TWI798765B - 用於鍺種子層的組合物及使用其的方法 - Google Patents
用於鍺種子層的組合物及使用其的方法 Download PDFInfo
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- TWI798765B TWI798765B TW110127119A TW110127119A TWI798765B TW I798765 B TWI798765 B TW I798765B TW 110127119 A TW110127119 A TW 110127119A TW 110127119 A TW110127119 A TW 110127119A TW I798765 B TWI798765 B TW I798765B
- Authority
- TW
- Taiwan
- Prior art keywords
- bis
- silane
- tris
- group
- butylamino
- Prior art date
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- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 229910052732 germanium Inorganic materials 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 89
- 239000000203 mixture Substances 0.000 title claims description 32
- 239000002243 precursor Substances 0.000 claims abstract description 184
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 95
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 95
- 239000010703 silicon Substances 0.000 claims abstract description 84
- 239000000758 substrate Substances 0.000 claims abstract description 69
- -1 C 6 alkyne Chemical class 0.000 claims description 108
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 43
- 238000010926 purge Methods 0.000 claims description 40
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 38
- 239000007789 gas Substances 0.000 claims description 37
- 239000001257 hydrogen Substances 0.000 claims description 36
- 229910052739 hydrogen Inorganic materials 0.000 claims description 36
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 34
- 229910052760 oxygen Inorganic materials 0.000 claims description 34
- 239000001301 oxygen Substances 0.000 claims description 34
- 238000006243 chemical reaction Methods 0.000 claims description 31
- DNAJDTIOMGISDS-UHFFFAOYSA-N prop-2-enylsilane Chemical compound [SiH3]CC=C DNAJDTIOMGISDS-UHFFFAOYSA-N 0.000 claims description 28
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 26
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 26
- 239000007983 Tris buffer Substances 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 24
- 229910000077 silane Inorganic materials 0.000 claims description 23
- HKILWKSIMZSWQX-UHFFFAOYSA-N tris(prop-2-enyl)silane Chemical compound C=CC[SiH](CC=C)CC=C HKILWKSIMZSWQX-UHFFFAOYSA-N 0.000 claims description 20
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 19
- 125000006309 butyl amino group Chemical group 0.000 claims description 18
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 18
- 125000003118 aryl group Chemical group 0.000 claims description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 15
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 14
- 125000004122 cyclic group Chemical group 0.000 claims description 13
- 125000000008 (C1-C10) alkyl group Chemical group 0.000 claims description 12
- 125000003277 amino group Chemical group 0.000 claims description 12
- 229910000078 germane Inorganic materials 0.000 claims description 10
- 150000002431 hydrogen Chemical class 0.000 claims description 10
- 125000003545 alkoxy group Chemical group 0.000 claims description 9
- 125000000304 alkynyl group Chemical group 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- 238000005137 deposition process Methods 0.000 claims description 9
- 125000000882 C2-C6 alkenyl group Chemical group 0.000 claims description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- 125000003342 alkenyl group Chemical group 0.000 claims description 8
- 125000000031 ethylamino group Chemical group [H]C([H])([H])C([H])([H])N([H])[*] 0.000 claims description 8
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 8
- 150000001412 amines Chemical class 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- VXGHASBVNMHGDI-UHFFFAOYSA-N digermane Chemical compound [Ge][Ge] VXGHASBVNMHGDI-UHFFFAOYSA-N 0.000 claims description 7
- 150000004820 halides Chemical class 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 6
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 6
- 125000001664 diethylamino group Chemical group [H]C([H])([H])C([H])([H])N(*)C([H])([H])C([H])([H])[H] 0.000 claims description 6
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 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
- 125000000250 methylamino group Chemical group [H]N(*)C([H])([H])[H] 0.000 claims description 6
- 125000004888 n-propyl amino group Chemical group [H]N(*)C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- 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 description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 4
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 4
- 229910052794 bromium Inorganic materials 0.000 claims description 4
- OPDQOJBKHNWJGO-UHFFFAOYSA-N butylgermane Chemical compound CCCC[GeH3] OPDQOJBKHNWJGO-UHFFFAOYSA-N 0.000 claims description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 4
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 4
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 3
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 3
- PQBRMCFHKXVJHS-UHFFFAOYSA-N benzylgermane Chemical group [GeH3]CC1=CC=CC=C1 PQBRMCFHKXVJHS-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
- MUDDKLJPADVVKF-UHFFFAOYSA-N trichlorogermane Chemical group 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
- PMSZNCMIJVNSPB-UHFFFAOYSA-N bis(ethenyl)silicon Chemical compound C=C[Si]C=C PMSZNCMIJVNSPB-UHFFFAOYSA-N 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- XVSBWQYHSLNOCU-UHFFFAOYSA-N ethenyl(dimethyl)silicon Chemical compound C[Si](C)C=C XVSBWQYHSLNOCU-UHFFFAOYSA-N 0.000 claims description 2
