%的范围内;N在约0%至约75%或约0%至50%的范围内;并且H在约0%至约50%的范围内,其中x+y+z+v+w=100原子重量百分比。使用本文所描述的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体和方法形成的含硅膜的另一个实例是碳氮化硅,其中通过XPS测量的碳含量为1原子%至80原子%。使用本文所描述的有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体和方法形成的含硅膜的又另一个实例是无定形硅,其中通过XPS测量的氮和碳含量的总和<10原子%,优选地<5原子%,最优选地<1原子%。
如前所述,本文所描述的方法可用于在衬底的至少一部分上沉积含硅膜。适合的衬底的实例包括但不限于,硅、锗掺杂硅、锗、SiO2、Si3N4、OSG、FSG、碳化硅、氢化碳化硅、氮化硅、氢化氮化硅、碳氮化硅、氢化碳氮化硅、氮化硼、抗反射涂层、光致抗蚀剂、柔性衬底、有机聚合物、多孔有机和无机材料、金属如铜和铝,和扩散阻挡层,例如但不限于,TiN、Ti(C)N、TaN、Ta(C)N、Ta、W或WN。膜与各种后续工艺步骤,例如,化学机械平坦化(CMP)和各向异性蚀刻工艺相容。
沉积的膜具有多种应用,其包括但不限于,计算机芯片、光学器件、磁性信息存储、在支撑材料或基质上的涂层、微机电系统(MEMS)、纳米机电系统、薄膜晶体管(TFT)、发光二极管(LED)、有机发光二极管(OLED)、IGZO和液晶显示器(LCD)。
本文所描述的方法提供包括锗、硅、碳化硅、氮化硅、碳掺杂氮化硅、氧化硅、氧氮化硅、碳掺杂氧氮化硅、碳掺杂氧化硅的高质量膜。术语“高质量”意旨表现出一种或多种以下特征的膜:约2.1g/cc或更高、2.2g/cc或更高、2.25g/cc或更高的密度;如在HF比水1:100的稀HF(0.5重量%dHF)酸溶液中测量的或更低、或更低、或更低、或更低、或更低、或更低、或更低、或更低的湿蚀刻速率,在至高6MV/cm下约1e-8A/cm2或更低的漏电流;如通过SIMS测量的约5e20 at/cc或更低的氢杂质;非常低的不均匀性、低水平的表面粗糙度及其组合。关于蚀刻速率,热生长的氧化硅膜在0.5重量%HF中具有的蚀刻速率。
在某些实施方式中,本文所描述的具有式I和式II的一种或多种硅前体可用于形成作为固体且非多孔或基本上无孔的含硅和氧的膜。
以下实施例说明了本文所描述的用于制备有机氨基-乙烯基硅烷和/或有机氨基-烯丙基硅烷前体、沉积含硅膜、形成乙烯基官能化和/或烯丙基官能化的表面和产生锗种子层的方法,并且不旨在以任何方式对其限制。
实施例
实施例1.三(乙基氨基)乙烯基硅烷的合成。
