TWI394802B - 含金屬氧化物之膜形成用組成物,含金屬氧化物膜、含金屬氧化物膜所形成之基板及使用其之圖型形成方法 - Google Patents
含金屬氧化物之膜形成用組成物,含金屬氧化物膜、含金屬氧化物膜所形成之基板及使用其之圖型形成方法 Download PDFInfo
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- TWI394802B TWI394802B TW097144883A TW97144883A TWI394802B TW I394802 B TWI394802 B TW I394802B TW 097144883 A TW097144883 A TW 097144883A TW 97144883 A TW97144883 A TW 97144883A TW I394802 B TWI394802 B TW I394802B
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- acid
- film
- metal oxide
- ion
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- 229910044991 metal oxide Inorganic materials 0.000 title claims description 156
- 150000004706 metal oxides Chemical class 0.000 title claims description 156
- 239000000203 mixture Substances 0.000 title claims description 137
- 238000000034 method Methods 0.000 title claims description 93
- 239000000758 substrate Substances 0.000 title claims description 76
- 238000000059 patterning Methods 0.000 title claims 3
- -1 formic acid ion Chemical class 0.000 claims description 261
- 229920002120 photoresistant polymer Polymers 0.000 claims description 169
- 150000001875 compounds Chemical class 0.000 claims description 116
- 238000005530 etching Methods 0.000 claims description 81
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 80
- 238000001312 dry etching Methods 0.000 claims description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- 239000002253 acid Substances 0.000 claims description 49
- 239000003960 organic solvent Substances 0.000 claims description 49
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 42
- 229910052707 ruthenium Inorganic materials 0.000 claims description 42
- 125000004432 carbon atom Chemical group C* 0.000 claims description 34
- 238000009833 condensation Methods 0.000 claims description 32
- 125000003118 aryl group Chemical group 0.000 claims description 30
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 29
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- 230000007062 hydrolysis Effects 0.000 claims description 23
- 229910052799 carbon Inorganic materials 0.000 claims description 20
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 19
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
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- 239000001301 oxygen Substances 0.000 claims description 7
- MCRZWYDXIGCFKO-UHFFFAOYSA-N 2-butylpropanedioic acid Chemical compound CCCCC(C(O)=O)C(O)=O MCRZWYDXIGCFKO-UHFFFAOYSA-N 0.000 claims description 6
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- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- KKEYFWRCBNTPAC-UHFFFAOYSA-N benzene-dicarboxylic acid Natural products OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 6
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 6
- JXTHNDFMNIQAHM-UHFFFAOYSA-N dichloroacetic acid Chemical compound OC(=O)C(Cl)Cl JXTHNDFMNIQAHM-UHFFFAOYSA-N 0.000 claims description 6
- JFCQEDHGNNZCLN-UHFFFAOYSA-N glutaric acid Chemical compound OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 6
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 6
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- 229910052727 yttrium Inorganic materials 0.000 claims description 6
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- WXUAQHNMJWJLTG-VKHMYHEASA-N (S)-methylsuccinic acid Chemical compound OC(=O)[C@@H](C)CC(O)=O WXUAQHNMJWJLTG-VKHMYHEASA-N 0.000 claims description 5
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- 230000000052 comparative effect Effects 0.000 description 2
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- 230000006866 deterioration Effects 0.000 description 2
- TWXWPPKDQOWNSX-UHFFFAOYSA-N dicyclohexylmethanone Chemical compound C1CCCCC1C(=O)C1CCCCC1 TWXWPPKDQOWNSX-UHFFFAOYSA-N 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
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- SRUWDWCSOWUPIK-UHFFFAOYSA-L diphenyliodanium;carbonate Chemical compound [O-]C([O-])=O.C=1C=CC=CC=1[I+]C1=CC=CC=C1.C=1C=CC=CC=1[I+]C1=CC=CC=C1 SRUWDWCSOWUPIK-UHFFFAOYSA-L 0.000 description 2
- WQIRVUAXANLUPO-UHFFFAOYSA-M diphenyliodanium;iodide Chemical compound [I-].C=1C=CC=CC=1[I+]C1=CC=CC=C1 WQIRVUAXANLUPO-UHFFFAOYSA-M 0.000 description 2
- MVTYPWLHUYZVBS-UHFFFAOYSA-L dipotassium;2,2-dimethylpropanedioate Chemical compound [K+].[K+].[O-]C(=O)C(C)(C)C([O-])=O MVTYPWLHUYZVBS-UHFFFAOYSA-L 0.000 description 2
- HFXMCPGGROIARZ-UHFFFAOYSA-L dipotassium;2-butylpropanedioate Chemical compound [K+].[K+].CCCCC(C([O-])=O)C([O-])=O HFXMCPGGROIARZ-UHFFFAOYSA-L 0.000 description 2
- GMVIQOCPXTZUFJ-UHFFFAOYSA-L dipotassium;2-ethylpropanedioate Chemical compound [K+].[K+].CCC(C([O-])=O)C([O-])=O GMVIQOCPXTZUFJ-UHFFFAOYSA-L 0.000 description 2
- KGCHDZIEXHKCGM-UHFFFAOYSA-L dipotassium;2-propylpropanedioate Chemical compound [K+].[K+].CCCC(C([O-])=O)C([O-])=O KGCHDZIEXHKCGM-UHFFFAOYSA-L 0.000 description 2
- UZLGHNUASUZUOR-UHFFFAOYSA-L dipotassium;3-carboxy-3-hydroxypentanedioate Chemical compound [K+].[K+].OC(=O)CC(O)(C([O-])=O)CC([O-])=O UZLGHNUASUZUOR-UHFFFAOYSA-L 0.000 description 2
- CVOQYKPWIVSMDC-UHFFFAOYSA-L dipotassium;butanedioate Chemical compound [K+].[K+].[O-]C(=O)CCC([O-])=O CVOQYKPWIVSMDC-UHFFFAOYSA-L 0.000 description 2
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 description 2
- LXQXGFPPYLKKSD-UHFFFAOYSA-L disodium;2,2-diethylpropanedioate Chemical compound [Na+].[Na+].CCC(CC)(C([O-])=O)C([O-])=O LXQXGFPPYLKKSD-UHFFFAOYSA-L 0.000 description 2
- YPNVJUPWZCUTOD-UHFFFAOYSA-L disodium;2,2-dimethylpropanedioate Chemical compound [Na+].[Na+].[O-]C(=O)C(C)(C)C([O-])=O YPNVJUPWZCUTOD-UHFFFAOYSA-L 0.000 description 2
- XQUXFKCGNRWRIY-UHFFFAOYSA-L disodium;2-butylpropanedioate Chemical compound [Na+].[Na+].CCCCC(C([O-])=O)C([O-])=O XQUXFKCGNRWRIY-UHFFFAOYSA-L 0.000 description 2