- IQSBKDJPSOMMRZ-UHFFFAOYSA-N ethenyl(methyl)silane Chemical compound C[SiH2]C=C IQSBKDJPSOMMRZ-UHFFFAOYSA-N 0.000 claims description 2
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 2
- BNCOGDMUGQWFQE-UHFFFAOYSA-N tris(ethenyl)silicon Chemical compound C=C[Si](C=C)C=C BNCOGDMUGQWFQE-UHFFFAOYSA-N 0.000 claims description 2
- PYGSKMBEVAICCR-UHFFFAOYSA-N hexa-1,5-diene Chemical group C=CCCC=C PYGSKMBEVAICCR-UHFFFAOYSA-N 0.000 claims 3
- 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
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims 2
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 claims 2
- YQOTVKVZLFHCKW-UHFFFAOYSA-N bis(ethenyl)-methylsilane Chemical compound C=C[SiH](C)C=C YQOTVKVZLFHCKW-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
- ANWAYCXEBCXPDS-UHFFFAOYSA-N 1-N,1-N',2-N-tri(propan-2-yl)-2-silylethene-1,1,2-triamine Chemical compound CC(C)NC([SiH3])=C(NC(C)C)NC(C)C ANWAYCXEBCXPDS-UHFFFAOYSA-N 0.000 claims 1
- KNDAUNKFZNWQDC-UHFFFAOYSA-N 1-N,1-N',2-N-triethyl-1-N,1-N',2-N-trimethyl-2-silylethene-1,1,2-triamine Chemical compound C(C)N(C)C(=C(N(CC)C)N(CC)C)[SiH3] KNDAUNKFZNWQDC-UHFFFAOYSA-N 0.000 claims 1
- DYCAFSBAVJVVQZ-UHFFFAOYSA-N 1-N,1-N',2-N-trimethyl-2-silylethene-1,1,2-triamine Chemical compound CNC([SiH3])=C(NC)NC DYCAFSBAVJVVQZ-UHFFFAOYSA-N 0.000 claims 1
- LLWBDWYAIZEDJM-UHFFFAOYSA-N 1-N,1-N',2-N-tripropyl-2-silylethene-1,1,2-triamine Chemical compound CCCNC([SiH3])=C(NCCC)NCCC LLWBDWYAIZEDJM-UHFFFAOYSA-N 0.000 claims 1
- RQZYYCOREVDUCN-UHFFFAOYSA-N 1-N,1-N',2-N-tritert-butyl-2-silylethene-1,1,2-triamine Chemical compound C(C)(C)(C)NC(=C(NC(C)(C)C)NC(C)(C)C)[SiH3] RQZYYCOREVDUCN-UHFFFAOYSA-N 0.000 claims 1
- FKILQBLJPXJVFV-UHFFFAOYSA-N 1-N,1-N'-diethyl-1-N,1-N'-dimethyl-3-silylprop-2-ene-1,1-diamine Chemical compound C(C)N(C)C(N(CC)C)C=C[SiH3] FKILQBLJPXJVFV-UHFFFAOYSA-N 0.000 claims 1
- OBDJPEHJGIQFQF-UHFFFAOYSA-N 1-N,1-N'-diethyl-3-silylprop-2-ene-1,1-diamine Chemical compound C(C)NC(NCC)C=C[SiH3] OBDJPEHJGIQFQF-UHFFFAOYSA-N 0.000 claims 1
- HGHMAGZNILOXBQ-UHFFFAOYSA-N 1-N,1-N'-dimethyl-3-silylprop-2-ene-1,1-diamine Chemical compound CNC(NC)C=C[SiH3] HGHMAGZNILOXBQ-UHFFFAOYSA-N 0.000 claims 1
- IWQCJXBBQZOOAK-UHFFFAOYSA-N 1-N,1-N'-dipropyl-3-silylprop-2-ene-1,1-diamine Chemical compound C(CC)NC(NCCC)C=C[SiH3] IWQCJXBBQZOOAK-UHFFFAOYSA-N 0.000 claims 1
- LCKNILBGIZSDBX-UHFFFAOYSA-N 1-N,1-N'-ditert-butyl-3-silylprop-2-ene-1,1-diamine Chemical compound C(C)(C)(C)NC(NC(C)(C)C)C=C[SiH3] LCKNILBGIZSDBX-UHFFFAOYSA-N 0.000 claims 1
- OXXLYTYJKPAXFC-UHFFFAOYSA-N 1-N,1-N,1-N',1-N',2-N,2-N-hexamethyl-2-silylethene-1,1,2-triamine Chemical compound CN(C)C([SiH3])=C(N(C)C)N(C)C OXXLYTYJKPAXFC-UHFFFAOYSA-N 0.000 claims 1
- FGDGAYJQUFBEHU-UHFFFAOYSA-N 1-N,1-N,1-N',1-N'-tetraethyl-3-silylprop-2-ene-1,1-diamine Chemical compound C(C)N(CC)C(N(CC)CC)C=C[SiH3] FGDGAYJQUFBEHU-UHFFFAOYSA-N 0.000 claims 1
- 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 1
- GSHSUXAWVWLKNK-UHFFFAOYSA-N 3,3-di(piperidin-1-yl)prop-1-enylsilane Chemical compound N1(CCCCC1)C(N1CCCCC1)C=C[SiH3] GSHSUXAWVWLKNK-UHFFFAOYSA-N 0.000 claims 1
- MOFYWKAYHMTHHL-UHFFFAOYSA-N 3,3-dipyrrolidin-1-ylprop-1-enylsilane Chemical compound N1(CCCC1)C(N1CCCC1)C=C[SiH3] MOFYWKAYHMTHHL-UHFFFAOYSA-N 0.000 claims 1
- 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
- JDYBVMXLZQUVMU-UHFFFAOYSA-N C(C)N(CC)C(=C(N(CC)CC)N(CC)CC)[SiH3] Chemical compound C(C)N(CC)C(=C(N(CC)CC)N(CC)CC)[SiH3] JDYBVMXLZQUVMU-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
- QKSVAZOJBRGDRR-UHFFFAOYSA-N CCCNC[SiH](C=C)C=C Chemical compound CCCNC[SiH](C=C)C=C QKSVAZOJBRGDRR-UHFFFAOYSA-N 0.000 claims 1
- YECLNFRHUMDEHK-UHFFFAOYSA-N CCN(CC)C[SiH](C=C)C=C Chemical compound CCN(CC)C[SiH](C=C)C=C YECLNFRHUMDEHK-UHFFFAOYSA-N 0.000 claims 1
- BTMSCHNODALZOT-UHFFFAOYSA-N CCNC[SiH](C=C)C=C Chemical compound CCNC[SiH](C=C)C=C BTMSCHNODALZOT-UHFFFAOYSA-N 0.000 claims 1
- DLIHLVCEJBKTIL-UHFFFAOYSA-N CN(C(C=C[SiH3])N(C)C1=CC=CC=C1)C1=CC=CC=C1 Chemical compound CN(C(C=C[SiH3])N(C)C1=CC=CC=C1)C1=CC=CC=C1 DLIHLVCEJBKTIL-UHFFFAOYSA-N 0.000 claims 1
- CAFDJKXNGMQWHK-UHFFFAOYSA-N CN(C(C=C[SiH3])N(C)C1CCCCC1)C1CCCCC1 Chemical compound CN(C(C=C[SiH3])N(C)C1CCCCC1)C1CCCCC1 CAFDJKXNGMQWHK-UHFFFAOYSA-N 0.000 claims 1
- WJMVISVOURZCAR-UHFFFAOYSA-N CN(C(N(C)C1=CC=CC=C1)=C(N(C)C1=CC=CC=C1)[SiH3])C1=CC=CC=C1 Chemical compound CN(C(N(C)C1=CC=CC=C1)=C(N(C)C1=CC=CC=C1)[SiH3])C1=CC=CC=C1 WJMVISVOURZCAR-UHFFFAOYSA-N 0.000 claims 1
- OVLSHXGCNCWFNH-UHFFFAOYSA-N CN(C1CCCCC1)C(N(C)C1CCCCC1)=C(N(C)C1CCCCC1)[SiH3] Chemical compound CN(C1CCCCC1)C(N(C)C1CCCCC1)=C(N(C)C1CCCCC1)[SiH3] OVLSHXGCNCWFNH-UHFFFAOYSA-N 0.000 claims 1
- XSPSZYNINVDFMI-UHFFFAOYSA-N CN(C[SiH](C=C)C=C)C1=CC=CC=C1 Chemical compound CN(C[SiH](C=C)C=C)C1=CC=CC=C1 XSPSZYNINVDFMI-UHFFFAOYSA-N 0.000 claims 1
- GQSUXVFTKQFNPJ-UHFFFAOYSA-N CN(C[SiH](C=C)C=C)C1CCCCC1 Chemical compound CN(C[SiH](C=C)C=C)C1CCCCC1 GQSUXVFTKQFNPJ-UHFFFAOYSA-N 0.000 claims 1
- MSIMSBAIFIHIQB-UHFFFAOYSA-N CNC[SiH](C=C)C=C Chemical compound CNC[SiH](C=C)C=C MSIMSBAIFIHIQB-UHFFFAOYSA-N 0.000 claims 1
- SMYULUMLLSYCMM-UHFFFAOYSA-N N-(2-methylprop-1-enylsilyl)methanamine Chemical compound CN[SiH2]C=C(C)C SMYULUMLLSYCMM-UHFFFAOYSA-N 0.000 claims 1
- AIZMLGUZUBYMER-UHFFFAOYSA-N N-(2-methylprop-1-enylsilyl)propan-2-amine Chemical compound CC(=C[SiH2]NC(C)C)C AIZMLGUZUBYMER-UHFFFAOYSA-N 0.000 claims 1
- 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 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