在氮气保护下,在配备有机械搅拌器和回流冷凝器的3升3颈圆底烧瓶中,将乙胺在THF中的溶液(800mL,2.0M,1.60mol)通过套管添加至三乙胺(175g,1.73mol)在己烷(1升)中的溶液。将合并的溶液冷却至-20℃并搅拌。在-20℃下,在2小时内向该混合物中滴加三氯乙烯基硅烷(80.0g,0.495mol)在己烷(80g)中的溶液。将所得的白色浆液温热至室温,并再搅拌2小时。通过在玻璃料(glass frit)上过滤去除白色固体,并在室温下减压(20托)去除溶剂。通过真空蒸馏(1托/45℃)纯化所得浓缩的粗液体,得到55.4g三(乙基氨基)乙烯基硅烷。通过DSC测定沸点为199℃。GC-MS分析显示以下质量峰:m/z=187(M+),172(M-15),160,143,129,118,100,86,72,57,44。
实施例2.用三(乙基氨基)乙烯基硅烷处理硅胶。
在氮气保护下,将0.5g硅胶(DavasilTM级别645,60-100目, )在5mL三(乙基氨基)乙烯基硅烷在THF中的50重量%溶液在80℃下搅拌2小时。倾析液相,并且在真空干燥之前用热THF冲洗固体数次。未处理和经处理的硅胶通过FTIR光谱以KBr压片的方式分析。在经处理的硅胶的FTIR光谱中未检测到未处理硅胶的FTIR光谱中与分离的表面Si-OH基团对应的3741cm-1处的尖峰。处理的硅胶在FTIR光谱中显示出以下新峰:3418(N-H),3062(乙烯基C-H),3021(乙烯基C-H),2968(乙烯基C-H),2935(乙基C-H),2876(乙基C-H)。这显示硅胶的表面在用三(乙基氨基)乙烯基硅烷处理后,在相对低的温度和少量的时间内被乙烯基和乙基氨基官能化。
实施例3.三乙氧基乙烯基硅烷与叔丁基锗烷的反应。
将约1mL的三乙氧基乙烯基硅烷和叔丁基锗烷的1:1摩尔混合物密封在配备有内部压力传感器和热电偶的9.5mL不锈钢池中。将样品加热至250℃并等温保持1小时。未检测到显著的压力升高,但在约212℃处的温度升高时观察到温和的放热性热事件。当混合物冷却回室温时,通过GC和GC-MS对其进行分析。1,1-加成和1,2-加成氢锗化产物1-三乙氧基甲硅烷基-1-(叔丁基锗烷基)乙烷(次要)和1-三乙氧基甲硅烷基-2-(叔丁基锗烷基)乙烷(主要)分别根据以下质量峰进行检测:(次要)m/z=324(M+),308,280,266,238,222,210,194,179,163,147,135,119,101,89,79,57,41;(主要)m/z=324(M+),308,280,268,238,222,211,193,181,163,149,135,119,103,91,79,57,41。这证明在没有催化剂的情况下,前体中的Ge-H键,例如锗烷、乙锗烷和叔丁基锗烷,可在200-250℃之间与Si-乙烯基反应。这支持了通过首先用乙烯基将表面官能化,然后与锗烷或乙锗烷反应以在锗CVD生长之前形成Ge-H封端的表面而在SiO2衬底上形成Ge-种子层的方案。
尽管已参照某些优选的实施方式对本公开进行了描述,但本领域技术人员将理解,在不脱离本发明的范围的情况下,可以进行各种改变并且可以用等同物替换其元素。此外,在不脱离本发明的基本范围的情况下,可进行许多修改以使特定情况或材料适应本发明的教导。因此,意图的是本发明不限于特定实施方式,而是本发明将包括落入所附权利要求书的范围内的所有实施方式。