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- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
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- LQNUMILKBSMSMM-UHFFFAOYSA-M lithium;butanedioate;hydron Chemical compound [Li+].OC(=O)CCC([O-])=O LQNUMILKBSMSMM-UHFFFAOYSA-M 0.000 description 2
- DXUUIDJNCBRHDV-UHFFFAOYSA-M lithium;hydron;oxalate Chemical compound [Li+].OC(=O)C([O-])=O DXUUIDJNCBRHDV-UHFFFAOYSA-M 0.000 description 2
- BDJSOPWXYLFTNW-UHFFFAOYSA-N methyl 3-methoxypropanoate Chemical compound COCCC(=O)OC BDJSOPWXYLFTNW-UHFFFAOYSA-N 0.000 description 2
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- IZJVVXCHJIQVOL-UHFFFAOYSA-N nitro(phenyl)methanesulfonic acid Chemical class OS(=O)(=O)C([N+]([O-])=O)C1=CC=CC=C1 IZJVVXCHJIQVOL-UHFFFAOYSA-N 0.000 description 2
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- ORVIOKALGSDSHU-UHFFFAOYSA-L pentanedioate;tetrabutylazanium Chemical compound [O-]C(=O)CCCC([O-])=O.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC ORVIOKALGSDSHU-UHFFFAOYSA-L 0.000 description 2
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- GZCKIUIIYCBICZ-UHFFFAOYSA-L disodium;benzene-1,3-dicarboxylate Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=CC(C([O-])=O)=C1 GZCKIUIIYCBICZ-UHFFFAOYSA-L 0.000 description 1
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- 125000004185 ester group Chemical group 0.000 description 1
- NPYRBYNTERJZBA-UHFFFAOYSA-N ethanesulfonic acid;1-hydroxypyrrole-2,5-dione Chemical compound CCS(O)(=O)=O.ON1C(=O)C=CC1=O NPYRBYNTERJZBA-UHFFFAOYSA-N 0.000 description 1
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- 125000006232 ethoxy propyl group Chemical group [H]C([H])([H])C([H])([H])OC([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- LRANRHDJNHABBA-UHFFFAOYSA-N ethoxyarsenic Chemical compound CCO[As] LRANRHDJNHABBA-UHFFFAOYSA-N 0.000 description 1
- MXWVIHZQMUONMP-UHFFFAOYSA-N ethoxyboron Chemical compound [B]OCC MXWVIHZQMUONMP-UHFFFAOYSA-N 0.000 description 1
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- 125000005745 ethoxymethyl group Chemical group [H]C([H])([H])C([H])([H])OC([H])([H])* 0.000 description 1
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- CEIPQQODRKXDSB-UHFFFAOYSA-N ethyl 3-(6-hydroxynaphthalen-2-yl)-1H-indazole-5-carboximidate dihydrochloride Chemical compound Cl.Cl.C1=C(O)C=CC2=CC(C3=NNC4=CC=C(C=C43)C(=N)OCC)=CC=C21 CEIPQQODRKXDSB-UHFFFAOYSA-N 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
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- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 125000001207 fluorophenyl group Chemical group 0.000 description 1
- VZCYOOQTPOCHFL-OWOJBTEDSA-L fumarate(2-) Chemical class [O-]C(=O)\C=C\C([O-])=O VZCYOOQTPOCHFL-OWOJBTEDSA-L 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 125000002541 furyl group Chemical group 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- WRXPZSXSFWLBSD-UHFFFAOYSA-M heptanoate;tetrabutylazanium Chemical compound CCCCCCC([O-])=O.CCCC[N+](CCCC)(CCCC)CCCC WRXPZSXSFWLBSD-UHFFFAOYSA-M 0.000 description 1
- QHZOCFVYIBVNMJ-UHFFFAOYSA-M heptanoate;tetramethylazanium Chemical compound C[N+](C)(C)C.CCCCCCC([O-])=O QHZOCFVYIBVNMJ-UHFFFAOYSA-M 0.000 description 1
- WTQMEYZTFXQLCX-UHFFFAOYSA-M heptanoate;tetrapropylazanium Chemical compound CCCCCCC([O-])=O.CCC[N+](CCC)(CCC)CCC WTQMEYZTFXQLCX-UHFFFAOYSA-M 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- LMWSRVWOZUNBFI-UHFFFAOYSA-L hexanedioate;tetrabutylazanium Chemical compound [O-]C(=O)CCCCC([O-])=O.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC LMWSRVWOZUNBFI-UHFFFAOYSA-L 0.000 description 1
- RAGCYQGLSMWPJY-UHFFFAOYSA-L hexanedioate;tetrapropylazanium Chemical compound [O-]C(=O)CCCCC([O-])=O.CCC[N+](CCC)(CCC)CCC.CCC[N+](CCC)(CCC)CCC RAGCYQGLSMWPJY-UHFFFAOYSA-L 0.000 description 1
- LRKWNOHBWJKTGW-UHFFFAOYSA-M hexanoate;tetramethylazanium Chemical compound C[N+](C)(C)C.CCCCCC([O-])=O LRKWNOHBWJKTGW-UHFFFAOYSA-M 0.000 description 1
- WODXYOFAEMUOJG-UHFFFAOYSA-M hexanoate;tetrapropylazanium Chemical compound CCCCCC([O-])=O.CCC[N+](CCC)(CCC)CCC WODXYOFAEMUOJG-UHFFFAOYSA-M 0.000 description 1
- QXFORXKQXOSOOB-UHFFFAOYSA-M hexanoate;triphenylsulfanium Chemical compound CCCCCC([O-])=O.C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1 QXFORXKQXOSOOB-UHFFFAOYSA-M 0.000 description 1
- PNLSQMMDWXZWHO-UHFFFAOYSA-N hexoxyboron Chemical compound [B]OCCCCCC PNLSQMMDWXZWHO-UHFFFAOYSA-N 0.000 description 1
- 229910000042 hydrogen bromide Inorganic materials 0.000 description 1
- ARRNBPCNZJXHRJ-UHFFFAOYSA-M hydron;tetrabutylazanium;phosphate Chemical compound OP(O)([O-])=O.CCCC[N+](CCCC)(CCCC)CCCC ARRNBPCNZJXHRJ-UHFFFAOYSA-M 0.000 description 1
- CSFWPUWCSPOLJW-UHFFFAOYSA-N hydroxynaphthoquinone Natural products C1=CC=C2C(=O)C(O)=CC(=O)C2=C1 CSFWPUWCSPOLJW-UHFFFAOYSA-N 0.000 description 1
- 150000004340 hydroxynaphthoquinones Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 description 1
- 229940006461 iodide ion Drugs 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-L isophthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC(C([O-])=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-L 0.000 description 1
- 150000002596 lactones Chemical group 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- LLHSVDPAGWNSGM-GRHBHMESSA-M lithium (Z)-4-hydroxy-4-oxobut-2-enoate dihydrate Chemical compound [Li+].O.O.OC(=O)\C=C/C([O-])=O LLHSVDPAGWNSGM-GRHBHMESSA-M 0.000 description 1
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 1
- 229940031993 lithium benzoate Drugs 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229940008015 lithium carbonate Drugs 0.000 description 1