- OCTHFCZOQHUXHH-UHFFFAOYSA-N N-ethyl-N-(2-methylprop-1-enylsilyl)ethanamine Chemical compound C(C)N(CC)[SiH2]C=C(C)C OCTHFCZOQHUXHH-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
- 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 1
- 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 1
- 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 1
- 150000001335 aliphatic alkanes Chemical class 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
- BYGPHVDRRUADAB-UHFFFAOYSA-N butyl-bis(ethenyl)silane Chemical compound CCCC[SiH](C=C)C=C BYGPHVDRRUADAB-UHFFFAOYSA-N 0.000 claims 1
- GLOFHIIPHZHSCO-UHFFFAOYSA-N ethenyl-dimethyl-piperidin-1-ylsilane Chemical compound C=C[Si](C)(C)N1CCCCC1 GLOFHIIPHZHSCO-UHFFFAOYSA-N 0.000 claims 1
- 125000005394 methallyl group Chemical group 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
- ODVDDQFBQGTLIA-UHFFFAOYSA-N n-[bis(ethenyl)-(ethylamino)silyl]ethanamine Chemical compound CCN[Si](C=C)(C=C)NCC ODVDDQFBQGTLIA-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
- 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 1
- 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 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
- 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
- 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
- PTLBSZDLZXSEDD-UHFFFAOYSA-N n-tris(ethenyl)silylethanamine Chemical compound CCN[Si](C=C)(C=C)C=C PTLBSZDLZXSEDD-UHFFFAOYSA-N 0.000 claims 1
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/188—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-O linkages
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/10—Compounds having one or more C—Si linkages containing nitrogen having a Si-N linkage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/1892—Preparation; Treatments not provided for in C07F7/20 by reactions not provided for in C07F7/1876 - C07F7/1888
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
-
- 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
- C23C16/06—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 metallic material
-
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Abstract
本發明關於用於(a)形成含矽膜及(b)將基材表面官能化以生成適用於沉積鍺膜的鍺種子層之前驅物及方法。在一態樣中,提供如本文所述的式I的前驅物及/或式II的前驅物:
Description
本發明關於可用以沉積含矽膜並且生成適用於產生鍺種子層的乙烯基官能化表面之有機矽化合物,該鍺種子層有利於在固體基材表面上生長高品質的還原或金屬鍺膜。本發明也關於使用該化合物的方法。
本文描述的是經由熱原子層沉積(ALD)或電漿強化原子層 (PEALD)製程或其組合沉積含矽膜例如,但不限於,氧化矽、氧氮化矽、氧碳氮化矽或碳摻雜氧化矽之新穎有機胺基乙烯基矽烷及有機胺基烯丙基矽烷前驅物化合物及包含其的組合物及方法。更明確地,本文描述的是用於包括舉例來說約25°C至約350 ℃在內的約600°C或更低的一或更多沉積溫度下形成化學計量或非化學計量含矽膜或材料的組合物及方法,其中所得膜係於以乙烯基官能基封端並且適用於形成鍺種子層。
在介電基材例如使用鍺烷和二鍺烷的氧化矽表面上電漿強化化學氣相沉積(PECVD)或熱化學氣相沉積(CVD)鍺膜長期存在的問題之一係鍺烷化合物與基材表面羥基的反應性遠小於形成Ge-Ge鍵時使Ge-H鍵分解的反應性。此反應性失配的結果是該基材上形成了鍺塊島而不是平滑膜。為了克服此“島效應”或“島生長”,這會導致所得鍺膜的表面粗糙度很高,首先必須在該表面上舖一平滑種子層,這提供了一平滑的起始表面並且允許隨後的鍺膜均勻生長。然而,使用典型的PECVD或CVD鍺前驅物在介電基材表面上生長此種子層仍然遇到 CVD的典型缺點例如厚度控制、介電表面選擇性低、非自限反應性及低共形性(conformality)。
已知前驅物及方法的實例係揭示於以下公開、專利及專利申請案中。
公開編號EP1464724A2揭示具有式MX
aH
b(NR
1R
2)
cR
3 dR
4 e的含矽和鍺的前驅物,其適用於矽和鍺膜的化學氣相沉積。
Famá, S等人,
Appl. Phys. Lett. 2002,
81, 586描述矽上鍺的磊晶生長,首先藉由化學氣相沉積在350 °C下用GeH
4沉積薄Ge/Si緩衝層,然後在600 °C下化學氣相沉積較厚的鍺膜以達成製造
p-
i-
n光電探測器的目的。
Hair, M. L. 等人,
Phys. Chem. 1969,
73, 2372報導用氯矽烷將二氧化矽官能化的方法,與甲氧基矽烷(100至200 °C)相比,氯矽烷在300至400 °C之間以令人滿意的速率於氣相中發生。
Miao, Q. J. 等人,
Catal. Commun. 2003,
4, 637描述在回流條件作用之下在甲苯中用乙烯基三乙氧基矽烷處理發煙二氧化矽48小時,然後與水反應另外48小時以用乙烯基將該表面官能化。
Zapilko, C.等人,
J. Am. Chem. Soc. 2006,
128, 16266描述藉由在甲苯中用經乙烯基取代的三甲矽烷基胺在109 °C下處理15小時,用氯丙基二甲基矽烷基及乙烯基二甲基矽烷基對周期性介孔二氧化矽進行官能化。
美國專利第8,460,753 B2號描述藉由ALD或CVD沉積二氧化矽或氧化矽膜的前驅物及方法,其中該前驅物係具有式R
1 nR
2 mSi(NR
3R
4)
4-n-m的胺基乙烯基矽烷及具有式(R
1R
2SiNR
3)
p的環狀矽氮烷,其中R
1係烯基或芳族,例如乙烯基、烯丙基及苯基。
美國公開案第20150275355 A1號描述使用具有式R
1 nSi(NR
2R
3)
mH
4-m-n的前驅物,更明確地使用有機胺基甲基矽烷前驅物來形成氧化矽膜的組合物及方法。
美國公開案第20090162973 A1號描述使用具有式GeR
x 1(NR
2R
3)
(4-x)的含鍺前驅物將鍺膜或碲化鍺銻膜沉積於基材上,其中該方法涉及將該基材單獨或與氧化氣體或還原氣體聯合暴露於該含鍺前驅物。
美國公開案第20110036289 A1號描述一種使用GeH
4前驅物在低溫下經由CVD將鍺種子層沉積於經氫處理的矽基材上,接著在高溫下分別在膦或乙硼烷存在下使用GeH
4前驅物進行隨後n摻雜或p摻雜的鍺磊晶膜的生長之方法。
美國公開案第20110084308 A1號揭示一種在圖案化矽基材上選擇性地生長高品質應變或應變弛豫鍺的方法,該方法首先經由CVD在350至400 °C下用S
i2H
6及GeH
4前驅物生長矽鍺緩衝層,然後經由 CVD在350至400 °C下用 GeH
4前驅物生長鍺種子層,然後經由CVD在550至600 °C下用GeH
4前驅物生長鍺磊晶膜。
美國公開案第20130230975 A1號及第20140331928 A1號二者皆描述使用以胺基鍺烷為主的氣體在基材上形成鍺種子層,然後使用以鍺烷為主的氣體生長鍺膜。
將先前確定的專利及專利申請案的揭示內容以引用的方式併入本文。
本領域中仍然需要用於介電基材表面上沉積平滑的高品質還原或金屬鍺膜的前驅物及方法。
與先前技藝相比,本文揭示的發明中的種子層前驅物利用矽-胺官能基作為錨定基團將乙烯基或烯丙基連接到表面。此化學反應將富含羥基的表面轉化為富含乙烯基或烯丙基的表面。然後,將鍺烷或二鍺烷或另一具有至少一Ge-H鍵的鍺前驅物引入艙室並且在鍺氫化反應(hydrogermylation reaction)中與乙烯基及/或烯丙基反應,並且在該表面上形成碳鍵合的鍺烷基或二鍺烷基。後續使用鍺前驅物沉積的鍺膜將立即長在此富含鍺烷基的表面上而不會形成島。
本文描述的是包含至少一乙烯基或烯丙基和至少一有機胺基錨定基團的有機胺基乙烯基矽烷和有機胺基烯丙基矽烷家族之矽前驅物、包含其之組合物以及使用其沉積含矽膜和形成包含矽和乙烯基的單層膜之方法,其可促進適用於沉積金屬薄膜,明確地說鍺薄膜,的種子層之沉積。除此之外,本文描述的是包含有機胺基乙烯基矽烷或有機胺基烯丙基矽烷的組合物,其實質上不含至少一選自有機胺、醇、鹵化物、較高分子量物種及痕量金屬的雜質物種。該組合物可另外包含溶劑。本文也揭示了在待加工的物體例如半導體晶圓上形成包含矽和乙烯基的膜或塗層之方法。
在本文所述方法之一具體實例中,在用於生成適用於生長鍺種子層及隨後高品質鍺膜的乙烯基封端層的條件之下,在沉積艙中使用有機胺基乙烯基矽烷或有機胺基烯丙基矽烷前驅物將包含矽和乙烯基的膜沉積於基材上。
更特別的是,上述目的及其他目的係藉由用於形成鍺種子層的方法來實現,其包括以下步驟:
a. 將基材提供至反應器中;
b. 將至少一由式I及/或II所示的前驅物引入該反應器中;
I II
其中R
1係選自由線性或分支C
1至C
10烷基、線性或分支C
3至C
10烯基、線性或分支C
3至C
10炔基、C
3至C
10環狀烷基及C
6至C
10芳基所組成的群組;R
2係選自由氫、線性或分支C
1至C
10烷基、線性或分支C
2至C
6烯基、線性或分支C
3至C
6炔基、C
3至C
10環狀烷基及C
6至C
10芳基所組成的群組;R
3及R
4係獨立地選自由以下所組成的群組:氫、線性或分支C
1至C
10烷基、線性或分支C
2至C
6烯基、線性或分支C
3至C
6炔基、C
3至C
10環狀烷基、C
6至C
10芳基、C
1至C
10線性、環狀或分支烷氧基、如上文定義的有機胺基(NR
1R
2)及選自由Cl、Br及I所組成的群組之鹵基(halide),
c. 用吹掃氣體吹掃該反應器;
d. 在一定溫度下引入至少一包含至少一Ge-H鍵的鍺前驅物以使該基材被塗覆至少一單層鍺;
e. 用吹掃氣體吹掃該反應器;
f. 視需要地引入氫或氫電漿源;
g. 視需要地用吹掃氣體吹掃該反應器;及
h. 在適於生長具有所需厚度的包含鍺的膜之溫度下引入與步驟d中相同或不同的鍺前驅物。
在本文所述方法之一具體實例中,該具有至少一Ge-H基團的鍺前驅物包括,但不限於,三氯鍺烷(Cl
3GeH)、鍺烷(GeH
4)、二鍺烷(Ge
2H
6)、第三丁基鍺烷(
tBuGeH