Claims (12)
1.一种通过沉积工艺在衬底的至少一个表面上形成含锗膜的方法,所述方法包括:
在反应室中提供所述衬底的该至少一个表面,所述衬底具有暴露的表面羟基;
向所述反应室中引入至少一种由下式I表示的包含连接到至少一个硅原子的至少一个乙烯基和至少一个有机氨基锚定基团的有机氨基-乙烯基硅烷前体,或至少一种由下式II表示的包含连接到至少一个硅原子的至少一个烯丙基和至少一个有机氨基锚定基团的有机氨基-烯丙基硅烷前体:
其中R1选自直链或支链C1至C10烷基、直链或支链C3至C10烯基、直链或支链C3至C10炔基、C3至C10环烷基和C6至C10芳基;R2选自氢、直链或支链C1至C10烷基、直链或支链C2至C6烯基、直链或支链C3至C6炔基、C3至C10环烷基和C6至C10芳基;R3和R4各自独立地选自氢、直链或支链C1-C10烷基、直链或支链C2-C6烯基、直链或支链C3-C6炔基、C3-C10环烷基、C6-C10芳基、C1-C10直链、环状或支链烷氧基,如上所定义的有机氨基(NR1R2)和选自Cl、Br和I的卤基;
用吹扫气体吹扫所述反应室;
将至少一种包含至少一个Ge-H键的第一含锗前体引入到所述反应室中;
用吹扫气体吹扫所述反应室;
将与所述第一含锗前体相同或不同的至少一种第二含锗前体引入到所述反应室中。
2.根据权利要求1所述的方法,其中所述至少一种有机氨基-乙烯基硅烷前体包含至少一种选自以下的化合物:三(甲基氨基)乙烯基硅烷、三(乙基氨基)乙烯基硅烷、三(正丙基氨基)乙烯基硅烷、三(异丙基氨基)乙烯基硅烷、三(仲丁基氨基)乙烯基硅烷、三(叔丁基氨基)乙烯基硅烷、三(二甲基氨基)乙烯基硅烷、三(N-乙基甲基氨基)乙烯基硅烷、三(二乙基氨基)乙烯基硅烷、三(N-甲基环己基氨基)乙烯基硅烷、三(N-甲基苯基氨基)乙烯基硅烷、三(吡咯烷基)乙烯基硅烷、三(哌啶子基)乙烯基硅烷、三(吡咯基)乙烯基硅烷、双(甲基氨基)甲基乙烯基硅烷、双(乙基氨基)甲基乙烯基硅烷、双(正丙基氨基)甲基乙烯基硅烷、双(异丙基氨基)甲基乙烯基硅烷、双(仲丁基氨基)甲基乙烯基硅烷、双(叔丁基氨基)甲基乙烯基硅烷、双(二甲基氨基)甲基乙烯基硅烷、双(N-乙基甲基氨基)甲基乙烯基硅烷、双(二乙基氨基)甲基乙烯基硅烷、双(N-甲基环己基氨基)甲基乙烯基硅烷、双(N-甲基苯基氨基)甲基乙烯基硅烷、二(吡咯烷基)甲基乙烯基硅烷、二(哌啶子基)甲基乙烯基硅烷、二(吡咯基)甲基乙烯基硅烷、双(甲基氨基)二乙烯基硅烷、双(乙基氨基)二乙烯基硅烷、双(正丙基氨基)二乙烯基硅烷、双(异丙基氨基)二乙烯基硅烷、双(仲丁基氨基)二乙烯基硅烷、双(叔丁基氨基)二乙烯基硅烷、双(二甲基氨基)二乙烯基硅烷、双(N-乙基甲基氨基)二乙烯基硅烷、双(二乙基氨基)二乙烯基硅烷、双(N-甲基环己基氨基)二乙烯基硅烷、双(N-甲基苯基氨基)二乙烯基硅烷、二(吡咯烷基)二乙烯基硅烷、二(哌啶子基)二乙烯基