- 229910000032 lithium hydrogen carbonate Inorganic materials 0.000 description 1
- 229960004254 lithium succinate Drugs 0.000 description 1
- OLMNIZJJAAWPAB-NBTZWHCOSA-M lithium;(9z,12z)-octadeca-9,12-dienoate Chemical compound [Li+].CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O OLMNIZJJAAWPAB-NBTZWHCOSA-M 0.000 description 1
- BLKXGOSKCMAKDP-TYYBGVCCSA-M lithium;(e)-4-hydroxy-4-oxobut-2-enoate Chemical compound [Li+].OC(=O)\C=C\C([O-])=O BLKXGOSKCMAKDP-TYYBGVCCSA-M 0.000 description 1
- AVOVSJYQRZMDQJ-KVVVOXFISA-M lithium;(z)-octadec-9-enoate Chemical compound [Li+].CCCCCCCC\C=C/CCCCCCCC([O-])=O AVOVSJYQRZMDQJ-KVVVOXFISA-M 0.000 description 1
- HOIXWIJGBXDJIX-UHFFFAOYSA-M lithium;2,2,2-trichloroacetate Chemical compound [Li+].[O-]C(=O)C(Cl)(Cl)Cl HOIXWIJGBXDJIX-UHFFFAOYSA-M 0.000 description 1
- OHXYLFVFSUFWPO-UHFFFAOYSA-M lithium;2-chloroacetate Chemical compound [Li+].[O-]C(=O)CCl OHXYLFVFSUFWPO-UHFFFAOYSA-M 0.000 description 1
- PSBOOKLOXQFNPZ-UHFFFAOYSA-M lithium;2-hydroxybenzoate Chemical compound [Li+].OC1=CC=CC=C1C([O-])=O PSBOOKLOXQFNPZ-UHFFFAOYSA-M 0.000 description 1
- OUHZLYYIQKBPDL-UHFFFAOYSA-M lithium;3-butoxy-3-oxopropanoate Chemical compound [Li+].CCCCOC(=O)CC([O-])=O OUHZLYYIQKBPDL-UHFFFAOYSA-M 0.000 description 1
- RGEQBXRWZNWGIC-UHFFFAOYSA-M lithium;3-oxo-3-propoxypropanoate Chemical compound [Li+].CCCOC(=O)CC([O-])=O RGEQBXRWZNWGIC-UHFFFAOYSA-M 0.000 description 1
- LDJNSLOKTFFLSL-UHFFFAOYSA-M lithium;benzoate Chemical compound [Li+].[O-]C(=O)C1=CC=CC=C1 LDJNSLOKTFFLSL-UHFFFAOYSA-M 0.000 description 1
- WIAVVDGWLCNNGT-UHFFFAOYSA-M lithium;butanoate Chemical compound [Li+].CCCC([O-])=O WIAVVDGWLCNNGT-UHFFFAOYSA-M 0.000 description 1
- XKPJKVVZOOEMPK-UHFFFAOYSA-M lithium;formate Chemical compound [Li+].[O-]C=O XKPJKVVZOOEMPK-UHFFFAOYSA-M 0.000 description 1
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- XNWSMNKRGNKRKP-UHFFFAOYSA-M propanoate;tetramethylazanium Chemical compound CCC([O-])=O.C[N+](C)(C)C XNWSMNKRGNKRKP-UHFFFAOYSA-M 0.000 description 1
- VTIZRIDYIWLCRE-UHFFFAOYSA-M propanoate;tetrapropylazanium Chemical compound CCC([O-])=O.CCC[N+](CCC)(CCC)CCC VTIZRIDYIWLCRE-UHFFFAOYSA-M 0.000 description 1
- BVLKECPAIWFGHO-UHFFFAOYSA-M propanoate;triphenylsulfanium Chemical compound CCC([O-])=O.C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1 BVLKECPAIWFGHO-UHFFFAOYSA-M 0.000 description 1
- 125000006233 propoxy propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])OC([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
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- 229940001593 sodium carbonate Drugs 0.000 description 1
- 229940080263 sodium dichloroacetate Drugs 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- 229940005573 sodium fumarate Drugs 0.000 description 1
- 235000019294 sodium fumarate Nutrition 0.000 description 1
- UDWXLZLRRVQONG-UHFFFAOYSA-M sodium hexanoate Chemical compound [Na+].CCCCCC([O-])=O UDWXLZLRRVQONG-UHFFFAOYSA-M 0.000 description 1
- PRWXGRGLHYDWPS-UHFFFAOYSA-L sodium malonate Chemical compound [Na+].[Na+].[O-]C(=O)CC([O-])=O PRWXGRGLHYDWPS-UHFFFAOYSA-L 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- BYKRNSHANADUFY-UHFFFAOYSA-M sodium octanoate Chemical compound [Na+].CCCCCCCC([O-])=O BYKRNSHANADUFY-UHFFFAOYSA-M 0.000 description 1
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 1
- 229940039790 sodium oxalate Drugs 0.000 description 1
- JXKPEJDQGNYQSM-UHFFFAOYSA-M sodium propionate Chemical compound [Na+].CCC([O-])=O JXKPEJDQGNYQSM-UHFFFAOYSA-M 0.000 description 1
- 239000004324 sodium propionate Substances 0.000 description 1
- 235000010334 sodium propionate Nutrition 0.000 description 1
- 229960003212 sodium propionate Drugs 0.000 description 1
- 229960004025 sodium salicylate Drugs 0.000 description 1
- WYPBVHPKMJYUEO-NBTZWHCOSA-M sodium;(9z,12z)-octadeca-9,12-dienoate Chemical compound [Na+].CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O WYPBVHPKMJYUEO-NBTZWHCOSA-M 0.000 description 1
- UNZSHUCNBUBSGW-IFNWOZJISA-M sodium;(9z,12z,15z)-octadeca-9,12,15-trienoate Chemical compound [Na+].CC\C=C/C\C=C/C\C=C/CCCCCCCC([O-])=O UNZSHUCNBUBSGW-IFNWOZJISA-M 0.000 description 1
- VRVKOZSIJXBAJG-ODZAUARKSA-M sodium;(z)-but-2-enedioate;hydron Chemical compound [Na+].OC(=O)\C=C/C([O-])=O VRVKOZSIJXBAJG-ODZAUARKSA-M 0.000 description 1
- UYCAUPASBSROMS-AWQJXPNKSA-M sodium;2,2,2-trifluoroacetate Chemical compound [Na+].[O-][13C](=O)[13C](F)(F)F UYCAUPASBSROMS-AWQJXPNKSA-M 0.000 description 1
- LUPNKHXLFSSUGS-UHFFFAOYSA-M sodium;2,2-dichloroacetate Chemical compound [Na+].[O-]C(=O)C(Cl)Cl LUPNKHXLFSSUGS-UHFFFAOYSA-M 0.000 description 1
- JPFUMBONGCPIDF-UHFFFAOYSA-M sodium;3-methoxy-3-oxopropanoate Chemical compound [Na+].COC(=O)CC([O-])=O JPFUMBONGCPIDF-UHFFFAOYSA-M 0.000 description 1
- KTXXZLNFBWJCSV-UHFFFAOYSA-M sodium;3-oxo-3-propoxypropanoate Chemical compound [Na+].CCCOC(=O)CC([O-])=O KTXXZLNFBWJCSV-UHFFFAOYSA-M 0.000 description 1
- KDWCFTLLFHIQHU-UHFFFAOYSA-M sodium;4-methoxy-4-oxobutanoate Chemical compound [Na+].COC(=O)CCC([O-])=O KDWCFTLLFHIQHU-UHFFFAOYSA-M 0.000 description 1
- NMTDPTPUELYEPL-UHFFFAOYSA-M sodium;heptanoate Chemical compound [Na+].CCCCCCC([O-])=O NMTDPTPUELYEPL-UHFFFAOYSA-M 0.000 description 1
- GOGGIOPQLKEIGC-UHFFFAOYSA-M sodium;hexanedioate;hydron Chemical compound [Na+].OC(=O)CCCCC([O-])=O GOGGIOPQLKEIGC-UHFFFAOYSA-M 0.000 description 1
- UJRAXLUXHBUNDO-UHFFFAOYSA-M sodium;hydron;oxalate Chemical compound [Na+].OC(=O)C([O-])=O UJRAXLUXHBUNDO-UHFFFAOYSA-M 0.000 description 1
- LXWZLYDXYCQRJT-UHFFFAOYSA-M sodium;hydron;propanedioate Chemical compound [H+].[Na+].[O-]C(=O)CC([O-])=O LXWZLYDXYCQRJT-UHFFFAOYSA-M 0.000 description 1