3)、苯基鍺烷、第二丁基鍺烷、異丁基鍺烷及苯甲基鍺烷中之其一或更多。
如同該方法之一步驟,根據一具體實例使用該式I的有機胺基乙烯基矽烷前驅物及/或該式II的有機胺基烯丙基矽烷前驅物及含氧源在產生氧化矽或碳摻雜氧化矽膜於基材上的條件之下將含矽和氧的膜沉積於該基材上。如同該方法之一步驟,根據另一具體實例使用該式I的有機胺基乙烯基矽烷前驅物及/或該式II的有機胺基烯丙基矽烷前驅物及含氮源在產生氮化矽、碳摻雜氮化矽、氧氮化矽或氧碳氮化矽膜於基材上的條件之下將包含矽和氮的膜沉積於該基材上。在另一具體實例中,以根據式I的有機胺基乙烯基矽烷前驅物及/或式II的有機胺基烯丙基矽烷前驅物用作含金屬膜的摻雜劑,例如但不限於,金屬氧化物膜或金屬氮化物膜。
在上述方法的某些具體實例中,步驟d和h可在相同溫度下進行,或步驟d可以在低於步驟h的溫度下進行以避免或限制步驟d中鍺膜的CVD,直到形成足夠的鍺種子層為止。在一些具體實例中,步驟d在高於步驟h的溫度下進行。在其他具體實例中,在步驟 d之後升高溫度以便在步驟g中的後續鍺CVD膜沉積之前對該至少一鍺單層(稱之為該種子層)進行熱退火或在視需要的氫或氫電漿處理期間進行退火。在又另一具體實例中,該至少一包含至少一Ge-H鍵的鍺前驅物與該鍺CVD前驅物相同。在其他具體實例中,該至少一包含至少一Ge-H鍵的鍺前驅物與該鍺CVD前驅物不同。
在另一態樣中,提供一種將固體基材,例如,但不限於,二氧化矽、氧化鋁、金屬氧化物、矽晶圓、介電薄膜或具有乙烯基及/或烯丙基的金屬表面,的表面官能化之方法,該方法包含以下步驟:
a. 將基材提供到反應器中;
b. 將至少一下式I所示的有機胺基乙烯基矽烷前驅物及/或至少一下式II所示的有機胺基烯丙基矽烷前驅物引入該反應器中,該有機胺基乙烯基矽烷前驅物包含連接到至少一矽原子的至少一乙烯基及至少一有機胺基錨定基團,該有機胺基烯丙基矽烷前驅物包含連接到至少一矽原子的至少一烯丙基及至少一有機胺基錨定基團;及
c. 用溶劑及/或吹掃氣體從該基材除去殘留的有機胺基乙烯基矽烷或有機胺基烯丙基矽烷。
在一些具體實例中,本文揭示的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物可以純液體的方式、以溶劑中溶液的方式或以有或沒有載氣的蒸氣相的方式在 介於0 °C 至 500 °C 的溫度下引至該固體基材上。
本文揭示的是矽前驅物化合物及使用其沉積含矽膜以及將用於後續加工(包括,但不限於,該鍺膜的沉積)的基材表面官能化之方法。
一種用於形成鍺種子層之特定方法包括以下步驟:
a. 將基材提供至反應器中;
b. 將至少一式I所示的有機胺基乙烯基矽烷前驅物及/或至少一下式II所示的有機胺基烯丙基矽烷前驅物引入該反應器中,該有機胺基乙烯基矽烷前驅物包含連接到至少一矽原子的至少一乙烯基及至少一有機胺基錨定基團,該有機胺基烯丙基矽烷前驅物包含連接到至少一矽原子的至少一烯丙基及至少一有機胺基錨定基團;
I II
其中R
1係選自由線性或分支C
1至C
10烷基、線性或分支C
3至C
10烯基、線性或分支C
3至C
10炔基、C
3至C
10環狀烷基及C
6至C
10芳基所組成的群組;R
2係選自由氫、線性或分支C
1至C
10烷基、線性或分支C
2至C
6烯基、線性或分支C
3至C
6炔基、C
3至C
10環狀烷基及C
6至C
10芳基所組成的群組;R
3及R
4係獨立地選自由以下所組成的群組:氫、線性或分支C
1至C
10烷基、線性或分支C
2至C
6烯基、線性或分支C
3至C
6炔基、C
3至C
10環狀烷基、C
6至C
10芳基、C
1至C
10線性、環狀或分支烷氧基、如上文定義的有機胺基(NR
1R
2)及選自由Cl、Br及I所組成的群組之鹵基,
c. 用吹掃氣體吹掃該反應器;
d. 在一定溫度下引入至少一包含至少一Ge-H鍵的鍺前驅物以使該基材被塗覆至少一單層鍺;
e. 用吹掃氣體吹掃該反應器;
f. 視需要地引入氫或氫電漿源;
g. 視需要地用吹掃氣體吹掃該反應器;及
h. 在適於生長具有所需厚度的包含鍺的膜之溫度下引入與步驟d中相同或不同的鍺前驅物。
在某些具體實例中,R
1與R
2相同。在其他具體實例中,R
1與R
2不同。在某些具體實例中,R
3與R
4相同。在其他具體實例中,R
3與R
4不同。
在一些較佳具體實例中,R
3及R
4係獨立地選自由氫、甲基、乙烯基及烯丙基所組成的群組。
本文所述的有機胺基乙烯基矽烷和有機胺基烯丙基矽烷前驅物係用以形成含矽加上乙烯基及/或烯丙基的單層膜以及化學計量和非化學計量含矽膜,例如但不限於、非晶矽、結晶矽、氧化矽、碳摻雜氧化矽、氧碳化矽、氮化矽、氧氮化矽及氧碳化矽。這些前驅物也可用作,舉例來說,含金屬膜的摻雜劑。半導體製程中使用的有機胺基乙烯基矽烷和有機胺基烯丙基矽烷前驅物通常為高純度的揮發性液體化學品,其係汽化並且以氣體的方式輸送到沉積艙或反應器以經由用於半導體裝置的CVD或ALD製程沉積含矽膜,然而,其也可以液相(純態或有溶劑)被引到基材處。用於沉積的前驅物材料的選擇取決於所需的所得含矽材料或膜。舉例來說,前驅物材料可根據其化學元素的含量、化學元素的化學計量比及/或在CVD作用之下形成的所得含矽膜或塗層來選擇。該前驅物材料也可根據各種其他特性例如成本、相對低的毒性、處理特性、在室溫下保持液相的能力、揮發性、分子量、熱安定性及/或其他考慮因素來選擇。在某些具體實例中,本文所述的前驅物可藉由多種方式,較佳地使用裝配適當閥及配件的可加壓不銹鋼容器,輸送到該反應器系統以允許輸送液相或氣相前驅物物到該沉積艙或反應器。
另一用於形成鍺種子層的特定方法包括以下步驟:
a. 將基材提供至反應器中;
b. 將至少一式I所示的有機胺基乙烯基矽烷前驅物及/或至少一下式II所示的有機胺基烯丙基矽烷前驅物引入該反應器中,該有機胺基乙烯基矽烷前驅物包含連接到至少一矽原子的至少一乙烯基及至少一有機胺基錨定基團,該有機胺基烯丙基矽烷前驅物包含連接到至少一矽原子的至少一烯丙基及至少一有機胺基錨定基團;
I II
其中R
1係選自由線性或分支C
1至C
10烷基、線性或分支C
3至C
10烯基、線性或分支C
3至C
10炔基、C
3至C
10環狀烷基及C
6至C
10芳基所組成的群組;R
2係選自由氫、線性或分支C
1至C
10烷基、線性或分支C
2至C
6烯基、線性或分支C
3至C
6炔基、C
3至C
10環狀烷基及C
6至C
10芳基所組成的群組;R
3及R
4係獨立地選自由以下所組成的群組:氫、線性或分支C
1至C
10烷基、線性或分支C
2至C
6烯基、線性或分支C
3至C
6炔基、C
3至C
10環狀烷基、C
6至C
10芳基、C
1至C
10線性、環狀或分支烷氧基、如上文定義的有機胺基(NR
1R
2)及選自由Cl、Br及I所組成的群組之鹵基(halide),
c. 用吹掃氣體吹掃該反應器;
d. 引入含氧源;
e. 用吹掃氣體吹掃該反應器;
f. 再引入上述有機胺基乙烯基矽烷或有機胺基烯丙基矽烷前驅物;
g. 用吹掃氣體吹掃該反應器;
h. 在一定溫度下引入至少一包含至少一Ge-H鍵的鍺前驅物以使該基材被塗覆至少一單層鍺;
i. 用吹掃氣體吹掃該反應器;
j. 視需要地引入氫或氫電漿源;
k. 視需要地用吹掃氣體吹掃該反應器;及
l. 在適於生長具有所需厚度的包含鍺的膜之溫度下引入與步驟d中相同或不同的鍺前驅物;
其中重複步驟b到e直到在沉積該鍺種子層及隨後的含鍺膜之前沉積所需厚度的含矽膜為止。
在某些具體實例中,R
1與R
2相同。在其他具體實例中,R
1與R
2不同。在某些具體實例中,R
3與R
4相同。在其他具體實例中,R
3與R
4不同。
在一些較佳具體實例中,R
3及R
4係獨立地選自由氫、甲基、乙烯基及烯丙基所組成的群組。
使用本文所述的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物沉積的含矽膜,無論是單一單層或大於單一單層,皆可用作適合與包含至少一Ge-H鍵的鍺前驅物反應的基材。不欲受理論的束縛,據信當該基材的表面與本文所述的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物反應時,其便會被乙烯基及/或烯丙基官能化,或更明確地說被乙烯基矽烷基及/或烯丙基矽烷基官能化。這些基團隨後可與鍺前驅物分子的Ge-H鍵進行鍺氫化反應,因此只要有可用的乙烯基及/或烯丙基基團便能將鍺原子或鍺基團錨定於該表面上。此反應中的乙烯基及/或烯丙基轉化為Si及Ge原子之間的伸乙基、亞乙基(ethylidene)、伸丙基或甲基伸乙基連接基。一旦該基材的表面均勻地塗佈鍺烷基,其就可備用於藉由ALD、PEALD、CVD、循環式CVD或PECVD製程沉積鍺膜,大多數情況下在升高的溫度下,但是在某些情況下在相同的溫度下。在某些具體實例中,錨固於該表面上的鍺烷基必須先用還原氣體(例如,但不限於,氫氣或氫電漿)還原,以產生以–GeH
x(x = 0、1、2、3)封端的表面。
包含至少一Ge-H鍵的例示性鍺前驅物包括,但不限於,三氯鍺烷(Cl
3GeH)、鍺烷(GeH
4)、二鍺烷(Ge
2H
6)、第三丁基鍺烷(
tBuGeH
3)、苯基鍺烷、第二丁基鍺烷、異丁基鍺烷及苯甲基鍺烷。
圖1描繪整體架構,其中使用本文揭示的具有式I的有機胺基乙烯基矽烷前驅物以(a)用乙烯基將基材表面官能化,使其適用於(b)經由與包含至少一Ge-H鍵的鍺前驅物的鍺氫化反應形成鍺種子層,允許(c)隨後使用至少一ALD或CVD Ge前驅物在該種子層頂部生長平滑均勻的鍺膜。相同類型的架構適用於在圖1的步驟(a)中使用具有本文揭示的式II的有機胺基烯丙基矽烷前驅物之方法,不同之處在於該基材將用烯丙基而不是用乙烯基來官能化。
據信,當基材以-GeH
x(x = 0、1、2、3)基團均勻封端時,由於預先用本文揭示的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物對其均勻處理,於是將其用作種子層,其允許具有非常低不均勻性和低表面粗糙度的非晶性或結晶性鍺膜的後續生長。咸認為藉由在鍺膜沉積開始時消除熟知該領域之習知技藝者已知的“島生長”現象能夠獲得平滑且均勻的鍺膜。藉由將非反應性有機、介電、金屬或任何其他非反應性表面轉化為用鍺原子或鍺烷基官能化的反應性表面,人們可開始沉積鍺膜而不會使該表面形成“島”。此平滑的保形初始層係高品質鍺種子層的特徵。
本文所述的有機胺基乙烯基矽烷及有機胺基烯丙基矽烷前驅物顯現出反應性及安定性的平衡,這使得其非常適合作為微電子裝置製程中的CVD或ALD前驅物。關於反應性,本發明的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷具有至少一有機胺基基團(NR
1R
2),其有助於使有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物與羥基表面在ALD製程期間起反應。儘管本發明中最常提到的羥基表面係介電表面例如氧化矽、氮化矽、矽(具有天然氧化物)、金屬氧化物、金屬氮化物或金屬(具有天然氧化物),但是預期其他可能含有表面羥基的材料,舉例來說,有機聚合物、有機矽、樹脂、塑料、珠粒、吸附劑、非晶形碳、活性碳、礦物質、有機物質、容器及紡織品也對本文所述的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物上的至少一有機胺基團具有反應性。
預期本文所述的有機胺基乙烯基矽烷及有機胺基烯丙基矽烷前驅物中的有機胺基錨定基團能提供優於氯乙烯基矽烷、烷氧基乙烯基矽烷、乙烯基二矽氮烷、氯烯丙基矽烷、烷氧基烯丙基矽烷及烯丙基二矽氮烷前驅物與–OH封端的表面之反應,尤其是在低溫及氣相中。舉例來說,在特定溫度下用三乙氧基乙烯基矽烷處理基材可使該基材表面幾乎沒有或沒有被乙烯基官能化,而在相同溫度下用有機胺基乙烯基矽烷處理該基材可提供高出許多的官能化程度。類似地,在特定溫度下用三乙氧基烯丙基矽烷處理基材可使該基材表面幾乎沒有或沒有被烯丙基官能化,而在相同溫度下用有機胺基烯丙基矽烷處理該基材可提供高出許多的官能化程度。這使得具有式I及II的有機胺基乙烯基矽烷及有機胺基烯丙基矽烷有利於作為用於除隨後沉積鍺膜之外的目的之表面改質劑。可受益於表面乙烯基及/或烯丙基的高飽和度的當前製程之實例包括,但不限於,(a)將諸如觸媒、離子交換官能基、吸附劑或金屬清除劑(metal scavenger)的物種固定於固體載體上;(b)提高基材的疏水性;(c)改變用於顯示應用的基材的光學性質或折射率;及/或(d)提供在後續塗層的UV/熱退火之後附著力更好的交聯位點。
某些前驅物可能具有太高的沸點而無法被汽化並輸送到該反應器,無法採膜的方式沉積於基材上,因此較佳為選擇較小的有機胺基及較小的R基團以提供具有250℃或更低的沸點,較佳地200℃或更低的沸點之前驅物。具有二或更多有機胺基會大幅提高沸點;具有較高相對沸點的前驅物需要在指定真空度之下將輸送容器及管路加熱至該前驅物的沸點或更高以防止在該容器、管路或兩者中冷凝或形成顆粒。關於安定性,當其他前驅物降解時可能生成甲矽烷(SiH