硅烷、二(吡咯基)二乙烯基硅烷、(甲基氨基)二甲基乙烯基硅烷、(乙基氨基)二甲基乙烯基硅烷、(正丙基氨基)二甲基乙烯基硅烷、(异丙基氨基)二甲基乙烯基硅烷、(仲丁基氨基)二甲基乙烯基硅烷、(叔丁基氨基)二甲基乙烯基硅烷、(二甲基氨基)二甲基乙烯基硅烷、(N-乙基甲基氨基)二甲基乙烯基硅烷、(二乙基氨基)二甲基乙烯基硅烷、(N-甲基环己基氨基)二甲基乙烯基硅烷、(N-甲基苯基氨基)二甲基乙烯基硅烷、(吡咯烷基)二甲基乙烯基硅烷、(哌啶子基)二甲基乙烯基硅烷、(吡咯基)二甲基乙烯基硅烷、(甲基氨基)甲基二乙烯基硅烷、(乙基氨基)甲基二乙烯基硅烷、(正丙基氨基)甲基二乙烯基硅烷、(异丙基氨基)甲基二乙烯基硅烷、(仲丁基氨基)甲基二乙烯基硅烷、(叔丁基氨基)甲基二乙烯基硅烷、(二甲基氨基)甲基二乙烯基硅烷、(N-乙基甲基氨基)甲基二乙烯基硅烷、(二乙基氨基)甲基二乙烯基硅烷、(N-甲基环己基氨基)甲基二乙烯基硅烷、(N-甲基苯基氨基)甲基二乙烯基硅烷、(吡咯烷基)甲基二乙烯基硅烷、(哌啶子基)甲基二乙烯基硅烷、(吡咯基)甲基二乙烯基硅烷、(甲基氨基)三乙烯基硅烷、(乙基氨基)三乙烯基硅烷、(正丙基氨基)三乙烯基硅烷、(异丙基氨基)三乙烯基硅烷、(仲丁基氨基)三乙烯基硅烷、(叔丁基氨基)三乙烯基硅烷、(二甲基氨基)三乙烯基硅烷、(N-乙基甲基氨基)三乙烯基硅烷、(二乙基氨基)三乙烯基硅烷、(N-甲基环己基氨基)三乙烯基硅烷、(N-甲基苯基氨基)甲基二乙烯基硅烷、(吡咯烷基)甲基三乙烯基硅烷、(哌啶子基)三乙烯基硅烷和(吡咯基)三乙烯基硅烷。
3.根据权利要求1所述的方法,其中所述至少一种有机氨基-烯丙基硅烷前体包含至少一种选自以下的化合物:三(甲基氨基)烯丙基硅烷、三(乙基氨基)烯丙基硅烷、三(正丙基氨基)烯丙基硅烷、三(异丙基氨基)烯丙基硅烷、三(仲丁基氨基)烯丙基硅烷、三(叔丁基氨基)烯丙基硅烷、三(二甲基氨基)烯丙基硅烷、三(N-乙基甲基氨基)烯丙基硅烷、三(二乙基氨基)烯丙基硅烷、三(N-甲基环己基氨基)烯丙基硅烷、三(N-甲基苯基氨基)烯丙基硅烷、三(吡咯烷基)烯丙基硅烷、三(哌啶子基)烯丙基硅烷、三(吡咯基)烯丙基硅烷、双(甲基氨基)甲基烯丙基硅烷、双(乙基氨基)甲基烯丙基硅烷、双(正丙基氨基)甲基烯丙基硅烷、双(异丙基氨基)甲基烯丙基硅烷、双(仲丁基氨基)甲基烯丙基硅烷、双(叔丁基氨基)甲基烯丙基硅烷、双(二甲基氨基)甲基烯丙基硅烷、双(N-乙基甲基氨基)甲基烯丙基硅烷、双(二乙基氨基)甲基烯丙基硅烷、双(N-甲基环己基氨基)甲基烯丙基硅烷、双(N-甲基苯基氨基)甲基烯丙基硅烷、二(吡咯烷基)甲基烯丙基硅烷、二(哌啶子基)甲基烯丙基硅烷、二(吡咯基)甲基烯丙基硅烷、双(甲基氨基)二烯丙基硅烷、双(乙基氨基)二烯丙基硅烷、双(正丙基氨基)二烯丙基硅烷、双(异丙基氨基)二烯丙基硅烷、双(仲丁基氨基)二烯丙基硅烷、双(叔丁基氨基)二烯丙基硅烷、双(二甲基氨基)二烯丙基硅烷、双(N-乙基甲基氨基)二烯丙基硅烷、双(二乙基氨基)