- LHYPLJGBYPAQAK-UHFFFAOYSA-M sodium;pentanoate Chemical compound [Na+].CCCCC([O-])=O LHYPLJGBYPAQAK-UHFFFAOYSA-M 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 229940114926 stearate Drugs 0.000 description 1
- 125000000547 substituted alkyl group Chemical group 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 229960002317 succinimide Drugs 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 108010059434 tapasin Proteins 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- XBLNHYLUTUZOGX-UHFFFAOYSA-L terephthalate;tetrabutylazanium Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC XBLNHYLUTUZOGX-UHFFFAOYSA-L 0.000 description 1
- SFZIOISNGCFHIC-UHFFFAOYSA-L terephthalate;tetramethylazanium Chemical compound C[N+](C)(C)C.C[N+](C)(C)C.[O-]C(=O)C1=CC=C(C([O-])=O)C=C1 SFZIOISNGCFHIC-UHFFFAOYSA-L 0.000 description 1
- VGOWDYSXYFYPBX-UHFFFAOYSA-L terephthalate;triphenylsulfanium Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1.C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1 VGOWDYSXYFYPBX-UHFFFAOYSA-L 0.000 description 1
- JAELLLITIZHOGQ-UHFFFAOYSA-N tert-butyl propanoate Chemical compound CCC(=O)OC(C)(C)C JAELLLITIZHOGQ-UHFFFAOYSA-N 0.000 description 1
- FLCDSBKFFIMXLQ-UHFFFAOYSA-M tetrabutylazanium;2,2,2-trichloroacetate Chemical compound [O-]C(=O)C(Cl)(Cl)Cl.CCCC[N+](CCCC)(CCCC)CCCC FLCDSBKFFIMXLQ-UHFFFAOYSA-M 0.000 description 1
- WTEXQPWIUJQYJQ-UHFFFAOYSA-M tetrabutylazanium;2,2,2-trifluoroacetate Chemical compound [O-]C(=O)C(F)(F)F.CCCC[N+](CCCC)(CCCC)CCCC WTEXQPWIUJQYJQ-UHFFFAOYSA-M 0.000 description 1
- MCZDHTKJGDCTAE-UHFFFAOYSA-M tetrabutylazanium;acetate Chemical compound CC([O-])=O.CCCC[N+](CCCC)(CCCC)CCCC MCZDHTKJGDCTAE-UHFFFAOYSA-M 0.000 description 1
- WGYONVRJGWHMKV-UHFFFAOYSA-M tetrabutylazanium;benzoate Chemical compound [O-]C(=O)C1=CC=CC=C1.CCCC[N+](CCCC)(CCCC)CCCC WGYONVRJGWHMKV-UHFFFAOYSA-M 0.000 description 1
- UVVFKNZCYIIHGM-UHFFFAOYSA-L tetrabutylazanium;carbonate Chemical compound [O-]C([O-])=O.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC UVVFKNZCYIIHGM-UHFFFAOYSA-L 0.000 description 1
- CDDFFMJAOKTPRF-UHFFFAOYSA-M tetrabutylazanium;chlorate Chemical compound [O-]Cl(=O)=O.CCCC[N+](CCCC)(CCCC)CCCC CDDFFMJAOKTPRF-UHFFFAOYSA-M 0.000 description 1
- SNMZANHSFVMKKA-UHFFFAOYSA-M tetrabutylazanium;formate Chemical compound [O-]C=O.CCCC[N+](CCCC)(CCCC)CCCC SNMZANHSFVMKKA-UHFFFAOYSA-M 0.000 description 1
- UZPGPVQCDJXSNM-UHFFFAOYSA-M tetrabutylazanium;iodate Chemical compound [O-]I(=O)=O.CCCC[N+](CCCC)(CCCC)CCCC UZPGPVQCDJXSNM-UHFFFAOYSA-M 0.000 description 1
- DPKBAXPHAYBPRL-UHFFFAOYSA-M tetrabutylazanium;iodide Chemical compound [I-].CCCC[N+](CCCC)(CCCC)CCCC DPKBAXPHAYBPRL-UHFFFAOYSA-M 0.000 description 1
- KBLZDCFTQSIIOH-UHFFFAOYSA-M tetrabutylazanium;perchlorate Chemical compound [O-]Cl(=O)(=O)=O.CCCC[N+](CCCC)(CCCC)CCCC KBLZDCFTQSIIOH-UHFFFAOYSA-M 0.000 description 1
- MNYPPALWIOMJJI-UHFFFAOYSA-N tetrabutylazanium;toluene Chemical compound CC1=CC=CC=C1.CCCC[N+](CCCC)(CCCC)CCCC MNYPPALWIOMJJI-UHFFFAOYSA-N 0.000 description 1
- DDFYFBUWEBINLX-UHFFFAOYSA-M tetramethylammonium bromide Chemical compound [Br-].C[N+](C)(C)C DDFYFBUWEBINLX-UHFFFAOYSA-M 0.000 description 1
- LROATHSBUUYETB-UHFFFAOYSA-M tetramethylazanium;2,2,2-trifluoroacetate Chemical compound C[N+](C)(C)C.[O-]C(=O)C(F)(F)F LROATHSBUUYETB-UHFFFAOYSA-M 0.000 description 1
- IEVVGBFMAHJELO-UHFFFAOYSA-M tetramethylazanium;benzoate Chemical compound C[N+](C)(C)C.[O-]C(=O)C1=CC=CC=C1 IEVVGBFMAHJELO-UHFFFAOYSA-M 0.000 description 1
- NAWVCYVCEVTDBQ-UHFFFAOYSA-M tetramethylazanium;bromate Chemical compound [O-]Br(=O)=O.C[N+](C)(C)C NAWVCYVCEVTDBQ-UHFFFAOYSA-M 0.000 description 1
- WJZPIORVERXPPR-UHFFFAOYSA-L tetramethylazanium;carbonate Chemical compound [O-]C([O-])=O.C[N+](C)(C)C.C[N+](C)(C)C WJZPIORVERXPPR-UHFFFAOYSA-L 0.000 description 1
- LUVHDTDFZLTVFM-UHFFFAOYSA-M tetramethylazanium;chlorate Chemical compound [O-]Cl(=O)=O.C[N+](C)(C)C LUVHDTDFZLTVFM-UHFFFAOYSA-M 0.000 description 1
- WWIYWFVQZQOECA-UHFFFAOYSA-M tetramethylazanium;formate Chemical compound [O-]C=O.C[N+](C)(C)C WWIYWFVQZQOECA-UHFFFAOYSA-M 0.000 description 1
- RXMRGBVLCSYIBO-UHFFFAOYSA-M tetramethylazanium;iodide Chemical compound [I-].C[N+](C)(C)C RXMRGBVLCSYIBO-UHFFFAOYSA-M 0.000 description 1
- ZCWKIFAQRXNZCH-UHFFFAOYSA-M tetramethylazanium;perchlorate Chemical compound C[N+](C)(C)C.[O-]Cl(=O)(=O)=O ZCWKIFAQRXNZCH-UHFFFAOYSA-M 0.000 description 1
- WGBAQVHWLZBRJU-UHFFFAOYSA-M tetrapropylazanium;2,2,2-trichloroacetate Chemical compound [O-]C(=O)C(Cl)(Cl)Cl.CCC[N+](CCC)(CCC)CCC WGBAQVHWLZBRJU-UHFFFAOYSA-M 0.000 description 1
- BQBCSZFEFRYJPX-UHFFFAOYSA-M tetrapropylazanium;2,2,2-trifluoroacetate Chemical compound [O-]C(=O)C(F)(F)F.CCC[N+](CCC)(CCC)CCC BQBCSZFEFRYJPX-UHFFFAOYSA-M 0.000 description 1
- PXJUBOLFJDSAQQ-UHFFFAOYSA-M tetrapropylazanium;acetate Chemical compound CC([O-])=O.CCC[N+](CCC)(CCC)CCC PXJUBOLFJDSAQQ-UHFFFAOYSA-M 0.000 description 1
- QOHLYFXRPYZSJX-UHFFFAOYSA-M tetrapropylazanium;benzoate Chemical compound [O-]C(=O)C1=CC=CC=C1.CCC[N+](CCC)(CCC)CCC QOHLYFXRPYZSJX-UHFFFAOYSA-M 0.000 description 1
- DKBLJGBNSOBLAO-UHFFFAOYSA-L tetrapropylazanium;carbonate Chemical compound [O-]C([O-])=O.CCC[N+](CCC)(CCC)CCC.CCC[N+](CCC)(CCC)CCC DKBLJGBNSOBLAO-UHFFFAOYSA-L 0.000 description 1
- XKRJGOGYPUVFOV-UHFFFAOYSA-M tetrapropylazanium;chlorate Chemical compound [O-]Cl(=O)=O.CCC[N+](CCC)(CCC)CCC XKRJGOGYPUVFOV-UHFFFAOYSA-M 0.000 description 1
- FBEVECUEMUUFKM-UHFFFAOYSA-M tetrapropylazanium;chloride Chemical compound [Cl-].CCC[N+](CCC)(CCC)CCC FBEVECUEMUUFKM-UHFFFAOYSA-M 0.000 description 1
- LENBOWGJEQXFCI-UHFFFAOYSA-M tetrapropylazanium;formate Chemical compound [O-]C=O.CCC[N+](CCC)(CCC)CCC LENBOWGJEQXFCI-UHFFFAOYSA-M 0.000 description 1