4)或乙矽烷(Si
2H
6)。甲矽烷於室溫下具有自燃性或其能自發性地燃燒而出現安全和處理上的問題。再者,甲矽烷或乙矽烷及其他副產物的形成使該前驅物的純度降低而且就可靠性半導體製造而言小到1至2%的化學純度變化可能就被視為不能接受。在某些具體實例中,儲存6個月或更久,或1年或更久的時間之後本文所述的具有式I及/或II的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物包含2重量%或更少,或1重量%或更少,或0.5重量%或更少的雜質(例如游離有機胺、醇、氯矽烷、鹵化物或較高分子量的歧化產物(disproportionation product)),那表示具有貯藏安定性。某些具有Si-H基團的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物(式I及/或II中的R
3和R
4中的至少其一為氫)可能易於經由通過分子間氫矽烷化反應(intermolecular hydrosilylation reaction)聚合而降解。也就是說,若式I及/或II中的R
1至R
4基團的大小不能提供足夠的空間保護,則一分子的Si-H基團與另一分子的乙烯基及/或烯丙基之間可能發生反應。此氫矽烷化反應可在儲存條件之下或在純化(例如,蒸餾)期間或在沉積製程期間緩慢或自發地發生,並且可被痕量雜質催化。因此,重要的是去除該有機胺基乙烯基矽烷前驅物中盡可能多地的雜質,這些雜質可能用作氫矽烷化/聚合觸媒。另外,必需仔細選擇R
1至R
4基團以允許該有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷在所需條件之下與該基材表面輕鬆反應,同時保持該前驅物的固有安定性。
在某些較佳具體實例中,式I及/或II中的R
3及R
4皆為有機胺基基團。在其他較佳具體實例中,式I及/或II中的R
3及R
4皆為甲基。在其他較佳具體實例中,式I及/或式II中的R
1-4皆為甲基。在其他較佳具體實例中,式I及/或II中的R
3及R
4皆為乙烯基。在其他較佳具體實例中,式I及/或II中的R
3及R
4皆為烯丙基。在其他較佳具體實例中,在式I中R
3為有機胺基,並且R
4為乙烯基。在其他較佳具體實例中,在式II中R
3為有機胺基,並且R
4為烯丙基。在其他較佳具體實例中,在式I中R
3為甲基並且R
4為乙烯基。在其他較佳具體實例中,在式II中R
3為甲基並且R
4為烯丙基。
在某些具體實例中,例如使用ALD、類ALD、PEALD或CCVD沉積方法沉積氧化矽或氮化矽或其他含矽膜時,本文所述的有機胺基乙烯基矽烷及有機胺基烯丙基矽烷前驅物能於相對較低的沉積溫度下沉積高密度材料,例如,1000°C或更低、800°C或更低、700°C或更低、500°C或更低、或400°C或更低、300°C或更低、200 °C或更低、100°C或更低、或50°C或更低。
在一具體實例中,本文描述的是一種用於形成含矽膜的組合物,其包含:本文所述的具有式I的有機胺基乙烯基矽烷及/或具有式II的有機胺基烯丙基矽烷及溶劑。
不欲受任何特定理論的束縛,據信與現有的矽前驅物例如TEOS、BDEAS、SiCl
4相比,本文所述的組合物可提供一或更多優點。這些優點包括:該有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷在半導體製程中更好的利用、長期儲存安定性更好、閃蒸更乾淨的汽化及/或整體更穩定的直接液體注入(DLI)化學氣相沉積製程,其允許沉積更高品質的含矽膜,再者其允許更優異的後續鍺膜沉積。該組合物中有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷的重量百分比可為1至99%,其餘為溶劑,其中該溶劑不會與該有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷反應,並且具有與該有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷相似的沸點。對於後者,該組合物中有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷與溶劑的沸點之差為40℃或更低,更佳地20℃或更低,或10℃或更低。
在一些具體實例中,有利的是使用本發明所述的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物沉積含矽膜,例如,但不限於,矽、碳化矽、氮化矽、碳摻雜的氮化矽、氧化矽、氧氮化矽、碳摻雜的氧氮化矽及碳摻雜的氧化矽,前提是金屬膜例如鍺膜隨後要沉積到該含矽膜上。不欲受特定理論的束縛,據信當該含矽膜沉積製程的最後一步為該有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物暴露時,所得含矽膜將更容易形成均勻的鍺種子層,從而於其後平滑的保形鍺膜的生長。在一些情況下,也可使用先前技藝中已知的各種其他矽前驅物及沈積方法達成本文所述的含矽膜的整體組成、物理性質及電氣性質。然而,這些膜在沉積還原或金屬鍺膜之前仍需要用本文所述的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物進行官能化,以使那些鍺膜具有相同的高品質。因此很清楚的是如何使用單一矽前驅物例如本文所述的有機胺基乙烯基矽烷或有機胺基烯丙基矽烷來進行含矽膜的沉積以及該膜用於後續鍺膜生長的乙烯基及/或烯丙基官能化,使用兩種不同的矽前驅物將更有利。
在某些具體實例中,式I及/或II中的取代基R
1及R
2可連接在一起形成一環結構。熟知此領域的習知技藝者將理解,當R
1及R
2連接在一起形成環時,R
1將包括與R
2連接的鍵,反之亦然。在這些具體實例中,該環結構可能是不飽和的例如環狀烷基環或飽和的例如芳環。以類似的方式,式I及/或II中的R
3及R
4可連接在一起形成一環結構。此外,在這些具體實例中,該環結構也可能經取代或未經取代。例示性環狀環基團包括,但不限於,吡咯烷基、2-甲基吡咯烷基、2,5,-二甲基吡咯烷基、六氫吡啶基、2,6-二甲基六氫吡啶基、吡咯基及咪唑基。在其他具體實例中,取代基R
1及R
2並不相連。在又其他具體實例中,R
3及R
4並不相連。
在該式及整個說明書中,該措辭“烷基”表示具有1至10或1至6個碳原子的線性或分支官能基。例示性烷基包括,但不限於,甲基、乙基、丙基、異丙基、丁基、異丁基、第二丁基、第三丁基、戊基、異戊基、第三戊基、己基、異己基及新己基。在某些具體實例中,該烷基可具有連接到其上之一或更多官能基例如,但不限於,烷氧基、二烷基胺基或其組合。在其他具體實例中,該烷基沒有連接到其上之一或更多官能基。
在該式及整個說明書中,該措辭“環狀烷基”表示具有3至10或4至10個碳原子或5至10個碳原子的環狀官能基。例示性環狀烷基包括,但不限於,環丁基、環戊基、環己基及環辛基。
在該式及整個說明書中,該措辭“芳基”表示具有5至12個碳原子或6至10個碳原子的芳族環狀官能基。例示性芳基包括,但不限於,苯基、苯甲基、氯苯甲基、甲苯基及鄰-二甲苯基。
在該式及整個說明書中,該措辭“烯基”表示具有一或更多碳-碳雙鍵並且具有3至10或3至6或3至4個碳原子的基團。例示性烯基包括,但不限於,乙烯基及烯丙基。
在該式及整個說明書中,該措辭“炔基”表示具有一或更多碳-碳叁鍵並且具有3至10或3至6或3至4個碳原子的基團。
在該式及整個說明書中,該措辭“有機胺基”表示具有至少一連接到氮原子的烷基或烴基並且具有1至10或2至6或2至4個碳原子的基團。例示性有機胺基包括,但不限於,甲基胺基、乙基胺基、正丙基胺、異丙基胺基、正丁基胺基、異丁基胺基、第二丁基胺基、第三丁基胺基、環戊基胺基、環己基胺基、苯基胺基、二甲基胺基、N-乙基甲基胺基、二乙基胺基、二異丙基胺基。
在該式及整個說明書中,該措辭“二烷基胺基”表示具有兩個連接到氮原子的烷基的基團,其中各烷基具有,舉例來說,1至10、2至6或2到4個碳原子。例示性二烷基胺基包括,但不限於,二甲基胺基、二乙基胺基、乙基甲基胺基、二正丙基胺、二異丙基胺基、二正丁基胺基、二異丁基胺基、二第二丁基胺基、二第三丁基胺基。
在某些具體實例中,式I及II中的烷基、烯基、炔基或芳基中的一或多者可為經取代或有一或更多原子或原子團被取代換掉,舉例來說,氫原子。例示性取代基包括,但不限於,氧、硫、鹵素原子(例如,F、Cl、I或Br)、氮及磷。
在某些具體實例中,該至少一具有式I的有機胺基乙烯基矽烷前驅物及/或該至少一具有式II的有機胺基烯丙基矽烷前驅物具有一或更多包含氧或氮原子的取代基。
據信本文所述的式I及II前驅物的獨特結構允許含矽膜的沉積及/或固體基材的表面官能化在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
oC或或更低或25
oC或或更低的溫度下進行。
表1列出根據式I的具有連接到至少一矽原子的至少一乙烯基及至少一有機胺基錨定基團之矽前驅物的實例。
表1. 例示性有機胺基乙烯基矽烷前驅物
表2列出根據式II的具有連接到至少一矽原子的至少一烯丙基及至少一有機胺基錨定基團之矽前驅物的實例。
表2. 例示性有機胺基烯丙基矽烷前驅物
叁(甲基胺基)乙烯基矽烷 | 叁(乙基胺基)乙烯基矽烷 |
叁(正丙基胺基)乙烯基矽烷 | 叁(異丙基胺基)乙烯基矽烷 |
叁(第二丁基胺基)乙烯基矽烷 | 叁(第三丁基胺基)乙烯基矽烷 |
叁(二甲基胺基)乙烯基矽烷 | 叁(N-乙基甲基胺基)乙烯基矽烷 |
叁(二乙基胺基)乙烯基矽烷 | 叁(N-甲基環己基胺基)乙烯基矽烷 |
叁(N-甲基苯基胺基)乙烯基矽烷 | 三吡咯烷基乙烯基矽烷 |
叁(六氫吡啶基)乙烯基矽烷 | 三吡咯基乙烯基矽烷 |
雙(甲基胺基)甲基乙烯基矽烷 | 雙(乙基胺基)甲基乙烯基矽烷 |
雙(正丙基胺基)甲基乙烯基矽烷 | 雙(異丙基胺基)甲基乙烯基矽烷 |
雙(第二丁基胺基)甲基乙烯基矽烷 | 雙(第三丁基胺基)甲基乙烯基矽烷 |
雙(二甲基胺基)甲基乙烯基矽烷 | 雙(N-乙基甲基胺基)甲基乙烯基矽烷 |
雙(二乙基胺基)甲基乙烯基矽烷 | 雙(N-甲基環己基胺基)甲基乙烯基矽烷 |
雙(N-甲基苯基胺基)甲基乙烯基矽烷 | 二吡咯烷基甲基乙烯基矽烷 |
雙(六氫吡啶基)甲基乙烯基矽烷 | 二吡咯基甲基乙烯基矽烷 |
雙(甲基胺基)二乙烯基矽烷 | 雙(乙基胺基)二乙烯基矽烷 |
雙(正丙基胺基)二乙烯基矽烷 | 雙(異丙基胺基)二乙烯基矽烷 |
雙(第二丁基胺基)二乙烯基矽烷 | 雙(第三丁基胺基)二乙烯基矽烷 |
雙(二甲基胺基)二乙烯基矽烷 | 雙(N-乙基甲基胺基)二乙烯基矽烷 |
雙(二乙基胺基)二乙烯基矽烷 | 雙(N-甲基環己基胺基)二乙烯基矽烷 |
雙(N-甲基苯基胺基)二乙烯基矽烷 | 二吡咯烷基二乙烯基矽烷 |
雙(六氫吡啶基)二乙烯基矽烷 | 二吡咯基二乙烯基矽烷 |
(甲基胺基)二甲基乙烯基矽烷 | (乙基胺基)二甲基乙烯基矽烷 |
(正丙基胺基)二甲基乙烯基矽烷 | (異丙基胺基)二甲基乙烯基矽烷 |
(第二丁基胺基)二甲基乙烯基矽烷 | (第三丁基胺基)二甲基乙烯基矽烷 |
(二甲基胺基)二甲基乙烯基矽烷 | (N-乙基甲基胺基)二甲基乙烯基矽烷 |
(二乙基胺基)二甲基乙烯基矽烷 | (N-甲基環己基胺基)二甲基乙烯基矽烷 |
(N-甲基苯基胺基)二甲基乙烯基矽烷 | 吡咯烷基二甲基乙烯基矽烷 |
六氫吡啶基二甲基乙烯基矽烷 | 吡咯基二甲基乙烯基矽烷 |
(甲基胺基)甲基二乙烯基矽烷 | (乙基胺基)甲基二乙烯基矽烷 |
(正丙基胺基)甲基二乙烯基矽烷 | (異丙基胺基)甲基二乙烯基矽烷 |
(第二丁基胺基)甲基二乙烯基矽烷 | (第三丁基胺基)甲基二乙烯基矽烷 |
(二甲基胺基)甲基二乙烯基矽烷 | (N-乙基甲基胺基)甲基二乙烯基矽烷 |
(二乙基胺基)甲基二乙烯基矽烷 | (N-甲基環己基胺基)甲基二乙烯基矽烷 |
(N-甲基苯基胺基)甲基二乙烯基矽烷 | 吡咯烷基甲基二乙烯基矽烷 |
六氫吡啶基甲基二乙烯基矽烷 | 吡咯基甲基二乙烯基矽烷 |
(甲基胺基)三乙烯基矽烷 | (乙基胺基)三乙烯基矽烷 |
(正丙基胺基)三乙烯基矽烷 | (異丙基胺基)三乙烯基矽烷 |
(第二丁基胺基)三乙烯基矽烷 | (第三丁基胺基)三乙烯基矽烷 |
(二甲基胺基)三乙烯基矽烷 | (N-乙基甲基胺基)三乙烯基矽烷 |
(二乙基胺基)三乙烯基矽烷 | (N-甲基環己基胺基)三乙烯基矽烷 |
(N-甲基苯基胺基)甲基二乙烯基矽烷 | 吡咯烷基甲基三乙烯基矽烷 |
六氫吡啶基三乙烯基矽烷 | 吡咯基三乙烯基矽烷 |
叁(甲基胺基)烯丙基矽烷 | 叁(乙基胺基)烯丙基矽烷 |
叁(正丙基胺基)烯丙基矽烷 | 叁(異丙基胺基)烯丙基矽烷 |
叁(第二丁基胺基)烯丙基矽烷 | 叁(第三丁基胺基)烯丙基矽烷 |