二烯丙基硅烷、双(N-甲基环己基氨基)二烯丙基硅烷、双(N-甲基苯基氨基)二烯丙基硅烷、二(吡咯烷基)二烯丙基硅烷、二(哌啶子基)二烯丙基硅烷、二(吡咯基)二烯丙基硅烷、(甲基氨基)二甲基烯丙基硅烷、(乙基氨基)二甲基烯丙基硅烷、(正丙基氨基)二甲基烯丙基硅烷、(异丙基氨基)二甲基烯丙基硅烷、(仲丁基氨基)二甲基烯丙基硅烷、(叔丁基氨基)二甲基烯丙基硅烷、(二甲基氨基)二甲基烯丙基硅烷、(N-乙基甲基氨基)二甲基烯丙基硅烷、(二乙基氨基)二甲基烯丙基硅烷、(N-甲基环己基氨基)二甲基烯丙基硅烷、(N-甲基苯基氨基)二甲基烯丙基硅烷、(吡咯烷基)二甲基烯丙基硅烷、(哌啶子基)二甲基烯丙基硅烷、(吡咯基)二甲基烯丙基硅烷、(甲基氨基)甲基二烯丙基硅烷、(乙基氨基)甲基二烯丙基硅烷、(正丙基氨基)甲基二烯丙基硅烷、(异丙基氨基)甲基二烯丙基硅烷、(仲丁基氨基)甲基二烯丙基硅烷、(叔丁基氨基)甲基二烯丙基硅烷、(二甲基氨基)甲基二烯丙基硅烷、(N-乙基甲基氨基)甲基二烯丙基硅烷、(二乙基氨基)甲基二烯丙基硅烷、(N-甲基环己基氨基)甲基二烯丙基硅烷、(N-甲基苯基氨基)甲基二烯丙基硅烷、(吡咯烷基)甲基二烯丙基硅烷、(哌啶子基)甲基二烯丙基硅烷、(吡咯基)甲基二烯丙基硅烷、(甲基氨基)三烯丙基硅烷、(乙基氨基)三烯丙基硅烷、(正丙基氨基)三烯丙基硅烷、(异丙基氨基)三烯丙基硅烷、(仲丁基氨基)三烯丙基硅烷、(叔丁基氨基)三烯丙基硅烷、(二甲基氨基)三烯丙基硅烷、(N-乙基甲基氨基)三烯丙基硅烷、(二乙基氨基)三烯丙基硅烷、(N-甲基环己基氨基)三烯丙基硅烷、(N-甲基苯基氨基)甲基二烯丙基硅烷、(吡咯烷基)甲基三烯丙基硅烷、(哌啶子基)三烯丙基硅烷和(吡咯基)三烯丙基硅烷。
4.根据权利要求1所述的方法,其中所述有机氨基-乙烯基硅烷或所述有机氨基-烯丙基硅烷基本上不含至少一种选自以下的杂质:有机胺、卤离子和金属离子。
5.根据权利要求1所述的方法,其中所述至少一种含锗前体选自:三氯锗烷(Cl3GeH)、锗烷(GeH4)、乙锗烷(Ge2H6)、叔丁基锗烷(tBuGeH3)、苯基锗烷、仲丁基锗烷、异丁基锗烷和苄基锗烷。
6.根据权利要求1所述的方法,其进一步包括在引入所述至少一种第一含锗前体之后将还原气体引入到所述反应室中。
7.根据权利要求1所述的方法,其中所述衬底的该至少一个表面是含硅膜,并且其中在反应室中提供所述衬底的该至少一个表面的步骤包括执行以下步骤直到实现所需厚度的所述含硅膜:
将式I和/或式II的所述至少一种有机氨基-乙烯基硅烷或有机氨基-烯丙基硅烷引入到所述反应器中,
用吹扫气体吹扫所述反应器,
将含氧源和/或含氮源引入到所述反应器中,并且
用吹扫气体吹扫所述反应器。
8.根据权利要求7所述的方法,其中所述含氮源选自:氨、肼、单烷基肼、二烷基肼、氮、氮/氢、氨等离子体、氮等离子体、氮/氢等离子体及其混合物。
9.根据权利要求7所述的方法,其中所述含氧源选自:水、过氧化氢、氧气、氧等离子体、臭氧(O3)、一氧化氮、一氧化二氮、二氧化氮、一氧化碳、二氧化碳及其混合物。