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 1
- AUDFRERWRXKGGS-UHFFFAOYSA-M tetrapropylazanium;iodate Chemical compound [O-]I(=O)=O.CCC[N+](CCC)(CCC)CCC AUDFRERWRXKGGS-UHFFFAOYSA-M 0.000 description 1
- GKXDJYKZFZVASJ-UHFFFAOYSA-M tetrapropylazanium;iodide Chemical compound [I-].CCC[N+](CCC)(CCC)CCC GKXDJYKZFZVASJ-UHFFFAOYSA-M 0.000 description 1
- HZPNJVXVIFRTRF-UHFFFAOYSA-N tetrapropylazanium;nitrate Chemical compound [O-][N+]([O-])=O.CCC[N+](CCC)(CCC)CCC HZPNJVXVIFRTRF-UHFFFAOYSA-N 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical compound [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- AANIRNIRVXARSN-UHFFFAOYSA-M trifluoromethanesulfonate;trimethylsulfanium Chemical compound C[S+](C)C.[O-]S(=O)(=O)C(F)(F)F AANIRNIRVXARSN-UHFFFAOYSA-M 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- QFCVQKSWGFVMTB-UHFFFAOYSA-N trihexoxyalumane Chemical compound [Al+3].CCCCCC[O-].CCCCCC[O-].CCCCCC[O-] QFCVQKSWGFVMTB-UHFFFAOYSA-N 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
- CYTQBVOFDCPGCX-UHFFFAOYSA-N trimethyl phosphite Chemical compound COP(OC)OC CYTQBVOFDCPGCX-UHFFFAOYSA-N 0.000 description 1
- LIJDDOXRYWAXQG-UHFFFAOYSA-N tripentoxyalumane Chemical compound CCCCCO[Al](OCCCCC)OCCCCC LIJDDOXRYWAXQG-UHFFFAOYSA-N 0.000 description 1
- GOUGVXDHOZBESW-UHFFFAOYSA-M triphenylsulfanium;benzoate Chemical compound [O-]C(=O)C1=CC=CC=C1.C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1 GOUGVXDHOZBESW-UHFFFAOYSA-M 0.000 description 1
- SPXRMAGRRRUEGL-UHFFFAOYSA-L triphenylsulfanium;carbonate Chemical compound [O-]C([O-])=O.C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1 SPXRMAGRRRUEGL-UHFFFAOYSA-L 0.000 description 1
- RCEIBALRNHFOOG-UHFFFAOYSA-M triphenylsulfanium;chlorate Chemical compound [O-]Cl(=O)=O.C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1 RCEIBALRNHFOOG-UHFFFAOYSA-M 0.000 description 1
- ZFEAYIKULRXTAR-UHFFFAOYSA-M triphenylsulfanium;chloride Chemical compound [Cl-].C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1 ZFEAYIKULRXTAR-UHFFFAOYSA-M 0.000 description 1
- UGPPZNGBFLGAKN-UHFFFAOYSA-M triphenylsulfanium;formate Chemical compound [O-]C=O.C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1 UGPPZNGBFLGAKN-UHFFFAOYSA-M 0.000 description 1
- CVJLQNNJZBCTLI-UHFFFAOYSA-M triphenylsulfanium;iodide Chemical compound [I-].C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1 CVJLQNNJZBCTLI-UHFFFAOYSA-M 0.000 description 1
- GSTFPARBGSPPTI-UHFFFAOYSA-M triphenylsulfanium;perchlorate Chemical compound [O-]Cl(=O)(=O)=O.C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1 GSTFPARBGSPPTI-UHFFFAOYSA-M 0.000 description 1
- OBROYCQXICMORW-UHFFFAOYSA-N tripropoxyalumane Chemical compound [Al+3].CCC[O-].CCC[O-].CCC[O-] OBROYCQXICMORW-UHFFFAOYSA-N 0.000 description 1
- QOPBTFMUVTXWFF-UHFFFAOYSA-N tripropyl phosphite Chemical compound CCCOP(OCCC)OCCC QOPBTFMUVTXWFF-UHFFFAOYSA-N 0.000 description 1
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229940070710 valerate Drugs 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- DJIFSIBYHXVGSS-UHFFFAOYSA-J zirconium(4+);tetraphenoxide Chemical compound [Zr+4].[O-]C1=CC=CC=C1.[O-]C1=CC=CC=C1.[O-]C1=CC=CC=C1.[O-]C1=CC=CC=C1 DJIFSIBYHXVGSS-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/02—Oxides
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/09—Photosensitive materials characterised by structural details, e.g. supports, auxiliary layers
- G03F7/11—Photosensitive materials characterised by structural details, e.g. supports, auxiliary layers having cover layers or intermediate layers, e.g. subbing layers
-
- 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
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/48—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
- C08G77/56—Boron-containing linkages
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/14—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/075—Silicon-containing compounds
- G03F7/0752—Silicon-containing compounds in non photosensitive layers or as additives, e.g. for dry lithography
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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Description
本發明為有關於半導體元件等之製造步驟中,微細加工所使用之多層光阻法中作為中間層使用之含金屬氧化物膜,特別是適合以迴轉塗佈形成中間層之含金屬氧化物之膜形成用組成物,使用其所形成之含金屬氧化物膜,含金屬氧化物膜所形成之基板及使用其之圖型形成方法之發明。
伴隨LSI之高積體化與高速度化,而使圖型規則急速的邁向微細化。微影蝕刻技術,伴隨該微細化,經由對光源之短波長化與與其相對之光阻組成物作適當選擇下,而達成形成微細圖型。而其中心,即為以單層使用之正型光阻組成物。該單層正型光阻組成物,於光阻樹脂中,具有對氯系或氟系之氣體電漿的乾式蝕刻具有耐蝕刻性之骨架,且於具有溶解曝光部之光阻機構,故於曝光部溶解後形成圖型,所殘留之光阻圖型則作為蝕刻遮罩,以對塗佈有光阻組成物之被加工基板進行乾式蝕刻加工者。
其中,使所使用之光阻膜的膜厚於無處理下使其微細化,即縮小圖型寬度之情形中,因光阻膜之解析性能降低,或使用顯影液將光阻膜進行圖型顯影時,將會造成所謂長徑比過大,其結果將會引起圖型崩壞。因此,伴隨微細化之過程,光阻膜厚將需趨向薄膜化。
又,對被加工基板之加工中,通常為使用形成圖型之光阻膜作為蝕刻遮罩,以乾式蝕刻方式對基板進行加工之方法,但實際上,於光阻膜與被加工基板之間並沒有可以取得完全蝕刻選擇性之乾式蝕刻方法,故於基板之加工中也會使光阻膜受到損傷,使基板加工中之光阻膜崩壞,進而無法將光阻圖型正確地轉印於被加工基板。其中,伴隨圖型之微細化過程,目前則尋求一種具有更高乾式蝕刻耐性的光阻組成物。
又,隨著曝光波長之短波長化中,光阻組成物所使用之樹脂,一般為尋求於曝光波長中具有較小光吸收之樹脂,其相對於i線、KrF、ArF之變化,可變化為酚醛清漆樹脂、聚羥基苯乙烯、具有脂肪族多環狀骨架之樹脂等,於實際上,將會形成上述乾式蝕刻條件中蝕刻速度較快之物,因此,解析性較高之最近的光阻組成物,毋寧說其耐蝕刻性具有降低之傾向。
基於前述說明,目前必須使用更薄且更低耐蝕刻性之光阻膜對被加工基板進行乾式蝕刻加工,因此,於該加工步驟中如何確保材料及製程則為目前之要務。
解決前述問題點之方法之一,為多層光阻法。該方法中,為將光阻膜,即光阻上層膜,與具有不同蝕刻選擇性之中間膜,使其介於光阻上層膜與被加工基板之間,於光阻上層膜得到圖型後,將上層光阻圖型作為乾式蝕刻遮罩,以乾式蝕刻將圖型轉印於中間膜,隨後再將中間膜作為乾式蝕刻遮罩,以乾式蝕刻法將圖形轉印於被加工基板之
方法。
多層光阻法中之一的2層光阻法中,例如,上層光阻組成物使用含矽之樹脂,中間膜使用酚醛清漆樹脂之方法(例如、專利文獻1:特開平6-95385號公報)。矽樹脂,對於使用氧電漿所進行之反應性乾式蝕刻,雖顯示出較佳之耐蝕刻性,但於使用氟系氣體電漿時,則容易被蝕刻去除。又,酚醛清漆樹脂於使用氧氣體電漿進行反應性乾式蝕刻時,則容易被蝕刻去除,但對於氟系氣體電漿或氯系氣體電漿進行之乾式蝕刻,則顯示出良好之耐蝕刻性。其中,於被加工基板上,將酚醛清漆樹脂膜以光阻中間膜形式形成膜,再於其上使用含矽之樹脂形成光阻上層膜。隨後,對含矽之光阻膜使用能量線照射及顯影等後處理以形成圖型,再將其作為乾式蝕刻遮罩,而以氧電漿進行反應性乾式蝕刻,以將去除光阻圖型之部份的酚醛清漆樹脂以乾式蝕刻法去除,而將圖形轉印於酚醛清漆膜,再將轉印於該酚醛清漆膜之圖型作為乾式蝕刻遮罩,對被加工基板使用氟系氣體電漿或氯系氣體電漿進行蝕刻,而可將圖形轉印。
使用該些乾式蝕刻之圖型轉印,因蝕刻遮罩具有充分之耐蝕刻性之情形中,可以較良好之形狀得到轉印圖型,且不容易引起於光阻顯影時因顯影液所造成之摩擦等原因所造成之圖型倒塌等問題,而可得到具有較高長徑比之圖型。因此,例如使用酚醛清漆樹脂所得之光阻膜作為中間膜之膜厚具有相當厚度之場合中,相對於因長徑比之問題