叁(二甲基胺基)烯丙基矽烷 | 叁(N-乙基甲基胺基)烯丙基矽烷 |
叁(二乙基胺基)烯丙基矽烷 | 叁(N-甲基環己基胺基)烯丙基矽烷 |
叁(N-甲基苯基胺基)烯丙基矽烷 | 三吡咯烷基烯丙基矽烷 |
叁(六氫吡啶基)烯丙基矽烷 | 三吡咯基烯丙基矽烷 |
雙(甲基胺基)甲基烯丙基矽烷 | 雙(乙基胺基)甲基烯丙基矽烷 |
雙(正丙基胺基)甲基烯丙基矽烷 | 雙(異丙基胺基)甲基烯丙基矽烷 |
雙(第二丁基胺基)甲基烯丙基矽烷 | 雙(第三丁基胺基)甲基烯丙基矽烷 |
雙(二甲基胺基)甲基烯丙基矽烷 | 雙(N-乙基甲基胺基)甲基烯丙基矽烷 |
雙(二乙基胺基)甲基烯丙基矽烷 | 雙(N-甲基環己基胺基)甲基烯丙基矽烷 |
雙(N-甲基苯基胺基)甲基烯丙基矽烷 | 二吡咯烷基甲基烯丙基矽烷 |
雙(六氫吡啶基)甲基烯丙基矽烷 | 二吡咯基甲基烯丙基矽烷 |
雙(甲基胺基)二烯丙基矽烷 | 雙(乙基胺基)二烯丙基矽烷 |
雙(正丙基胺基)二烯丙基矽烷 | 雙(異丙基胺基)二烯丙基矽烷 |
雙(第二丁基胺基)二烯丙基矽烷 | 雙(第三丁基胺基)二烯丙基矽烷 |
雙(二甲基胺基)二烯丙基矽烷 | 雙(N-乙基甲基胺基)二烯丙基矽烷 |
雙(二乙基胺基)二烯丙基矽烷 | 雙(N-甲基環己基胺基)二烯丙基矽烷 |
雙(N-甲基苯基胺基)二烯丙基矽烷 | 二吡咯烷基二烯丙基矽烷 |
雙(六氫吡啶基)二烯丙基矽烷 | 二吡咯基二烯丙基矽烷 |
(甲基胺基)二甲基烯丙基矽烷 | (乙基胺基)二甲基烯丙基矽烷 |
(正丙基胺基)二甲基烯丙基矽烷 | (異丙基胺基)二甲基烯丙基矽烷 |
(第二丁基胺基)二甲基烯丙基矽烷 | (第三丁基胺基)二甲基烯丙基矽烷 |
(二甲基胺基)二甲基烯丙基矽烷 | (N-乙基甲基胺基)二甲基烯丙基矽烷 |
(二乙基胺基)二甲基烯丙基矽烷 | (N-甲基環己基胺基)二甲基烯丙基矽烷 |
(N-甲基苯基胺基)二甲基烯丙基矽烷 | 吡咯烷基二甲基烯丙基矽烷 |
六氫吡啶基二甲基烯丙基矽烷 | 吡咯基二甲基烯丙基矽烷 |
(甲基胺基)甲基二烯丙基矽烷 | (乙基胺基)甲基二烯丙基矽烷 |
(正丙基胺基)甲基二烯丙基矽烷 | (異丙基胺基)甲基二烯丙基矽烷 |
(第二丁基胺基)甲基二烯丙基矽烷 | (第三丁基胺基)甲基二烯丙基矽烷 |
(二甲基胺基)甲基二烯丙基矽烷 | (N-乙基甲基胺基)甲基二烯丙基矽烷 |
(二乙基胺基)甲基二烯丙基矽烷 | (N-甲基環己基胺基)甲基二烯丙基矽烷 |
(N-甲基苯基胺基)甲基二烯丙基矽烷 | 吡咯烷基甲基二烯丙基矽烷 |
六氫吡啶基甲基二烯丙基矽烷 | 吡咯基甲基二烯丙基矽烷 |
(甲基胺基)三烯丙基矽烷 | (乙基胺基)三烯丙基矽烷 |
(正丙基胺基)三烯丙基矽烷 | (異丙基胺基)三烯丙基矽烷 |
(第二丁基胺基)三烯丙基矽烷 | (第三丁基胺基)三烯丙基矽烷 |
(二甲基胺基)三烯丙基矽烷 | (N-乙基甲基胺基)三烯丙基矽烷 |
(二乙基胺基)三烯丙基矽烷 | (N-甲基環己基胺基)三烯丙基矽烷 |
(N-甲基苯基胺基)甲基二烯丙基矽烷 | 吡咯烷基甲基三烯丙基矽烷 |
六氫吡啶基三烯丙基矽烷 | 吡咯基三烯丙基矽烷 |
根據本發明的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物及包含根據本發明的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物之組合物較佳為實質上不含有機胺或鹵離子(halide ion)。如本文所用,該措辭“實質上不含” 當其關係到鹵離子(或鹵化物)例如,舉例來說,氯化物和氟化物、溴化物及碘化物時,意指小於5 ppm (以重量計),較佳地小於3 ppm,更佳地小於1 ppm,而且更佳地0 ppm。如本文所用,該措辭“不含”當其關係到鹵離子或其他雜質時意指0ppm。據悉氯化物用作有機胺基乙烯基矽烷及有機胺基烯丙基矽烷的分解觸媒。最終產物中有顯著量的氯化物會造成該有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物降解。該有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷逐漸降解可能直接衝擊到該膜沉積製程或表面官能化製程,使半導體製造廠商難以符合膜的規範。除此之外,該儲存壽命或安定性受到該有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷較高降解速率的負面衝擊,從而使其難以保證1至2年的儲存壽命。因此,該有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷的加速分解帶來了與這些易燃及/或自燃性氣態副產物(有機胺,其包括,但不限於,C
1至C
10有機胺、有機二胺)的形成有關的安全性及性能問題。該具有式I及II的矽前驅物化合物較佳為實質上不含金屬離子例如,Li
+、Na
+、K
+、Mg
2+、Ca
2+、Al
3+、Fe
2+、Fe
2+、Fe
3+、Ni
2+、Cr
3+。如本文所用的,當關係到Li、Na、K、Mg、Ca、Al、Fe、Ni、Cr、貴金屬(例如來自合成時使用的釕或鉑觸媒之揮發性釕或鉑錯合物)時,該措辭“實質上不含”意指藉由ICP-MS或其他用於測量痕量金屬的分析方法測得小於5 ppm (以重量計),較佳地小於3 ppm,更佳地小於1 ppm,並且最佳地0.1 ppm。
用以形成該含矽膜或塗層的方法係沉積製程。用於本文所揭示的方法之適當沉積製程的實例包括,但不限於,循環式CVD (CCVD)、MOCVD (金屬有機CVD)、熱化學氣相沉積、電漿強化化學氣相沉積(“PECVD”)、高密度PECVD、光子輔助CVD、電漿-光子輔助(“PPECVD”)、低溫化學氣相沉積、化學輔助氣相沉積、熱絲化學氣相沉積、液體聚合物前驅物的CVD、由超臨界流體來沉積及低能CVD (LECVD)。在某些具體實例中,該含金屬的膜係經由原子層沉積(ALD)、電漿強化ALD (PEALD)或電漿強化循環式CVD (PECCVD)製程來沉積。如本文所用的,該措辭“化學氣相沉積製程”表示使基材暴露於一或更多揮發性前驅物,該揮發性前驅物於該基材表面上反應及/或分解以產生預期沉積,的任何製程。如本文所用的,該措辭“原子層沉積製程”表示把材料的膜沉積於不同組成的基材上之自限性(例如,各反應周期所沉積的膜材料量恆定)連續表面化學。儘管本文所用的前驅物、試劑及來源有時候可能被描述成“氣態”,但是咸了解該前驅物可能是液態或固態,該前驅物係經由直接汽化、起泡或昇華利用或沒用惰性氣體輸送至該反應器中。在某些情況下,該經汽化的前驅物能通過電漿產生器。在一具體實例中,該含矽膜係利用ALD製程來沉積。在另一具體實例中,該含矽膜係利用CCVD製程來沉積。在另一具體實例中,該含矽膜係利用熱CVD製程來沉積。本文所用的措辭“反應器”包括,但不限於,反應艙或沉積艙。
在某些具體實例中,本文所揭示的方法藉由運用ALD或CCVD方法在引入該反應器以前及/或期間分開該前驅物而避免該前驅物的預反應。關此,用沉積技術例如ALD或CCVD製程來沉積該含矽膜。在一具體實例中,該膜係經由ALD製程,藉由使該基材表面輪流暴露於一或更多含矽前驅物、含氧源、含氮源或其他前驅物或試劑來沉積。膜的生長係藉由表面反應的自限性控制、各前驅物或試劑的脈衝時間長度及沉積溫度來進行。但是,一旦該基材表面飽和了,該膜的生長就會停止。
在某些具體實例中,本文所述的方法另外包含一或更多具有上述式I及/或II的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物以外的一或更多其他含矽前驅物。其他含矽前驅物的實例包括,但不限於,單胺基矽烷(例如,二異丙基胺基矽烷、二第二丁基胺基矽烷、苯基甲基胺基矽烷);有機矽化合物例如三甲矽烷基胺(TSA);單胺基矽烷類(二異丙基胺基矽烷、二第二丁基胺基矽烷、苯基甲基胺基矽烷);矽氧烷類(例如,六甲基二矽氧烷(HMDSO)和二甲基矽氧烷(DMSO)和六氯二矽氧烷(HCDSO));有機矽烷類(例如,甲基矽烷、二甲基矽烷、二乙基矽烷、乙烯基三甲基矽烷、三甲基矽烷、四甲基矽烷、乙基矽烷、二甲矽烷基甲烷、2,4-二矽雜戊烷、1,4-二矽雜丁烷、2,5-二矽雜己烷、2,2-二甲矽烷基丙烷、1,3,5-三矽雜環己烷及這些化合物的氟化衍生物);含苯基的有機矽化合物(例如,二甲基苯基矽烷和二苯基甲基矽烷);含氧的有機矽化合物,例如,二甲基二甲氧基矽烷;1,3,5,7-四甲基環四矽氧烷;1,1,3,3-四甲基二矽氧烷;1,3,5,7-四矽雜-4-側氧基-庚烷;2,4,6,8-四矽雜-3,7-二側氧基-壬烷;2,2-二甲基-2,4,6,8-四矽雜-3,7-二側氧基-壬烷;八甲基環四矽氧烷;[1,3,5,7,9]-五甲基環五矽氧烷;1,3,5,7-四矽雜-2,6-二側氧基-環辛烷;六甲基環三矽氧烷;1,3-二甲基二矽氧烷;1,3,5,7,9-五甲基環五矽氧烷;六甲氧基二矽氧烷及這些化合物的氟化衍生物。
依據該沉積方法,在某些具體實例中,該一或更多含矽前驅物可以預定莫耳體積或約0.1至約1000微莫耳引入該反應器。在各個不同具體實例中,該含矽及/或有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物可經歷預定時間引入該反應器。在某些具體實例中,該時間介於約0.001至約500秒。
在某些具體實例中,利用本文所述的方法沉積旳含矽膜係於氧存在的情形下使用包含氧的含氧源、試劑或包含氧的前驅物形成。含氧源可依照至少一含氧源的形式引進該反應器及/或可附帶地存在於該沉積製程中使用的其他前驅物中。合適的含氧源氣體可包括,舉例來說,水(H
2O) (例如,去離子水、純水及/或蒸餾水)、過氧化氫(H
2O
2)、氧(O
2)、氧電漿、臭氧(O
3)、NO、N
2O、NO
2、一氧化碳(CO)、二氧化碳(CO
2)及其組合。在某些具體實例中,該含氧源包含以介於約1至約2000標準立方釐米(sccm)或約1至約1000 sccm的流速下引入該反應器的含氧源氣體。該含氧源能引入經歷介於約0.1至約100秒的時間。在一特定具體實例中,該含氧源包含具有10°C或更高溫度的水。在藉由ALD或循環式CVD製程沉積該膜的具體實例中,該前驅物脈衝可具有大於0.01秒的脈衝時間,而且該含氧源可具有小於0.01秒的脈衝時間,而該水脈衝持續時間可具有小於0.01秒的脈衝持續時間。在又另一具體實例中,介於該脈衝之間的吹掃持續時間可能小到0秒或連續地脈衝而於其間沒有吹掃。該含氧源或試劑係依照對該矽前驅物小於1:1的比率的分子用量提供,所以至少有一些碳留在原沉積的含矽膜(as deposited silicon-containing film)中。
在某些具體實例中,該含矽膜包含矽及氮。在這些具體實例中,使用本文所述的方法所沉積的含矽膜係於含氮源存在之下形成。含氮源可依照至少一含氮源的形式引入該反應器及/或可能附帶地存在於該沉積製程所用的其他前驅物中。適合的含氮源氣體可包括,舉例來說,氨、肼、單烷基肼、二烷基肼、氮、氮/氫、氨電漿、氮電漿、氮/氫電漿及其混合物。在某些具體實例中,該含氮源包含氨電漿或氫/氮電漿源氣體,其以介於約1至約2000標準立方釐米(sccm)或約1至約1000 sccm的流速引入該反應器。該含氮源可引入介於約0.1至約100秒的時間。在藉由ALD或循環式CVD製程沉積該膜的具體實例中,該前驅物脈衝可具有大於0.01秒的脈衝持續時間,並且該含氮源可具有小於0.01秒的脈衝持續時間,而該水脈衝持續時間可具有小於0.01秒的脈衝持續時間。在又另一具體實例中,該脈衝之間的吹掃持續時間可小到0秒或連續脈衝而中間沒有吹掃。
本文所揭露的沉積方法可能涉及一或更多吹掃氣體。該吹掃氣體,其係用以吹掃掉沒消耗的反應物及/或反應副產物,係不會與該前驅物反應的惰性氣體。例示性吹掃氣體包括,但不限於,氬(Ar)、氮(N
2)、氦(He)、氖、氫(H
2)及其混合物。在某些具體實例中,吹掃氣體例如Ar係於介於約10至約2000 sccm的流速下供入該反應器經歷約0.1至1000秒,藉以吹掃該未反應的材料和可能留在該反應器中的任何副產物。
供應該前驅物、含氧源、該含氮源、及/或其他前驅物、來源氣體及/或試劑的相應步驟可藉由變化其供應時間來進行以改變所得的膜之化學計量組成。
把能量施加於該前驅物、含氧源、含氮源、還原劑、其他前驅物或其組合中的至少其一以引發反應並且將該含矽膜或塗層形成於該基材上。此能量可藉由,但不限於,熱、電漿、脈衝電漿、螺旋電漿、高密度電漿、感應耦合電漿、X-射線、電子束、光子、遠程電漿方法及其組合,來提供。在某些具體實例中,二次射頻頻率源可用以變更該基材表面處的電漿特性。在該沉積涉及電漿的具體實例中,該電漿產生的製程可包含該電漿直接在該反應器中產生的直接電漿產生製程,或者電漿在該反應器外部產生並且供應至該反應器內的遠程電漿產生製程。