10.一种组合物,其包含至少一种由下式I表示的包含连接到至少一个硅原子的至少一个乙烯基和至少一个有机氨基锚定基团的有机氨基-乙烯基硅烷前体,或至少一种由下式II表示的包含连接到至少一个硅原子的至少一个烯丙基和至少一个有机氨基锚定基团的有机氨基-烯丙基硅烷前体:
其中R1选自直链或支链C1至C10烷基、直链或支链C3至C10烯基、直链或支链C3至C10炔基、C3至C10环烷基和C6至C10芳基;R2选自氢、直链或支链C1至C10烷基、直链或支链C2至C6烯基、直链或支链C3至C6炔基、C3至C10环烷基和C6至C10芳基;R3和R4各自独立地选自氢、直链或支链C1-C10烷基、直链或支链C2-C6烯基、直链或支链C3-C6炔基、C3-C10环烷基、C6-C10芳基、C1-C10直链、环状或支链烷氧基,如上所定义的有机氨基(NR1R2)和选自Cl、Br和I的卤基。
11.根据权利要求10所述的方法,其中所述至少一种有机氨基-乙烯基硅烷前体包含至少一种选自以下的化合物:三(乙基氨基)乙烯基硅烷、三(异丙基氨基)乙烯基硅烷、三(叔丁基氨基)乙烯基硅烷、三(N-乙基甲基氨基)乙烯基硅烷、三(N-甲基环己基氨基)乙烯基硅烷、三(N-甲基苯基氨基)乙烯基硅烷、三(吡咯烷基)乙烯基硅烷、三(哌啶子基)乙烯基硅烷、三(吡咯基)乙烯基硅烷、双(乙基氨基)甲基乙烯基硅烷、双(叔丁基氨基)甲基乙烯基硅烷、双(N-甲基环己基氨基)甲基乙烯基硅烷、双(N-甲基苯基氨基)甲基乙烯基硅烷、二(吡咯烷基)甲基乙烯基硅烷、二(哌啶子基)甲基乙烯基硅烷、二(吡咯基)甲基乙烯基硅烷、双(乙基氨基)二乙烯基硅烷、双(正丙基氨基)二乙烯基硅烷、双(仲丁基氨基)二乙烯基硅烷、双(N-乙基甲基氨基)二乙烯基硅烷、双(二乙基氨基)二乙烯基硅烷、双(N-甲基环己基氨基)二乙烯基硅烷、双(N-甲基苯基氨基)二乙烯基硅烷、二(吡咯烷基)二乙烯基硅烷、二(哌啶子基)二乙烯基硅烷、二(吡咯基)二乙烯基硅烷、(正丙基氨基)二甲基乙烯基硅烷、(仲丁基氨基)二甲基乙烯基硅烷、(叔丁基氨基)二甲基乙烯基硅烷、(N-乙基甲基氨基)二甲基乙烯基硅烷、(N-甲基环己基氨基)二甲基乙烯基硅烷、(N-甲基苯基氨基)二甲基乙烯基硅烷、(吡咯烷基)二甲基乙烯基硅烷、(哌啶子基)二甲基乙烯基硅烷、(吡咯基)二甲基乙烯基硅烷、(甲基氨基)甲基二乙烯基硅烷、(乙基氨基)甲基二乙烯基硅烷、(正丙基氨基)甲基二乙烯基硅烷、(异丙基氨基)甲基二乙烯基硅烷、(仲丁基氨基)甲基二乙烯基硅烷、(叔丁基氨基)甲基二乙烯基硅烷、(二甲基氨基)甲基二乙烯基硅烷、(N-乙基甲基氨基)甲基二乙烯基硅烷、(N-甲基环己基氨基)甲基二乙烯基硅烷、(N-甲基苯基氨基)甲基二乙烯基硅烷、(吡咯烷基)甲基二乙烯基硅烷、(哌啶子基)甲基二乙烯基硅烷、(吡咯基)甲基二乙烯基硅烷、(甲基氨基)三乙烯基硅烷、(乙基氨基)三乙烯基硅烷、(正丙基氨基)三乙烯基硅烷、(异丙基氨基)三乙烯基硅烷、(仲丁基氨基)三乙烯基硅烷、(叔丁基氨基)三乙烯基硅烷、(N-乙基甲基氨基)三乙烯基硅烷、(二乙基氨基)三乙烯基硅烷、(N-甲基环己基氨基)三乙烯基硅烷、(N-甲基苯基氨基)甲基二乙烯基硅烷、(吡咯烷基)甲基三乙烯基硅烷、(哌啶子基)三乙烯基硅烷和(吡咯基)三乙烯基硅烷。