而於顯影時造成圖型倒塌等,而無法直接形成之微細圖型而言,上述2層光阻法,被加工基板作為乾式蝕刻遮罩時,可得到具有充分厚度之酚醛清漆樹脂圖型。
又,多層光阻法,可使用單層光阻法所使用之一般性光阻組成物的3層光阻法。例如,於被加工基板上,使用以酚醛清漆等所得之有機膜以光阻下層膜之方式成膜,於其上再將含矽膜以光阻中間膜方式成膜,於其上,再將通常之有機系光阻膜以光阻上層膜形式形成。相對於氟系氣體電漿之乾式蝕刻,於有機系之光阻上層膜,因可取得相對於含矽光阻中間膜之良好蝕刻選擇比,故光阻圖型可以氟系氣體電漿之乾式蝕刻而轉印於含矽之光阻中間膜。依該方法,即使使用不易形成可對直接被加工基板進行加工之具有充分膜厚度之圖型的光阻組成物,或為加工基板所使用之不具有充分乾式蝕刻耐性之光阻組成物時,只要可將圖型轉印於含矽之膜時,其與2層光阻法相同般,可得到極適合加工之具有充分乾式蝕刻耐性之酚醛清漆膜之圖型。
如上述內容般,使用3層光阻法所使用之含矽之光阻中間膜,例如可使用CVD之含矽之無機膜,例如SiO2
膜(例如,專利文獻2:特開平7-183194號公報等)或SiON膜(例如,專利文獻3:特開平7-181688號公報等)、以迴轉塗佈方式製得膜之物,例如SOG(旋轉塗佈玻璃;spin-on-glass)膜(例如,專利文獻4:特開平5-291208號公報等、非專利文獻1:J.Appl.Polym.Sci.,Vol.88,636-
640(2003))或交聯性倍半矽氧烷膜(例如,專利文獻5:特表2005-520354號公報等)等,亦可使用聚矽烷膜(例如,專利文獻6:特開平11-60735號公報等)。其中,又以SiO2
膜或SiON膜具有對下層之有機膜進行乾式蝕刻之際,可作為乾式蝕刻遮罩之高性能膜,故需要特別之裝置進行成膜。相對於此,SOG膜或交聯性倍半矽氧烷膜、聚矽烷膜,僅需迴轉塗佈與加熱即可成膜,故推測其具有更高之製程效率。
多層光阻法之適用範圍,目前僅停留於嘗試提高光阻膜之解析界限之範圍中。如基板加工其中一個方法之比爾法斯特法般,其於加工中間體基板具有較大之高低差之情形中,於使用單一光阻膜形成圖型時,因光阻膜厚度具有較大之差距,故光阻曝光時會產生焦點無法正確地對齊等問題。該情形中,高低差則埋入犠牲膜使其平坦化後,於其上再形成光阻膜,以進行光阻圖型之形成時,此情形必然需使用上述多層光阻法(例如,專利文獻7:特開2004-349572號公報等)。
該些多層光阻法中,以往使用之含矽之膜中具有幾個問題。例如,欲以光微影蝕刻形成光阻圖型之情形,已知因曝光光被基板所反射,而與入射光產生干渉,而產生駐在波等問題,為得到不具有邊緣粗糙等光阻膜之微細圖型,中間膜必需置入抗反射膜。特別是最先端之高NA曝光條件中,控制反射為必要之條件。
因此,為控制反射,多層光阻法特別是於CVD中將含矽之膜形成為中間層之製程中,於光阻上層膜與含矽之中間膜之間必須置入有機抗反射膜。但是,置入有機抗反射膜時,因必須將光阻上層膜作為乾式蝕刻遮罩以對有機抗反射膜進行圖型加工,故於乾式蝕刻時,將光阻上層膜作為遮罩,以對抗反射膜進行乾式蝕刻加工後,再對含矽之中間層之加工。因此,就對抗反射膜加工部份而言,對上層光阻而言將會增加乾式蝕刻之負擔。特別是,最先端之光阻膜因膜厚變薄,故無法避免該乾式蝕刻之負荷。其中,如上所述般,一種不會產生上述般蝕刻負荷之將光吸收性含矽之膜作為中間膜使用之3層光阻法將受到極大之注目。
該些光吸收性含矽之中間膜,已知例如迴轉塗佈型之光吸收性含矽之中間膜。例如,具有使用芳香族構造作為光吸收構造之手法(專利文獻8:特開2005-15779號公報)。但是,可有效率吸收光之芳香環構造,其於使用氟系氣體電漿進行乾式蝕刻加工時,因會造成乾式蝕刻速度傾向降低等,故對於光阻膜不會增加負擔下對中間膜進行乾式蝕刻之方法為不利之方向。又,如此大量加入光吸收取代基為不佳狀態,因此,必須抑制至最低限之導入量。
此外,使用中間膜作為乾式蝕刻遮罩時,因對光阻下層膜進行加工之際,相對於一般所使用之氧氣體電漿所進行之反應性乾式蝕刻之乾式蝕刻速度,為提高中間膜與下層膜之蝕刻選擇比,而以越小越好,因此,相對於氟系蝕刻氣體,則極需要一種具有高反應性之高矽含量之中間膜。如此,相對於上層之光阻膜、下層之有機膜中任一膜之加工條件所要求之氟氣體而言,以反應性較高之成份、矽含量較高之中間膜為更佳。
但是,實際作為迴轉塗佈型含矽之中間膜形成用組成物中,為使含矽之化合物溶解於有機溶劑之方式作為有機取代基方式含有。以往已知之含矽之中間膜中,形成SOG膜之組成物,例如使用KrF準分子雷射光之微影蝕刻為揭示於非專利文獻1(J. Appl. Polym. Sci.,Vol. 88,636-640(2003))中。但是,該組成物中對於光吸收基因無任何相關敘述,故由該組成物所得到之含矽之膜可推想並不具有抗反射機能。因此,使用最先進之高NA曝光機進行微影蝕刻中,因無法抑制曝光時之反射,故極可能無法形成高精細之圖型形狀。
此外,使用上述高NA曝光機之最先進半導體製程中,因可大幅促進光阻之薄膜化,故將光阻作為蝕刻遮罩而對中間膜進行蝕刻之情形中,因具有抗反射機能且將矽含量提高時,推想也不容易將圖形轉印於含矽之中間膜上。因此,目前期待一種具有更快蝕刻速度之材料被推出。
除對於前述乾式蝕刻特性及抗反射效果之要求以外,其他例如為形成含矽率高之中間膜所使用之組成物中,特別會產生問題者為當該組成物之保存安定性。此時之保存安定性,係指組成物中所含之含矽之化合物之矽烷醇基是否會產生縮合,造成組成物之分子量產生變化之情形。產生變化時,將可由觀察膜厚變動或微影蝕刻性能之變動予以確認。特別是,微影蝕刻性能之變動因具有敏感性,故若無法由分子內之矽烷醇基產生縮合所造成之膜厚上昇或分子量變化之方式觀察時,亦可由高精細之圖型形狀的變化觀察而確認。
以往,將該些具有高反應性之矽烷醇基保存於酸性狀態下可得到比較安定化之效果,為記載於非專利文獻2(C.J.Brinker and G.W.Scherer,“Sol-Gel Science:The Physics and Chemistry of Sol-Gel Processing”,Academic Press,San Diego(1990))等。此外,非專利文獻1(J.Appl.Polym.Sci.,Vol.88,636-640(2003))、專利文獻9(特開2004-157469號公報)及專利文獻10(特開2004-191386號公報)等,也有揭示為提高保存安定性等目的而添加水等之方法。但是,依當該專利文獻所表示之方法所製造之含矽之化合物,即使進行前述方法時,實際上也無法完全停止矽烷醇基之縮合反應,其會伴隨時間之增長,而於組成物中之含矽之化合物緩緩變化,伴隨變化之組成物所製得之含矽之膜的性質也會產生變化。因此,目前必須將其冷凍或冷藏保存至使用之前,於使用之際再將其回復至使用溫度(通常為23℃),並必須儘速將其使用完畢。
[專利文獻1]特開平6-95385號公報
[專利文獻2]特開平7-183194號公報
[專利文獻3]特開平7-181688號公報
[專利文獻4]特開平5-291208號公報
[專利文獻5]特表2005-520354號公報
[專利文獻6]特開平11-60735號公報
[專利文獻7]特開2004-349572號公報
[專利文獻8]特開2005-15779號公報
[專利文獻9]特開2004-157469號公報
[專利文獻10]特開2004-191386號公報
[非專利文獻1]J. Appl. Polym. Sci., Vol. 88, 636-640(2003)
[非專利文獻2]C. J. Brinker and G. W. Scherer,“Sol-Gel Science:The Physics and Chemistry of Sol-Gel Processing”, Academic Press, San Diego(1990)
本發明之目的,為提供(1)於有機膜上所形成之含金屬氧化物膜上形成光阻膜,隨後形成光阻圖型之際,因含金屬氧化物膜因具有光吸收性能,故於高NA曝光條件下也可形成良好之圖型,(2)含金屬氧化物膜上層之光阻膜、下層之有機膜之間,形成可作為良好之乾式蝕刻遮罩使用之含金屬氧化物膜,(3)具有良好保存安定性之含金屬氧化物之膜形成用組成物,由該組成物所得之含金屬氧化物膜,由該含金屬氧化物膜所形成之基板,及圖型形成方法。
本發明者們,對於含金屬氧化物之中間膜形成用組成物之微影蝕刻特性或安定性進行深入研究結果,得知水解性矽化合物經過水解縮合所得之含金屬氧化物之化合物中,添加下述(B)成份、(C)成份及(D)成份時,確認
(1)於後述之導入光吸收性取代基時,無論於乾式、浸潤式中任一高NA曝光條件下,皆可抑制反射而得到含金屬氧化物膜,
(2)可得到作為乾式蝕刻遮罩之具有充分蝕刻選擇比之含金屬氧化物膜,
(3)可得到長期保持微影蝕刻性能,不會造成性能變化之含金屬氧化物之膜形成用組成物,
因而完成本發明。
即,本發明為提供一種熱硬化性含金屬氧化物之膜形成用組成物,其特徵為包含,
(A)通式(1)所表示之1種或2種以上的水解性矽化合物,與通式(2)所表示之1種或2種以上的水解性金屬化合物經水解縮合所得之含金屬氧化物之化合物,
R1 m1
R2 m2
R3 m3
Si(OR)(4-m1-m2-m3)
(1)
(式中,R為碳數1~6之烷基,R1
、R2
、R3
分別為氫原子,或碳數1~30之1價之有機基,m1、m2、m3為0或1;m1+m2+m3為0~3之整數)
U(OR4
)m4
(OR5
)m5
(2)
(式中,R4
、R5
為碳數1~30之有機基,m4+m5為依U的種類所決定之價數,m4、m5為0以上之整數,U為週期表之111族、IV族、或V族之元素,但為不含矽之元素)
(B)至少1種以上之下述通式(3)或(4)所表示之化合物,
La
Hb
X (3)
(式中,L為鋰、鈉、鉀、銣或銫,X為羥基,或碳數1~30之1價或2價以上之有機酸基,a為1以上之整數,b為0或1以上之整數,a+b為羥基或有機酸基之價數)
Ma
Hb
A (4)
(式中,M為鋶、碘鎓或銨,A為上述X或非親核性對向離子,a為1以上之整數,b為0或1以上之整數,a+b為羥基或有機酸基之價數)
(C)碳數為1~30之1價或2價以上之有機酸,
(D)有機溶劑
之熱硬化性含金屬氧化物之膜形成用組成物(申請專利範圍1)。
一般而言,水解性矽化合物及水解性金屬化合物(以下,兩者合稱為單體)於水解縮合觸媒存在下與水作用時,鍵結於單體之水解性取代基受到水解,而形成末端反應性基。該末端反應性基再與其他末端反應性基或未反應之水解性基進行縮合反應,而形成-SiOSi-鍵結、-SiOU-鍵結或-UOU-鍵結。隨後該反應依序重複發生,即形成所謂低聚物或聚合物,依情況不同亦有稱為凝膠之含金屬氧化物之化合物。此時,反應系内依水解縮合反應所生成之單體、低聚物、聚合物等所產生之末端反應性基中,由反應性最高之基依序進行縮合反應,而使單體、低聚物、聚合物等之末端反應性基消耗,而形成含金屬氧化物之化合物。隨後,此縮合反應持續進行,而有至最後之含金屬氧化物之化合物溶液形成凝膠化為止之情形。此時,多數情形為,最後之反應性較低之矽烷醇基則以末端反應性基形式殘留。
該末端矽烷醇基所具有之特定之pH中,具有可抑制縮合反應之情形,係揭示於非專利文獻2(C. J. Brinker and G. W. Scherer,“Sol-Gel Science:The Physics and Chemistry of Sol-Gel Processing”,Academic Press,San Diego(1990))等,特別是非專利文獻1(J. Appl. Polym. Sci.,Vol. 88,636-640(2003))中,則揭示pH為1.5左右(以下,稱為安定pH)可呈安定化之記載。
本發明中,使用(C)成份控制安定pH時,確認可提高保存安定性。
以往,多於300℃以上之高溫,或熱酸發生劑促使酸觸媒使含金屬氧化物之化合物硬化。本發明則於塗佈組成物進行加熱硬化之際,經由所添加之(B)成份之作用使末端矽烷醇基周邊之pH,由安定之pH轉變為不安定之pH區域(pH3附近,記載於非專利文獻2:C. J. Brinker and G. W. Scherer,“Sol-Gel Science:The Physics and Chemistry of Sol-Gel Processing”,Academic Press,San Diego(1990)),即可有效率地使含金屬氧化物膜硬化。即,使用與以往之溫度條件為相同之條件進行加熱硬化時,其可提供相較於以往之硬化膜為更具有交聯性之膜。因此,可使光阻膜中之有效成份向含金屬氧化物膜之移動受到抑制,而可得到具有與通常之有機抗反射膜相同程度之微影蝕刻特性。
如此,將pH控制、添加安定劑及添加交聯觸媒等技術組合時,可得到於室溫下具有安定性,硬化時可有效率的硬化之組成物,如此即可得到與以往之有機抗反射膜具有相同安定性之含金屬氧化物之抗反射膜形成用組成物。
本發明,提供一種含有由通式(5)所表示之1種或2種以上之水解性矽化合物經水解縮合所得之含矽之化合物(E)為特徵之如申請專利範圍1之熱硬化性含金屬氧化物之膜形成用組成物(申請專利範圍2)。
R6 m6
R7 m7
R8 m8
Si(OR9
)(4-m6-m7-m8)
(5)
(式中,R9
為碳數1~6之烷基,R6
、R7
、R8