該有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物、其他含矽前驅物及/或鍺前驅物可以各種不同方式輸送至該反應艙例如CVD或ALD反應器。在一具體實例中,可利用液體運送系統。在一替代具體實例中,可運用合併液體輸送及閃蒸(flash vaporization)處理單元,例如,舉例來說,明尼蘇達州,休爾瓦的MSP股份有限公司所製造的渦輪汽化器,使低揮發性材料能夠以容積測流方式輸送,導致可再現的輸送及沉積而不會使該前驅物熱分解。在液體運送配方中,本文所述的前驅物可以純液體形式輸送,或者,可以溶劑配方或其組合物方式運用。因此,在某些具體實例中,該前驅物配方可包括可能想要的適合特性和在特定最終用途應用中有優點的溶劑組分以將膜形成於基材上。
對於包含溶劑及本文所述的具有式I及/或II的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物之組合物中使用該具有式I及/或II的前驅物的那些具體實例,所挑選的溶劑或其混合物不會與該有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷反應。在該組合物中以重量百分比計的溶劑量介於0.5重量%至99.5重量%或10重量%至75重量%。在各個不同具體實例中,該溶劑具有類似於該具有式I及/或II的前驅物的沸點之沸點(b.p.)或介於該溶劑的沸點與該具有式I及/或II的前驅物的沸點之間的差異係40°C或更低,30°C或更低,或20°C或更低,或10°C。或者,該沸點之間的差異介於以下端點中之任一或更多者:0、10、20、30或40°C。沸點差異適合範圍的實例包括,但不限於,0至40°C、20°至30°C或10°至30°C。該組合物中的適合溶劑的實例包括,但不限於,醚(例如1,4-二噁烷、二丁基醚)、三級胺(例如吡啶、1-甲基六氫吡啶、1-乙基六氫吡啶、N,N'-二甲基六氫吡嗪、N,N,N',N'-四甲基伸乙二胺)、腈化物(例如苯甲腈)、烷基烴(例如辛烷、壬烷、十二烷、乙基環己烷)、芳烴(例如甲苯、均三甲苯(mesitylene))、三級胺基醚(例如雙(2-二甲基胺基乙基)醚)或其混合物。
在另一具體實例中,本文描述的是用於沉積包含一或更多具有式I或II的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物的含矽膜之容器。在一特定具體實例中,該容器包含至少一裝配適當閥和配件的可加壓容器(較佳由不銹鋼製成)以使一或更多前驅物能運送至該反應器供CVD或ALD製程用。在各個不同具體實例中,該具有式I及/或II的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物係供入包含不銹鋼的可加壓容器中,而且該前驅物的純度係98重量%或更高或99.5%或更高,其適用於大多數半導體應用。在某些具體實例中,這樣的容器也可具有用於混合該前驅物與必要的話還有一或更多其他前驅物的裝置。在各個不同具體實例中,該容器的內容物能與另一前驅物預先混合。或者,該有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物及/或其他前驅物能保持於獨立容器或具有分離裝置的單一容器中,該分離裝置係用於使該有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物與其他前驅物在儲存的期間保持分開。
在本文所述的方法之一具體實例中,可採用循環式沉積製程例如CCVD、ALD或PEALD,其中使用的是至少一選自具有本文所述式的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物之含矽前驅物及視需要地含氮源例如,舉例來說,氨、肼、單烷基肼、二烷基肼、氮、氮/氫、氨電漿、氮電漿、氮/氫電漿。
在某些具體實例中,將從該前驅物藥罐連到該反應艙的氣體管路根據該製程要求加熱到一或更多溫度,並且將該具有本文所述式I及/或II的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物的容器保持於一或更多的起泡溫度。在其他具體實例中,將包含該至少一具有本文所述式的含矽前驅物的溶液注入保持於一或更多溫度下的汽化器以進行直接液體注入(direct liquid injection)。
氬及/或其他氣體流皆可用作載氣以於該前驅物脈衝期間協助將該至少一有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物的蒸氣輸送至該反應艙。在某些具體實例中,該反應艙製程壓力係約10托耳或更低。在另一具體實例中,該反應艙製程壓力係5托耳或更低。
對於多組分含矽膜,可將其他前驅物例如含矽前驅物、含氮前驅物、還原劑或其他試劑輪流引入該反應艙。
在本文所述的方法之一具體實例中,使用熱ALD製程及包含氫的電漿沉積該氧化矽或碳含量介於0原子%至20原子%之碳摻雜的氧化矽膜以改善膜性質。在此具體實例中,該方法包含:
a. 將一或更多包含表面特徵的基材放入反應器中,並且將該反應器加熱至介於環境溫度至約550℃之一或更多溫度,並且視需要地將該反應器保持於100托耳或更低的壓力下;
b. 將至少一式I及/或II所示的有機胺基乙烯基矽烷前驅物及/或有機胺基烯丙基矽烷前驅物引入該反應器中,該有機胺基乙烯基矽烷前驅物及/或有機胺基烯丙基矽烷前驅物包含連接到至少一矽原子的至少一乙烯基及/或烯丙基及至少一有機胺基錨定基團;
c. 用惰性氣體吹掃該反應器,從而除去未反應的矽前驅物,並且形成包含該吹掃氣體及矽前驅物的組合物;
d. 將含氧源提供到該反應器中以與該表面反應形成含矽和氧的膜;
e. 用惰性氣體吹掃以除去反應副產物;
f. 重複步驟b至e以提供所需厚度之氧化矽或碳摻雜的氧化矽;
在各個不同具體實例中,該UV曝光步驟可在膜沉積期間或一旦完成沉積之後就進行。在另一具體實例中,可使用如本文所述的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷,以上概述的相同步驟沉積含矽和氮的膜例如氮化矽或碳氮化矽,不同之處在於使用含氮源代替含氧源。
在一具體實例中,該基材包括至少一特徵,其中該特徵包含具有1:9或更高的深寬比及/或180 nm或更小的開口之圖案溝槽。
在用電漿處理該膜的具體實例中,該電漿源係選自由氫電漿、包含氫和氦的電漿及包含氫和氬的電漿所組成的群組。氫電漿使膜的介電常數降低,並且增強對後續電漿灰化製程的抗損傷性(damage resistance),同時仍然使主體中的碳含量幾乎保持不變。
在整個說明書中,該措辭“ ALD或類ALD”表示包括,但不限於,以下製程的製程:a) 將包括矽前驅物及反應性氣體的各自反應物依次引入反應器例如單晶圓ALD反應器、半批次ALD反應器或批式爐ALD反應器;b) 藉由將該基材移動或旋轉至該反應器的不同區段而使包括矽前驅物及反應性氣體的各自反應物暴露於基材,並且藉由惰性氣幕(即空間ALD反應器或輥對輥ALD反應器)將各區段分開。
在整個說明書中,該措辭“灰化”表示在半導體製程中使用包含氧源的電漿(例如O
2/惰性氣體電漿、O
2電漿、CO
2電漿、CO電漿、H
2/O
2電漿或其組合)移除光阻劑或碳硬罩(carbon hard mask)的製程。
在整個說明書中,該措辭“抗損傷性”表示在氧灰化製程之後的膜性質。將良好或高的抗損傷性定義為以下氧灰化之後的膜性質:膜介電常數低於4.5;主體中的碳含量(在膜深超過50Å處)在灰化之前的5原子%之內;藉由膜表面附近(小於50Å深度)與膜主體(大於50Å深度)之間的稀HF蝕刻速率差異觀察到少於50Å的膜受損。
在某些具體實例中,本文所述的具有式I及/或II的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物也能用作含金屬膜,例如但不限於,金屬氧化物膜或金屬氮化物膜,的摻雜劑。在這些具體實例中,該含金屬膜係利用ALD或CVD製程例如本文所述的那些製程使用金屬烷氧化物、金屬醯胺或揮發性有機金屬前驅物來沉積。可配合本文所揭示的方法一起使用的適當金屬烷氧化物前驅物的實例包括,但不限於,3至6族金屬烷氧化物、兼具經烷氧基和烷基取代的環戊二烯基配位子的3至6族金屬錯合物、兼具經烷氧基和烷基取代的吡咯基配位子的3至6族金屬錯合物、兼具經烷氧基和二酮酸根配位子的3至6族金屬錯合物;兼具經烷氧基和酮酯配位子的3至6族金屬錯合物。可配合本文所揭示的方法一起使用之適當金屬醯胺前驅物的實例包括,但不限於,肆(二甲基胺基)鋯(TDMAZ)、肆(二乙基胺基)鋯(TDEAZ)、肆(乙基甲基胺基)鋯(TEMAZ)、肆(二甲基胺基)鉿(TDMAH)、肆(二乙基胺基)鉿(TDEAH)及肆(乙基甲基胺基)鉿(TEMAH)、肆(二甲基胺基)鈦(TDMAT)、肆(二乙基胺基)鈦(TDEAT)、肆(乙基甲基胺基)鈦(TEMAT)、第三丁基亞胺基叁(二乙基胺基)鉭(TBTDET)、第三丁基亞胺基叁(二甲基胺基)鉭(TBTDMT)、第三丁基亞胺基叁(乙基甲基胺基)鉭(TBTEMT)、乙基亞胺基叁(二乙基胺基)鉭(EITDET)、乙基亞胺基叁(二甲基胺基)鉭(EITDMT)、乙基亞胺基叁(乙基甲基胺基)鉭(EITEMT)、第三戊基亞胺基叁(二甲基胺基)鉭(TAIMAT)、第三戊基亞胺基叁(二乙基胺基)鉭、伍(二甲基胺基)鉭、第三戊基亞胺基叁(乙基甲基胺基)鉭、雙(第三丁基亞胺基)雙(二甲基胺基)鎢(BTBMW)、雙(第三丁基亞胺基)雙(二乙基胺基)鎢、雙(第三丁基亞胺基)雙(乙基甲基胺基)鎢及其組合。可配合本文所揭示的方法一起使用之適當有機金屬前驅物的實例包括,但不限於,3族金屬環戊二烯基或烷基環戊二烯基。本文中例示性的3至6族金屬包括,但不限於,Y、La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Er、Yb、Lu、Ti、Hf、Zr、V、Nb、Ta、Cr、Mo及W。
在某些具體實例中,所得的含矽膜或塗層能夠暴露於沉積後處理例如,但不限於,電漿處理、化學處理、紫外線曝光、電子束曝光及/或其他處理以影響該膜的一或更多性質。
在某些具體實例中,本文所述的含矽膜具有6或更低的介電常數。在各個不同具體實例中,該膜可具有約5或更低,或約4或更低,或約3.5或更低的介電常數。然而,能想像具有其他介電常數(例如,更高或更低)的膜能依據該膜的預期最終用途形成。使用本文所述的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物及製程所形成的含矽膜之實例具有此配方Si
xO
yC
zN
vH
w,其中藉由舉例來說XPS或其他方法測定時,Si介於約10%至約40%;O介於約0%至約65%;C介於約0%至約75%或約0%至約50%;N介於約0%至約75%或約0%至50%;而且H介於約0%至約50%原子百分比重量%,其中x+y+z+v+w = 100個原子重量百分比。使用本文中所述的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物及製程形成的含矽膜之另一實例係碳氮化矽,其中該碳含量藉由XPS測量為1原子%至80原子%。然而,使用本文所述的有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物及製程形成的含矽膜的另一實例係非晶形矽,其中氮及碳含量的總和藉由XPS測得為< 10原子%,較佳地< 5原子%,最佳地< 1原子%。
如先前提及的,本文所述的方法可用以將含矽膜沉積於基材的至少一部分上。適合基材的實例包括但不限於,矽、鍺摻雜的矽、鍺、SiO
2、Si
3N
4、OSG、FSG、碳化矽、氫化的碳化矽、氮化矽、氫化的氮化矽、碳氮化矽、氫化的碳氮化矽、硼氮化物、抗反射塗層、光阻劑、撓性基材、有機聚合物、多孔性有機和無機材料、金屬例如銅和鋁及擴散阻絕層例如但不限於TiN、Ti(C)N、TaN、Ta(C)N、Ta、W或WN。該膜與多變的後續處理步驟例如,舉例來說,化學機械平坦化(CMP)和各向異性蝕刻製程相容。
所沉積的膜具有多種應用,其包括,但不限於,電腦晶片、光學裝置、磁性資料儲存、於支撐材料或基材上的塗層、微電機系統(MEMS)、奈米電機系統、薄膜電晶體(TFT)、發光二極體(LED)、有機發光二極體(OLED)、IGZO及液晶顯示器(LCD)。
本文所述的方法提供包括鍺、矽、碳化矽、氮化矽、碳摻雜氮化矽、氧化矽、氧氮化矽、碳摻雜氧氮化矽、碳摻雜氧化矽的高品質膜。該措辭“高質量”意指顯現以下一或更多特性的膜:約 2.1 g/cc或更高、2.2 g/cc或更高、2.25 g/cc或更高的密度;在HF對水1:100的稀HF (0.5重量% dHF)酸的溶液中測得2.5 Å/s或更低、2.0 Å/s或更低、1.5 Å/s或更低、1.0 Å/s或更低、0.5 Å/s或更低、0.1 Å/s或更低、0.05 Å/s或更小,0.01 Å/s或更小的濕蝕刻速率;在達於6 MV/cm下約1 e-8 A/cm2或更小的漏電流;藉由SIMS測得的氫雜質約 5 e20 at/cc或更少;非常低的不均勻性、低表面粗糙度及其組合。關於該蝕刻速率,熱生長的氧化矽膜在0.5重量% HF中0.5 Å/s的蝕刻速率。