12.根据权利要求10所述的方法,其中所述至少一种有机氨基-烯丙基硅烷前体包括至少一种选自以下的化合物:三(甲基氨基)烯丙基硅烷、三(乙基氨基)烯丙基硅烷、三(正丙基氨基)烯丙基硅烷、三(异丙基氨基)烯丙基硅烷、三(仲丁基氨基)烯丙基硅烷、三(叔丁基氨基)烯丙基硅烷、三(N-甲基环己基氨基)烯丙基硅烷、三(N-甲基苯基氨基)烯丙基硅烷、三(吡咯烷基)烯丙基硅烷、三(哌啶子基)烯丙基硅烷、三(吡咯基)烯丙基硅烷、双(乙基氨基)甲基烯丙基硅烷、双(正丙基氨基)甲基烯丙基硅烷、双(仲丁基氨基)甲基烯丙基硅烷、双(叔丁基氨基)甲基烯丙基硅烷、双(N-甲基环己基氨基)甲基烯丙基硅烷、双(N-甲基苯基氨基)甲基烯丙基硅烷、二(吡咯烷基)甲基烯丙基硅烷、二(哌啶子基)甲基烯丙基硅烷、二(吡咯基)甲基烯丙基硅烷、双(甲基氨基)二烯丙基硅烷、双(乙基氨基)二烯丙基硅烷、双(正丙基氨基)二烯丙基硅烷、双(仲丁基氨基)二烯丙基硅烷、双(二乙基氨基)二烯丙基硅烷、双(N-甲基环己基氨基)二烯丙基硅烷、双(N-甲基苯基氨基)二烯丙基硅烷、二(吡咯烷基)二烯丙基硅烷、二(哌啶子基)二烯丙基硅烷、二(吡咯基)二烯丙基硅烷、(乙基氨基)二甲基烯丙基硅烷、(正丙基氨基)二甲基烯丙基硅烷、(异丙基氨基)二甲基烯丙基硅烷、(仲丁基氨基)二甲基烯丙基硅烷、(叔丁基氨基)二甲基烯丙基硅烷、(N-乙基甲基氨基)二甲基烯丙基硅烷、(N-甲基环己基氨基)二甲基烯丙基硅烷、(N-甲基苯基氨基)二甲基烯丙基硅烷、(吡咯烷基)二甲基烯丙基硅烷、(哌啶子基)二甲基烯丙基硅烷、(吡咯基)二甲基烯丙基硅烷、(甲基氨基)甲基二烯丙基硅烷、(乙基氨基)甲基二烯丙基硅烷、(正丙基氨基)甲基二烯丙基硅烷、(异丙基氨基)甲基二烯丙基硅烷、(仲丁基氨基)甲基二烯丙基硅烷、(叔丁基氨基)甲基二烯丙基硅烷、(二甲基氨基)甲基二烯丙基硅烷、(N-乙基甲基氨基)甲基二烯丙基硅烷、(N-甲基环己基氨基)甲基二烯丙基硅烷、(N-甲基苯基氨基)甲基二烯丙基硅烷、(吡咯烷基)甲基二烯丙基硅烷、(哌啶子基)甲基二烯丙基硅烷、(吡咯基)甲基二烯丙基硅烷、(甲基氨基)三烯丙基硅烷、(乙基氨基)三烯丙基硅烷、(正丙基氨基)三烯丙基硅烷、(异丙基氨基)三烯丙基硅烷、(仲丁基氨基)三烯丙基硅烷、(叔丁基氨基)三烯丙基硅烷、(二甲基氨基)三烯丙基硅烷、(N-乙基甲基氨基)三烯丙基硅烷、(二乙基氨基)三烯丙基硅烷、(N-甲基环己基氨基)三烯丙基硅烷、(N-甲基苯基氨基)甲基二烯丙基硅烷、(吡咯烷基)甲基三烯丙基硅烷、(哌啶子基)三烯丙基硅烷和(吡咯基)三烯丙基硅烷。
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