分別為氫原子、或碳數1~30之1價之有機基,m6、m7、m8為0或1;m6+m7+m8為0~3之整數)。
本發明,經含有由含矽之單體的水解縮合反應所得之含矽之化合物,可與含金屬氧化物之化合物所具有之特性及含矽之化合物所具有之特性組合,而可得到具有超過以往有機抗反射膜之特性的含金屬氧化物之抗反射膜形成用組成物。
本發明,為提供一種含有將酸作為觸媒使用之由通式(1)及(2)之化合物經由水解縮合所得之含金屬氧化物之化合物為特徵之申請專利範圍1或2之熱硬化性含金屬氧化物之膜形成用組成物(申請專利範圍3)。
本發明,可得到將酸作為單體之水解縮合觸媒使用,而具有優良保存安定性,而具有與通常之有機抗反射膜相同程度之微影蝕刻特性的含金屬氧化物之抗反射膜形成用組成物。
本發明為提供一種酸觸媒,可使用由無機酸及磺酸衍生物所選出之1種以上之化合物作為酸觸媒使用為特徵之申請專利範圍3之熱硬化性含金屬氧化物之膜形成用組成物(申請專利範圍4)。
本發明,可使用無機酸及磺酸衍生物作為單體之水解縮合觸媒使用,而可得優良保存安定性,且具有與通常之有機抗反射膜相同程度之微影蝕刻特性的含金屬氧化物之抗反射膜形成用組成物。
本發明,為提供一種含有將水解縮合所得之含金屬氧化物之化合物的反應混合物經由實質上去除酸觸媒之步驟所得的含金屬氧化物之化合物為特徵之申請專利範圍3或4之熱硬化性含金屬氧化物之膜形成用組成物(申請專利範圍5)。
以往技術所製造之含金屬氧化物之化合物,其水解縮合時所使用之酸觸媒可於無須實際去除下,使用於塗佈膜形成用組成物。因此,組成物中因殘留縮合反應觸媒,故即使得到控制為安定pH之組成物時,也無法抑制矽烷醇基之縮合,而僅能得到保存安定性惡化之組成物。
本發明,因為於水解縮合中使用最佳之酸觸媒所得之含金屬氧化物之化合物,故實質上去除酸觸媒後,使用(C)成份也可提高保存安定性。
本發明,提供通式(2)之U為,硼、鋁、鎵、釔、鍺、鈦、鋯、鉿、鉍、錫、磷、釩、砷、銻、鈮,或鉭為特徵之申請專利範圍1~5中任一項之熱硬化性含金屬氧化物之膜形成用組成物(申請專利範圍6)。
上述內容中,含有以U表示之金屬之含金屬氧化物膜中,與不含U之含矽之膜相比較時,具有更快速之蝕刻速度,薄膜化之光阻作為蝕刻遮罩使用時,可形成具有圖型轉印功能之中間膜。
本發明,為提供一種通式(1)所表示之化合物與通式(2)所表示之化合物之莫耳比為(1)>(2)為特徵之中請專利範圍1~6中任一項之熱硬化性含金屬氧化物之膜形成用組成物(申請專利範圍7)。
上述內容中,矽含量多於以U表示之金屬時,使中間層作為蝕刻遮罩使用以對下層膜進行蝕刻之情形,可得到充分之蝕刻選擇比,可形成將圖型轉印於下層膜之中間膜。
本發明,為提供通式(4)之M為三級鋶、二級碘鎓或四級銨之申請專利範圍1~7中任一項之熱硬化性含金屬氧化物之膜形成用組成物(申請專利範圍8)。
(B)成份,於以使用通式(4)所表示之化合物所得之組成物形成硬化膜時,可提供進行交聯之膜。因此,使得光阻膜中之有效成份向含金屬氧化物膜之移動受到抑制,而可得到與通常之有機抗反射膜相同程度之微影蝕刻特性。
本發明,提供通式(4)之M為光分解性為特徵之申請專利範圍1~8中任一項之熱硬化性含金屬氧化物之膜形成用組成物(申請專利範圍9)。
(B)成份於加熱硬化時未全部揮發之情形,則含金屬氧化物膜中可能會殘留(B)成份。該成份,可能會造成光阻圖型形狀惡化。又,曝光時使用(B)成份之陽離子部份會產生分解之化合物時,則可防止曝光時之光阻圖型形狀的惡化。因此,可大幅提升含金屬氧化物之化合物的硬化性能,而可提供具有良好微影蝕刻形狀之含金屬氧化物之硬化膜。
本發明,提供一種更含有水之為特徵之申請專利範圍1~9中任一項之熱硬化性含金屬氧化物之膜形成用組成物(申請專利範圍10)。
添加水時,可使含金屬氧化物之化合物中之末端矽烷醇基活性化,於熱硬化反應可得到更緻密之膜。使用該緻密之膜時,可使上層之光阻層的微影蝕刻性能為一般有機抗反射膜之相同程度以上。
本發明,提供一種更含有光酸發生劑為特徵之申請專利範圍1~10中任一項之熱硬化性含金屬氧化物之膜形成用組成物(申請專利範圍11)。
(B)成份,於加熱硬化時或曝光時若不能完全揮發時,含金屬氧化物膜中所殘留之(B)成份將會有對圖型形狀產生影響之可能性。為防止該情形發生,於光阻圖型形成時,使含金屬氧化物膜中發生酸,則可防止光阻圖型形狀之惡化。
本發明,提供一種更含有具有以環狀醚作為取代基之1價或2價以上之醇為特徵之申請專利範圍1~11中任一項之熱硬化性含金屬氧化物之膜形成用組成物(申請專利範圍12)。
此外,對該含金屬氧化物之化合物中所含之末端矽烷醇基相互之縮合於室溫附近受到抑制部份,經過深入研究結果,得知將具有環狀醚作為取代基之1價或2價以上之醇作為安定劑添加時,於室溫附近之縮合則受到抑制,而使組成物之保存安定性大幅向上提升。
本發明,尚提供下述含金屬氧化物膜、基板及圖型形成方法。
提供一種於被加工基板上形成有機膜,於其上形成含金屬氧化物膜,再於其上使用由不含矽之化學増幅型光阻組成物形成光阻膜,對該光阻膜進行圖型加工後,使用該光阻膜圖型對含金屬氧化物膜進行圖型加工,將被加工之含金屬氧化物膜圖型作為蝕刻遮罩以對下層之有機膜進行圖型加工,再以被加工之有機膜作為蝕刻遮罩以對被加工基板進行蝕刻之多層光阻法中所使用之含金屬氧化物膜,係為申請專利範圍1~12中任一項之組成物所形成之含金屬氧化物膜(申請專利範圍13)。
提供一種化學増幅型光阻組成物所得之光阻膜與含金屬氧化物膜之間介有有機抗反射膜之申請專利範圍13之含金屬氧化物膜(申請專利範圍14)。
提供一種依序形成有機膜,與於該有機膜上由申請專利範圍1~12中任一項之組成物所形成之含金屬氧化物膜,與其上之光阻膜為特徵之基板(申請專利範圍15)。
提供一種含金屬氧化物膜與光阻膜之間介有有機抗反射膜為特徵之申請專利範圍15之基板(申請專利範圍16)。
提供上述有機膜為具有芳香族骨架之膜為特徵之申請專利範圍15或16之基板(申請專利範圍17)。
提供一種於基板上形成圖型之方法,其為準備申請專利範圍15之基板,使該基板之光阻膜的圖型電路區域曝光後,以顯影液顯影於光阻膜上形成光阻圖型,將該形成有光阻圖型之光阻膜作為蝕刻遮罩以對含金屬氧化物膜進行乾式蝕刻,以形成圖型之含金屬氧化物膜作為蝕刻遮罩蝕刻有機膜,以形成圖型之有機膜作為遮罩蝕刻基板,而於基板上形成圖型為特徵之圖型形成方法(申請專利範圍18)。
提供一種基板上形成圖型之方法,其為準備申請專利範圍16之基板,使該基板之光阻膜的圖型電路區域曝光後,以顯影液顯影於光阻膜上形成光阻圖型,將該形成有光阻圖型之光阻膜作為蝕刻遮罩以對有機抗反射膜及含金屬氧化物膜進行乾式蝕刻,以形成圖型之含金屬氧化物膜作為蝕刻遮罩蝕刻有機膜,以形成圖型之有機膜作為遮罩蝕刻基板,而於基板上形成圖型為特徵之圖型形成方法(申請專利範圍19)。
提供上述有機膜為具有芳香族骨架之膜為特徵之申請專利範圍18或19之圖型形成方法(申請專利範圍20)。
提供一種光阻圖型之形成,其為使用光微影蝕刻法,為使用波長300nm以下之光微影蝕刻法為特徵之申請專利範圍18、19或20之圖型形成方法(申請專利範圍21)。
使用本發明之中間膜或基板,以微影蝕刻於基板上形成圖型時,可於基板上以高精確度形成微細之圖型。此時,使用具有芳香族骨架之有機膜時,除於微影蝕刻步驟具有抗反射效果以外,於對基板進行蝕刻加工時,亦可得到具有充分耐蝕刻性之有機膜,而可進行蝕刻加工。本發明,於使用波長為300nm以下之光,特別是使用ArF準分子雷射之微影蝕刻形成圖型時,可以高精確度形成微細之圖型。
使用本發明之熱硬化性含金屬氧化物之膜形成用組成物所形成之含金屬氧化物之中間膜時,可使於其上所形成之光阻膜形成良好之圖型。又,與有機材料之間,因可得到高蝕刻選擇性,故可將所形成之光阻圖型,依含金屬氧化物之中間膜、有機下層膜之順序,以乾式蝕刻製程進行轉印。特別是半導體製程邁向微細化之過程中,因光阻之膜厚變薄,故將圖型轉印於以往之含矽之中間膜將變得更為困難,使用本發明之熱硬化性含金屬氧化物之膜形成用組成物時,因薄膜化之光阻亦可作為蝕刻遮罩使用,故可使光阻圖型以高精確性將圖型轉印於基板。又,可提供可抑制微影蝕刻後圖型缺陷之發生,而具有優良保存安定性之材料。
本發明之熱硬化性含金屬氧化物之膜形成用組成物中,本發明所使用之含金屬氧化物之化合物(A),為將單體水解縮合後製得。較佳之含金屬氧化物之化合物的製造方法,例如以下之方法等,但並非限定於該方法。
又,起始物質,可以下述通式(1)所表示。
R1 m1
R2 m2
R3 m3
Si(OR)(4-m1-m2-m3)
(1)
(式中,R為碳數1~6,特別是1~3之烷基;R1
、R2
、R3
分別為氫原子,或碳數1~30之1價之有機基;m1、m2、m3為0或1;m1+m2+m3為0~3之整數,特別是以0或1為佳)。
其中,有機基為含有碳之基之意,其可再含有氫,或 氮、氧、硫、矽等亦可。R1
、R2
、R3
之有機基,例如直鏈狀、分支狀、環狀之烷基,烯基、炔基、芳基、芳烷基等之無取代之1價烴基,及該些基之氫原子的1個或1個以上被環氧基、烷氧基、羥基等所取代之基,或介有-O-,-CO-,-OCO-,-COO-,-OCOO-之基等之後述通式(6)所表示之基,含矽-矽鍵結之有機基等。
通式(1)所表示之單體之R1
、R2
,R3
中較佳者為,氫原子、甲基、乙基、n-丙基、iso-丙基、n-丁基、iso-丁基、sec-丁基、t-丁基、n-戊基、2-乙基丁基、3-乙基丁基、2,2-二乙基丙基、環戊基、n-己基、環己基等之烷基,乙烯基、烯丙基等之烯基,乙炔基等之炔基,及作為光吸收性基之苯基、甲苯基等之芳基,苯甲基、苯乙基等之芳烷基。
例如、m1=0、m2=0、m3=0之四烷氧基矽烷,例如四甲氧基矽烷、四乙氧基矽烷、四-n-丙氧基矽烷、四-iso-丙氧基矽烷作為單體之例示。較佳為四甲氧基矽烷、四乙氧基矽烷。
例如,m1=1、m2=0、m3=0之三烷氧基矽烷,例如三甲氧基矽烷、三乙氧基矽烷、三-n-丙氧基矽烷、三-iso-丙氧基矽烷、甲基三甲氧基矽烷、甲基三乙氧基矽烷、甲基三-n-丙氧基矽烷、甲基三-iso-丙氧基矽烷、乙基三甲氧基矽烷、乙基三乙氧基矽烷、乙基三-n-丙氧基矽烷、乙基三-iso-丙氧基矽烷、乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、乙烯基三-n-丙氧基矽烷、乙烯基三-iso-丙氧基矽烷、n-丙基三甲氧基矽烷、n-丙基三乙氧基矽烷、n-丙基三-n-丙氧基矽烷、n-丙基三-iso-丙氧基矽烷、i-丙基三甲氧基矽烷、i-丙基三乙氧基矽烷、i-丙基三-n-丙氧基矽烷、i-丙基三-iso-丙氧基矽烷、n-丁基三甲氧基矽烷、n-丁基三乙氧基矽烷、n-丁基三-n丙氧基矽烷、n-丁基三-iso-丙氧基矽烷、sec-丁基三甲氧基矽烷、sec-丁基-三乙氧基矽烷、sec-丁基-三-n-丙氧基矽烷、sec-丁基-三-iso-丙氧基矽烷、t-丁基三甲氧基矽烷、t-丁基三乙氧基矽烷、t-丁基三-n丙氧基矽烷、t-丁基三-iso-丙氧基矽烷、環丙基三甲氧基矽烷、環丙基三乙氧基矽烷、環丙基-三-n-丙氧基矽烷、環丙基-三-iso-丙氧基矽烷、環丁基三甲氧基矽烷、環丁基三乙氧基矽烷、環丁基-三-n-丙氧基矽烷、環丁基-三-iso-丙氧基矽烷、環戊基三甲氧基矽烷、環戊基三乙氧基矽烷、環戊基-三-n-丙氧基矽烷、環戊基-三-iso-丙氧基矽烷、環己基三甲氧基矽烷、環己基三乙氧基矽烷、環己基-三-n-丙氧基矽烷、環己基-三-iso-丙氧基矽烷、環己烯基三甲氧基矽烷、環己烯基三乙氧基矽烷、環己烯基-三-n-丙氧基矽烷、環己烯基-三-iso-丙氧基矽烷、環己烯基乙基三甲氧基矽烷、環己烯基乙基三乙氧基矽烷、環己烯基乙基-三-n-丙氧基矽烷、環己烯基乙基三-iso-丙氧基矽烷、環辛烯基三甲氧基矽烷、環辛烯基三乙氧基矽烷、環辛烯基-三-n-丙氧基矽烷、環辛烯基-三-iso-丙氧基矽烷、環戊二烯基丙基三甲氧基矽烷、環戊二烯基丙基三乙氧基矽烷、環戊二烯基丙基-三-n-丙氧基矽烷、環戊二烯基丙基-三-iso-丙氧基矽烷、二環庚烯基三甲氧基矽烷、二環庚烯基三乙氧基矽烷、二環庚烯基-三-n-丙氧基矽烷、二環庚烯基-三-iso-丙氧基矽烷、二環庚基三甲氧基矽烷、二環庚基三乙氧基矽烷、二環庚基-三-n-丙氧基矽烷、二環庚基-三-iso-丙氧基矽烷、金剛烷基三甲氧基矽烷、金剛烷基三乙氧基矽烷、金剛烷基-三-n-丙氧基矽烷、金剛烷基-三-iso-丙氧基矽烷等。又,光吸收性單體,例如苯基三甲氧基矽烷、苯基三乙氧基矽烷、苯基三-n-丙氧基矽烷、苯基三-iso-丙氧基矽烷、苯甲基三甲氧基矽烷、苯甲基三乙氧基矽烷、苯甲基三-n-丙氧基矽烷、苯甲基三-iso-丙氧基矽烷、甲苯基三甲氧基矽烷、甲苯基三乙氧基矽烷、甲苯基三-n-丙氧基矽烷、甲苯基三-iso-丙氧基矽烷、苯乙基三甲氧基矽烷、苯乙基三乙氧基矽烷、苯乙基三-n-丙氧基矽烷、苯乙基三-iso-丙氧基矽烷、萘基三甲氧基矽烷、萘基三乙氧基矽烷、萘基三-n-丙氧基矽烷、萘基三-iso-丙氧基矽烷等。
較佳者為,甲基三甲氧基矽烷、甲基三乙氧基矽烷、乙基三甲氧基矽烷、乙基三乙氧基矽烷、乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、n-丙基三甲氧基矽烷、n-丙基三乙氧基矽烷、iso-丙基三甲氧基矽烷、iso-丙基三乙氧基矽烷、n-丁基三甲氧基矽烷、n-丁基三乙氧基矽烷、iso-丁基三甲氧基矽烷、iso-丁基三乙氧基矽烷、烯丙基三甲氧基矽烷、烯丙基三乙氧基矽烷、環戊基三甲氧基矽烷、環戊基三乙氧基矽烷、環己基三甲氧基矽烷、環己基三乙氧基矽烷、環己烯基三甲氧基矽烷、環己烯基三乙氧基矽烷、苯基三甲氧基矽烷、苯基三乙氧基矽烷、苯甲基三甲氧基矽烷、苯甲基三乙氧基矽烷、苯乙基三甲氧基矽烷、苯乙基三乙氧基矽烷。