在某些具體實例中,一或更多具有本文所述式I和II的矽前驅物可用以形成固體且非多孔性或實質上無孔之含矽和氧的膜。
下列實施例舉例說明本文所述的製備有機胺基乙烯基矽烷及/或有機胺基烯丙基矽烷前驅物,沉積含矽膜,生成乙烯基官能化的及/或烯丙基官能化的表面,及生產鍺種子層之方法,並且無意以任何方式限制彼。
實施例
實施例1. 叁(乙基胺基)乙烯基矽烷的合成
在氮氣保護之下,將THF中乙基胺的溶液(800 mL,2.0 M,1.60 mol)經由套管加到配有機械攪拌器和回流冷凝器的3升三頸圓底燒瓶中之己烷(1 升)中三乙基胺(175 g,1.73 mol)的溶液。將合併的溶液冷卻至-20 °C並且攪拌。在-20 °C 下,在 2 小時內向此混合物逐滴添加己烷(80 g)中三氯乙烯基矽烷(80.0 g,0.495 mol)的溶液。使所得的白色漿液暖化至室溫並且再攪拌2小時。藉由玻璃熔料(glass frit)過濾除去白色固體,並且在室溫下減壓(20托耳)除去溶劑。所得的濃縮粗液藉由真空蒸餾(1托耳/45℃)純化,得到55.4 g的叁(乙基胺基)乙烯基矽烷。沸點由DSC測定為199℃。GC-MS分析顯示以下質量峰:m/z = 187 (M+)、172 (M-15)、160、143、129、118、100、86、72、57、44。
實施例2. 用叁(乙基胺基)乙烯基矽烷處理矽膠
在氮氣保護之下,將0.5 g的矽膠(Davasil
TM等級 645,60至100目,150 Å)在 5 mL的THF中參(乙基胺基)乙烯基矽烷的50重量%溶液中在80 °C下攪拌2小時。傾析液相,在真空乾燥之前用熱THF沖洗固體數次。未經處理和經處理的矽膠皆藉由FTIR光譜以KBr壓片的方式分析。與該單離的表面Si-OH基團對應之未經處理的矽膠之FTIR 光譜中的3741 cm
-1處的尖峰在該經處理的矽膠之FTIR光譜中並未檢測到。該經處理的矽膠在FTIR光譜中顯示出以下新峰: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)。這顯示該矽膠的表面在用叁(乙基胺基)乙烯基矽烷處理之後在較低溫度下和較短時間內被乙烯基和乙基胺基官能化。
實施例3. 三乙氧基乙烯基矽烷與第三丁基鍺烷的反應
將約1 mL的三乙氧基乙烯基矽烷和第三丁基鍺烷的1:1莫耳混合物密封於配備內部壓力傳感器和熱電耦的9.5 mL不銹鋼槽中。將樣品加熱至250 °C並且保持等溫1小時。未檢測到顯著的壓力升高,但是在約212 °C的溫度上升時觀察到溫和的放熱性熱事件。當該混合物冷卻回室溫時,藉由GC和GC-MS對其進行分析。1,1-加成和1,2-加成鍺氫化產物1-三乙氧基矽烷基-1-(第三丁基鍺烷基)乙烷(次要)及1-三乙氧基矽烷基-2-(第三丁基鍺烷基)乙烷(主要)分別根據以下質量峰進行檢測:(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。這證實在沒有觸媒的情況下,前驅物中的Ge-H鍵像是鍺烷、二鍺烷及第三丁基鍺烷能於200與250 °C之間與Si-乙烯基反應。這支持首先藉由用乙烯基將該表面官能化,然後與鍺烷或二鍺烷反應以在鍺CVD生長之前建立一Ge-H封端的表面而在SiO
2基材上建立鍺種子層的方案。
儘管本發明已經引用某些較佳具體實例進行了描述,但是熟知該領域之習知技藝者可以理解,可完成各種變化並且用等效物取代其元素而不會悖離本發明的範疇。除此之外,可完成許多修飾以使特定情況或材料適應本發明的教導而不會悖離其基本範疇。因此,預期本發明並不限於特定具體實例,而是本發明將包括落於後附發明申請專利範圍以內的所有具體實例。
圖1係描繪整體架構的流程圖,其中使用本文揭示的具有式I (或式II)的有機胺基乙烯基矽烷前驅物以(a)用乙烯基將基材表面官能化,使其適用於(b)經由與包含至少一Ge-H鍵的鍺前驅物的鍺氫化反應形成鍺種子層,允許(c)隨後使用至少一ALD或CVD Ge前驅物在該種子層頂部生長平滑均勻的鍺膜。
Claims (9)
- 一種藉由沉積製程將含鍺膜形成於基材的至少一表面上之方法,該方法包含:將該基材的至少一表面提供至反應艙中,該基材具有暴露的表面羥基;將至少一下式I所示的有機胺基乙烯基矽烷前驅物或至少一下式II所示的有機胺基烯丙基矽烷前驅物引入該反應艙中,該有機胺基乙烯基矽烷前驅物包含連接到至少一矽原子的至少一乙烯基及至少一有機胺基錨定基團,該有機胺基烯丙基矽烷前驅物包含連接到至少一矽原子的至少一烯丙基及至少一有機胺基錨定基團:
- 如請求項1之方法,其中該至少一有機胺基乙烯基矽烷前驅物包含至少一選自由以下所組成的群組之化合物:叁(甲基胺基)乙烯基矽烷、叁(乙基胺基)乙烯基矽烷、叁(正丙基胺基)乙烯基矽烷、叁(異丙基胺基)乙烯基矽烷、叁(第二丁基胺基)乙烯基矽烷、叁(第三丁基胺基)乙烯基矽烷、叁(二甲基胺基)乙烯基矽烷、叁(N-乙基甲基胺基)乙烯基矽烷、叁(二乙基胺基)乙烯基矽烷、叁(N-甲基環己基胺基)乙烯基矽烷、叁(N-甲基苯基胺基)乙烯基矽烷、三吡咯烷基乙烯基矽烷、叁(六氫吡啶基)乙烯基矽烷、三吡咯基乙烯基矽烷、雙(甲基胺基)甲基乙烯基矽烷、雙(乙基胺基)甲基乙烯基矽烷、雙(正丙基胺基)甲基乙烯基矽烷、雙(異丙基胺基)甲基乙烯基矽烷、雙(第二丁基胺基)甲基乙烯基矽烷、雙(第三丁基胺基)甲基乙烯基矽烷、雙(二甲基胺基)甲基乙烯基矽烷、雙(N-乙基甲基胺基)甲基乙烯基矽烷、雙(二乙基胺基)甲基乙烯基矽烷、雙(N-甲基環己基胺基)甲基乙烯基矽烷、雙(N-甲基苯基胺基)甲基乙烯基矽烷、二吡咯烷基甲基乙烯基矽烷、雙(六氫吡啶基)甲基乙烯基矽烷、二吡咯基甲基乙烯基矽烷、雙(甲基胺基)二乙烯基矽烷、雙(乙基胺基)二乙烯基矽烷、雙(正丙基胺基)二乙烯基矽烷、雙(異丙基胺基)二乙烯基矽烷、雙(第二丁基胺基)二乙烯基矽烷、雙(第三丁基胺基)二乙烯基矽烷、雙(二甲基胺基)二乙烯基矽烷、雙(N-乙基甲基胺基)二乙烯基矽烷、雙(二乙基胺基)二乙烯基矽烷、雙(N-甲基環己基胺基)二乙烯基矽烷、雙(N-甲基苯基胺基)二乙烯基矽烷、二吡咯烷基二乙烯基矽烷、雙(六氫吡啶基)二乙烯基矽烷、二吡咯基二乙烯基矽烷、(甲基胺基)二甲基乙烯基矽烷、(乙基胺基)二甲基乙烯基矽烷、(正丙基胺基)二甲基乙烯基矽 烷、(異丙基胺基)二甲基乙烯基矽烷、(第二丁基胺基)二甲基乙烯基矽烷、(第三丁基胺基)二甲基乙烯基矽烷、(二甲基胺基)二甲基乙烯基矽烷、(N-乙基甲基胺基)二甲基乙烯基矽烷、(二乙基胺基)二甲基乙烯基矽烷、(N-甲基環己基胺基)二甲基乙烯基矽烷、(N-甲基苯基胺基)二甲基乙烯基矽烷、吡咯烷基二甲基乙烯基矽烷、六氫吡啶基二甲基乙烯基矽烷、吡咯基二甲基乙烯基矽烷、(甲基胺基)甲基二乙烯基矽烷、(乙基胺基)甲基二乙烯基矽烷、(正丙基胺基)甲基二乙烯基矽烷、(異丙基胺基)甲基二乙烯基矽烷、(第二丁基胺基)甲基二乙烯基矽烷、(第三丁基胺基)甲基二乙烯基矽烷、(二甲基胺基)甲基二乙烯基矽烷、(N-乙基甲基胺基)甲基二乙烯基矽烷、(二乙基胺基)甲基二乙烯基矽烷、(N-甲基環己基胺基)甲基二乙烯基矽烷、(N-甲基苯基胺基)甲基二乙烯基矽烷、吡咯烷基甲基二乙烯基矽烷、六氫吡啶基甲基二乙烯基矽烷、吡咯基甲基二乙烯基矽烷、(甲基胺基)三乙烯基矽烷、(乙基胺基)三乙烯基矽烷、(正丙基胺基)三乙烯基矽烷、(異丙基胺基)三乙烯基矽烷、(第二丁基胺基)三乙烯基矽烷、(第三丁基胺基)三乙烯基矽烷、(二甲基胺基)三乙烯基矽烷、(N-乙基甲基胺基)三乙烯基矽烷、(二乙基胺基)三乙烯基矽烷、(N-甲基環己基胺基)三乙烯基矽烷、(N-甲基苯基胺基)甲基二乙烯基矽烷、吡咯烷基甲基三乙烯基矽烷、六氫吡啶基三乙烯基矽烷及吡咯基三乙烯基矽烷。
- 如請求項1之方法,其中該至少一有機胺基烯丙基矽烷前驅物包含至少一選自由以下所組成的群組之化合物:叁(甲基胺基)烯丙基矽烷、叁(乙基胺基)烯丙基矽烷、叁(正丙基胺基)烯丙基矽烷、叁(異丙基胺基)烯丙基矽烷、叁(第二丁基胺基)烯丙基矽烷、叁(第三丁基胺基)烯丙基矽烷、叁(二甲基胺基)烯丙基矽烷、叁(N-乙基甲基胺基)烯丙基矽烷、叁(二乙基胺基)烯丙基矽 烷、叁(N-甲基環己基胺基)烯丙基矽烷、叁(N-甲基苯基胺基)烯丙基矽烷、三吡咯烷基烯丙基矽烷、叁(六氫吡啶基)烯丙基矽烷、三吡咯基烯丙基矽烷、雙(甲基胺基)甲基烯丙基矽烷、雙(乙基胺基)甲基烯丙基矽烷、雙(正丙基胺基)甲基烯丙基矽烷、雙(異丙基胺基)甲基烯丙基矽烷、雙(第二丁基胺基)甲基烯丙基矽烷、雙(第三丁基胺基)甲基烯丙基矽烷、雙(二甲基胺基)甲基烯丙基矽烷、雙(N-乙基甲基胺基)甲基烯丙基矽烷、雙(二乙基胺基)甲基烯丙基矽烷、雙(N-甲基環己基胺基)甲基烯丙基矽烷、雙(N-甲基苯基胺基)甲基烯丙基矽烷、二吡咯烷基甲基烯丙基矽烷、雙(六氫吡啶基)甲基烯丙基矽烷、二吡咯基甲基烯丙基矽烷、雙(甲基胺基)二烯丙基矽烷、雙(乙基胺基)二烯丙基矽烷、雙(正丙基胺基)二烯丙基矽烷、雙(異丙基胺基)二烯丙基矽烷、雙(第二丁基胺基)二烯丙基矽烷、雙(第三丁基胺基)二烯丙基矽烷、雙(二甲基胺基)二烯丙基矽烷、雙(N-乙基甲基胺基)二烯丙基矽烷、雙(二乙基胺基)二烯丙基矽烷、雙(N-甲基環己基胺基)二烯丙基矽烷、雙(N-甲基苯基胺基)二烯丙基矽烷、二吡咯烷基二烯丙基矽烷、雙(六氫吡啶基)二烯丙基矽烷、二吡咯基二烯丙基矽烷、(甲基胺基)二甲基烯丙基矽烷、(乙基胺基)二甲基烯丙基矽烷、(正丙基胺基)二甲基烯丙基矽烷、(異丙基胺基)二甲基烯丙基矽烷、(第二丁基胺基)二甲基烯丙基矽烷、(第三丁基胺基)二甲基烯丙基矽烷、(二甲基胺基)二甲基烯丙基矽烷、(N-乙基甲基胺基)二甲基烯丙基矽烷、(二乙基胺基)二甲基烯丙基矽烷、(N-甲基環己基胺基)二甲基烯丙基矽烷、(N-甲基苯基胺基)二甲基烯丙基矽烷、吡咯烷基二甲基烯丙基矽烷、六氫吡啶基二甲基烯丙基矽烷、吡咯基二甲基烯丙基矽烷、(甲基胺基)甲基二烯丙基矽烷、(乙基胺基)甲基二烯丙基矽烷、(正丙基胺基)甲基二烯丙基矽烷、(異丙基胺基)甲基二烯丙基矽烷、(第二丁基胺基)甲基二烯丙基矽 烷、(第三丁基胺基)甲基二烯丙基矽烷、(二甲基胺基)甲基二烯丙基矽烷、(N-乙基甲基胺基)甲基二烯丙基矽烷、(二乙基胺基)甲基二烯丙基矽烷、(N-甲基環己基胺基)甲基二烯丙基矽烷、(N-甲基苯基胺基)甲基二烯丙基矽烷、吡咯烷基甲基二烯丙基矽烷、六氫吡啶基甲基二烯丙基矽烷、吡咯基甲基二烯丙基矽烷、(甲基胺基)三烯丙基矽烷、(乙基胺基)三烯丙基矽烷、(正丙基胺基)三烯丙基矽烷、(異丙基胺基)三烯丙基矽烷、(第二丁基胺基)三烯丙基矽烷、(第三丁基胺基)三烯丙基矽烷、(二甲基胺基)三烯丙基矽烷、(N-乙基甲基胺基)三烯丙基矽烷、(二乙基胺基)三烯丙基矽烷、(N-甲基環己基胺基)三烯丙基矽烷、(N-甲基苯基胺基)甲基二烯丙基矽烷、吡咯烷基甲基三烯丙基矽烷、六氫吡啶基三烯丙基矽烷及吡咯基三烯丙基矽烷。
- 如請求項1之方法,其中該有機胺基乙烯基矽烷或該有機胺基烯丙基矽烷實質上不含至少一選自由有機胺、鹵離子及金屬離子所組成的群組之雜質。
- 如請求項1之方法,其中該至少一含鍺前驅物係選自由三氯鍺烷(Cl3GeH)、鍺烷(GeH4)、二鍺烷(Ge2H6)、第三丁基鍺烷(tBuGeH3)、苯基鍺烷、第二丁基鍺烷、異丁基鍺烷及苯甲基鍺烷所組成的群組。
- 如請求項1之方法,其另外包含在引入該至少一第一含鍺前驅物之後,將還原氣體引入該反應艙。
- 如請求項1之方法,其中該基材的至少一表面為含矽膜,並且其中將該基材的至少一表面提供到反應艙中的步驟包含進行以下步驟直到達成所需的含矽膜厚度為止: 將該至少一式I及/或式II所示的有機胺基乙烯基矽烷或有機胺基烯丙基矽烷引入該反應艙中,用吹掃氣體吹掃該反應艙,將含氧源及/或含氮源引入該反應艙中,及使用吹掃氣體吹掃該反應艙。
- 如請求項7之方法,其中該含氮源係選自由氨、肼、單烷基肼、二烷基肼、氮、氮/氫、氨電漿、氮電漿、氮/氫電漿及其混合物所組成的群組。
- 如請求項7之方法,其中該含氧源係選自由水、過氧化氫、氧氣、氧電漿、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所組成的群組。
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TW201910358A (zh) * | 2017-07-27 | 2019-03-16 | 瑞士商盛禧奧歐洲有限責任公司 | 橡膠之製造中特定胺基矽基單體之用途 |
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