例如,m1=1、m2=1、m3=0之二烷氧基矽烷,例如,二甲基二甲氧基矽烷、二甲基二乙氧基矽烷、甲基乙基二甲氧基矽烷、甲基乙基二乙氧基矽烷、二甲基-二-n-丙氧基矽烷、二甲基-二-iso-丙氧基矽烷、二乙基二甲氧基矽烷、二乙基二乙氧基矽烷、二乙基-二-n-丙氧基矽烷、二乙基-二-iso-丙氧基矽烷、二-n-丙基二甲氧基矽烷、二-n-丙基二乙氧基矽烷、二-n-丙基-二-n-丙氧基矽烷、二-n-丙基-二-iso-丙氧基矽烷、二-iso-丙基二甲氧基矽烷、二-iso-丙基二乙氧基矽烷、二-iso-丙基-二-n-丙氧基矽烷、二-iso-丙基-二-iso-丙氧基矽烷、二-n-丁基二甲氧基矽烷、二-n-丁基二乙氧基矽烷、二-n-丁基二-n-丙氧基矽烷、二-n-丁基-二-iso-丙氧基矽烷、二-sec-丁基二甲氧基矽烷、二-sec-丁基二乙氧基矽烷、二-sec-丁基-二-n-丙氧基矽烷、二-sec-丁基-二-iso-丙氧基矽烷、二-t-丁基二甲氧基矽烷、二-t-丁基二乙氧基矽烷、二-t-丁基-二-n-丙氧基矽烷、二-t-丁基-二-iso-丙氧基矽烷、二-環丙基二甲氧基矽烷、二-環丙基二乙氧基矽烷、二-環丙基-二-n-丙氧基矽烷、二-環丙基-二-iso-丙氧基矽烷、二-環丁基二甲氧基矽烷、二-環丁基二乙氧基矽烷、二-環丁基-二-n-丙氧基矽烷、二-環丁基-二-iso-丙氧基矽烷、二-環戊基二甲氧基矽烷、二-環戊基二乙氧基矽烷、二-環戊基-二-n-丙氧基矽烷、二-環戊基-二-iso-丙氧基矽烷、二-環己基二甲氧基矽烷、二-環己基二乙氧基矽烷、二-環己基-二-n-丙氧基矽烷、二-環己基-二-iso-丙氧基矽烷、二-環己烯基二甲氧基矽烷、二-環己烯基二乙氧基矽烷、二環己烯基-二-n-丙氧基矽烷、二-環己烯基-二-iso-丙氧基矽烷、二-環己烯基乙基二甲氧基矽烷、二-環己烯基乙基二乙氧基矽烷、二-環己烯基乙基-二-n-丙氧基矽烷、二-環己烯基乙基-二-iso-丙氧基矽烷、二-環辛烯基二甲氧基矽烷、二-環辛烯基二乙氧基矽烷、二環辛烯基-二-n-丙氧基矽烷、二-環辛烯基-二-iso-丙氧基矽烷、二-環戊二烯基丙基二甲氧基矽烷、二-環戊二烯基丙基二乙氧基矽烷、二-環戊二烯基丙基-二-n-丙氧基矽烷、二-環戊二烯基丙基-二-iso-丙氧基矽烷、雙-二環庚烯基二甲氧基矽烷、雙-二環庚烯基二乙氧基矽烷、雙-二環庚烯基-二-n-丙氧基矽烷、雙-二環庚烯基-二-iso-丙氧基矽烷、雙-二環庚基二甲氧基矽烷、雙-二環庚基二乙氧基矽烷、雙-二環庚基-二-n-丙氧基矽烷、雙-二環庚基-二-iso-丙氧基矽烷、雙-金剛烷基二甲氧基矽烷、雙-金剛烷基二乙氧基矽烷、雙-金剛烷基-二-n-丙氧基矽烷、雙-金剛烷基-二-iso-丙氧基矽烷等。又,光吸收性單體,例如,二苯基二甲氧基矽烷、二苯基-二-乙氧基矽烷、甲基苯基二甲氧基矽烷、甲基苯基二乙氧基矽烷、二苯基-二-n丙氧基矽烷、二苯基-二-iso
-丙氧基矽烷等。
較佳者為,二甲基二甲氧基矽烷、二甲基二乙氧基矽烷、二乙基二甲氧基矽烷、二乙基二乙氧基矽烷、甲基乙基二甲氧基矽烷、甲基乙基二乙氧基矽烷、二-n-丙基-二-甲氧基矽烷、二-n-丁基二-甲氧基矽烷、甲基苯基二甲氧基矽烷、甲基苯基二乙氧基矽烷等。
例如,m1=1、m2=1、m3=1之單烷氧基矽烷,例如三甲基甲氧基矽烷、三甲基乙氧基矽烷、二甲基乙基甲氧基矽烷、二甲基乙基乙氧基矽烷等。又,光吸收性單體,例如二甲基苯基甲氧基矽烷、二甲基苯基乙氧基矽烷、二甲基苯甲基甲氧基矽烷、二甲基苯甲基乙氧基矽烷、二甲基苯乙基甲氧基矽烷、二甲基苯乙基乙氧基矽烷等。
較佳為,三甲基甲氧基矽烷、二甲基乙基甲氧基矽烷、二甲基苯基甲氧基矽烷、二甲基苯甲基甲氧基矽烷、二甲基苯乙基甲氧基矽烷等。
上述R1
、R2
、R3
所表示之有機基之其他例示,例如具有1個以上之碳-氧單鍵或碳-氧雙鍵之有機基等。具體而言,例如,具有由環氧基、酯基、烷氧基、羥基所成群中所選擇之1個以上之基的有機基。通式(1)中之具有1個以上之碳-氧單鍵、碳-氧雙鍵的有機基,例如,下述通式(6)所表示之基等。
(P-Q1
-(S1
)v1
-Q2
-)u
-(T)v2
-Q3
-(S2
)v3
-Q4
- (6)
(上述式中,P為氫原子、羥基、
碳數1~4之烷氧基、碳數1~6之烷基羰氧基、或碳數1~6之烷基羰基,Q1
與Q2
與Q3
與Q4
為分別獨立之-Cq
H(2q-p
)Pp
-(式中,P係與上述為相同之內容,p為0~3之整數,q為0~10之整數(其中,q=0為表示單鍵之情形)),u為0~3之整數,S1
與S2
為分別獨立之-O-、-CO-、-OCO-、-COO-或-OCOO-。v1、v2、v3分別獨立表示0或1。與其同時,T為可含有雜原子之脂環或芳香環所形成之2價之基,T之可含有氧原子等之雜原子之脂環或芳香環之例示,係如以下所示。T中,Q2
與Q3
鍵結之位置,並未有特別限定,其可於於考慮立體性之因素所造成之反應性,或反應所使用之市售藥劑取得之容易性等作適當之選擇)。
通式(5)中之具有1個以上碳-氧單鍵或碳-氧雙鍵之有機基的較佳例示,例如以下所列舉之內容。又,下述式中,(Si)為表示與Si鍵結之處所記載者。
又,R1
、R2
、R3
之有機基之例示,例如可使用含有矽-矽鍵結之有機基。具體而言,例如下述所列舉之內容。
其他之起始物質,可以下述通式(2)所表示。
U(OR4
)m4
(OR5
)m5
(2)
(式中,R4
、R5
為碳數1~30之有機基,m4+m5為依U的種類所決定之價數,m4、m5為0以上之整數,U為週期表之III族、IV族、或V族之元素,且為不含矽之元素)。
其中,有機基為表示含有碳之基之意,其可再含有氫,或可含有氮、氧、硫、矽等。R4
、R5
,例如可為直鏈狀、分支狀、環狀之烷基、烯基、炔基、芳基、芳烷基等之無取代的1價烴基,及該些之基的氫原子的1個或1個以上被環氧基、烷氧基、羥基等所取代之基,或介有-O-,-CO-,-OCO-,-COO-,-OCOO-之基等。
U為硼之情形,式(2)所表示之化合物,例如甲氧基硼、乙氧基硼、丙氧基硼、丁氧基硼、戊氧基硼、己氧基硼、環戊氧基硼、環己氧基硼、烯丙氧基硼、苯氧基硼、甲氧基乙氧基硼等單體。
U為鋁之情形,式(2)所表示之化合物,例如甲氧基鋁、乙氧基鋁、丙氧基鋁、丁氧基鋁、戊氧基鋁、己氧基鋁、環戊氧基鋁、環己氧基鋁、烯丙氧基鋁、苯氧基鋁、甲氧基乙氧基鋁、乙氧基乙氧基鋁、二丙氧基乙基乙醯乙酸基鋁、二丁氧基乙基乙醯乙酸基鋁、丙氧基雙乙基乙醯乙酸基鋁、丁氧基雙乙基乙醯乙酸基鋁、2,4-戊二酮酸鋁、2,2,6,6-四甲基-3,5-庚二酮酸鋁等單體。
U為鎵之情形,式(2)所表示之化合物,例如甲氧基鎵、乙氧基鎵、丙氧基鎵、丁氧基鎵、戊氧基鎵、己氧基鎵、環戊氧基鎵、環己氧基鎵、烯丙氧基鎵、苯氧基鎵、甲氧基乙氧基鎵、乙氧基乙氧基鎵、二丙氧基乙基乙醯乙酸基鎵、二丁氧基乙基乙醯乙酸基鎵、丙氧基雙乙基乙醯乙酸基鎵、丁氧基雙乙基乙醯乙酸基鎵、2,4-戊二酮酸鎵、2,2,6,6-四甲基-3,5-庚二酮酸鎵等單體。
U為釔之情形,式(2)所表示之化合物,例如甲氧基釔、乙氧基釔、丙氧基釔、丁氧基釔、戊氧基釔、己氧基釔、環戊氧基釔、環己氧基釔、烯丙氧基釔、苯氧基釔、甲氧基乙氧基釔、乙氧基乙氧基釔、二丙氧基乙基乙醯乙酸基釔、二丁氧基乙基乙醯乙酸基釔、丙氧基雙乙基乙醯乙酸基釔、丁氧基雙乙基乙醯乙酸基釔、2,4-戊二酮酸釔、2,2,6,6-四甲基-3,5-庚二酮酸釔等單體。
U為鍺之情形,式(2)所表示之化合物,例如甲氧基鍺、乙氧基鍺、丙氧基鍺、丁氧基鍺、戊氧基鍺、己氧基鍺、環戊氧基鍺、環己氧基鍺、烯丙氧基鍺、苯氧基鍺、甲氧基乙氧基鍺、乙氧基乙氧基鍺等單體。
U為鈦之情形,式(2)所表示之化合物,例如甲氧基鈦、乙氧基鈦、丙氧基鈦、丁氧基鈦、戊氧基鈦、己氧基鈦、環戊氧基鈦、環己氧基鈦、烯丙氧基鈦、苯氧基鈦、甲氧基乙氧基鈦、乙氧基乙氧基鈦、二丙氧基雙乙基乙醯乙酸基鈦、二丁氧基雙乙基乙醯乙酸基鈦、二丙氧基雙2,4-戊二酮酸鈦、二丁氧基雙2,4-戊二酮酸鈦等單體。
U為鉿之情形,式(2)所表示之化合物,例如甲氧基鉿、乙氧基鉿、丙氧基鉿、丁氧基鉿、戊氧基鉿、己氧基鉿、環戊氧基鉿、環己氧基鉿、烯丙氧基鉿、苯氧基鉿、甲氧基乙氧基鉿、乙氧基乙氧基鉿、二丙氧基雙乙基乙醯乙酸基鉿、二丁氧基雙乙基乙醯乙酸基鉿、二丙氧基雙2,4-戊二酮酸鉿、二丁氧基雙2,4-戊二酮酸鉿等單體。
U為錫之情形,式(2)所表示之化合物,例如甲氧基錫、乙氧基錫、丙氧基錫、丁氧基錫、苯氧基錫、甲氧基乙氧基錫、乙氧基乙氧基錫、2,4-戊二酮酸錫、2,2,6,6-四甲基-3,5-庚二酮酸錫等單體。
U為砷之情形,式(2)所表示之化合物,例如甲氧基砷、乙氧基砷、丙氧基砷、丁氧基砷、苯氧基砷等單體。
U為銻之情形,式(2)所表示之化合物,例如甲氧基銻、乙氧基銻、丙氧基銻、丁氧基銻、苯氧基銻、乙酸銻、丙酸銻等單體。
U為鈮之情形,式(2)所表示之化合物,例如甲氧基鈮、乙氧基鈮、丙氧基鈮、丁氧基鈮、苯氧基鈮等單體。
U為鉭之情形,式(2)所表示之化合物,例如甲氧基鉭、乙氧基鉭、丙氧基鉭、丁氧基鉭、苯氧基鉭等單體。
U為鉍之情形,式(2)所表示之化合物,例如甲氧基鉍、乙氧基鉍、丙氧基鉍、丁氧基鉍、苯氧基鉍等單體。
U為磷之情形,式(2)所表示之化合物,例如三甲基亞磷酸鹽、三乙基亞磷酸鹽、三丙基亞磷酸鹽、三甲基磷酸鹽、三乙基磷酸鹽、三丙基磷酸鹽等單體。
U為釩之情形,式(2)所表示之化合物,例如雙(2,4-戊二酮酸)釩氧化物、2,4-戊二酮酸釩、三丁氧基釩氧化物、三丙氧基釩氧化物等單體。
U為鋯之情形,式(2)所表示之化合物,例如甲氧基鋯、乙氧基鋯、丙氧基鋯、丁氧基鋯、苯氧基鋯、二丁氧基雙(2,4-戊二酮酸)鋯、二丙氧基雙(2,2,6,6-四甲基-3,5-庚二酮酸)鋯等單體。
U為鉭之情形,式(2)所表示之化合物,例如甲氧基鉭、乙氧基鉭、丙氧基鉭、丁氧基鉭、苯氧基鉭等單體。
亦可由該些單體選擇1種或2種以上之通式(1)所表示之單體,1種或2種以上通式(2)所表示之單體,於反應前或反應中混合以形成含金屬氧化物之化合物,作為反應原料。
含金屬氧化物之化合物,以由式(1)及式(2)之單體,較佳為配合無機酸、脂肪族磺酸及芳香族磺酸所選出之一種以上之化合物作為酸觸媒使用,再進行水解縮合之方式即可製造。
此時所使用之酸觸媒,例如氟酸、鹽酸、溴化氫酸、硫酸、硝酸、過氯酸、磷酸、甲烷磺酸、苯磺酸、甲苯磺酸等。觸媒之使用量,對矽單體1莫耳為10-6
~10莫耳,較佳為10-5
~5莫耳,更佳為10-4
~1莫耳。
該些單體經由水解縮合以製得含金屬氧化物之化合物時之水量,以鍵結於單體之水解性取代基1莫耳添加0.01~100莫耳,更佳為0.05~50莫耳,最佳為0.1~30莫耳為宜。添加超過100莫耳時,造成反應所使用之裝置過大,而為不具經濟性。
操作方法,例如於觸媒水溶液中添加單體,以開始進行水解縮合反應。此時,可於觸媒水溶液中加入有機溶劑亦可,或將單體稀釋於有機溶劑中亦可,或兩者皆可。反應溫度為0~100℃,較佳為5~80℃。以單體滴下時保持5~80℃之溫度,其後再於20~80℃下熟成之方法為佳。
可加入觸媒水溶液,或可稀釋單體之有機溶劑,例如以,甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-1-丙醇、丙酮、乙腈、四氫呋喃、甲苯、己烷、乙酸乙酯、環己酮、甲基-2-n-戊酮、丁二醇單甲基醚、丙二醇單甲基醚、乙二醇單甲基醚、丁二醇單乙基醚、丙二醇單乙基醚、乙二醇單乙基醚、丙二醇二甲基醚、二乙二醇二甲基醚、丙二醇單甲基醚乙酸酯、丙二醇單乙基醚乙酸酯、丙酮酸乙酯、乙酸丁酯、3-甲氧基丙酸甲酯、3-乙氧基丙酸乙酯、乙酸tert-丁酯、丙酸tert-丁酯、丙二醇單tert-丁基醚乙酸酯、γ-丁內酯及其混合物等為佳。
該些溶劑中較佳者為具有水可溶性之溶劑。例如,甲醇、乙醇、1-丙醇、2-丙醇等之醇類,乙二醇、丙二醇等之多元醇,丁二醇單甲基醚、丙二醇單甲基醚、乙二醇單甲基醚、丁二醇單乙基醚、丙二醇單乙基醚、乙二醇單乙基醚、丁二醇單丙基醚、丙二醇單丙基醚、乙二醇單丙基醚等多元醇縮合物衍生物,丙酮、乙腈、四氫呋喃等。其中,特佳者為,沸點為100℃以下者。
又,有機溶劑之使用量,相對於單體1莫耳為0~1,000ml,特別是以0~500ml為佳。有機溶劑之使用量過多時,將造成反應容器過大,而不具經濟性。
其後,必要時可進行觸媒之中和反應,將水解縮合反應所生成之醇減壓去除,而得反應混合物水溶液。此時,可作為中和使用之鹼性物質之量,以對觸媒所使用之酸為0.1~2當量為佳。只要該鹼性物質於水中可顯示出鹼性性質者,可使用任意之物質。
隨後,以將水解縮合反應所生成之醇等副產物由反應混合物中去除為佳。此時將反應混合物加熱之溫度,依所添加之有機溶劑與反應所發生之醇等之種類而有所不同,較佳為0~100℃,更佳為10~90℃,最佳為15~80℃。又,此時之減壓度,依需去除之有機溶劑及醇等之種類、排氣裝置、凝縮裝置及加熱溫度而有所不同,較佳為大氣壓以下,更佳為絕對壓為80kPa以下,最佳為絕對壓為50kPa以下。雖無法正確得知此時所去除之醇量,但以去除所生成之醇等的約80質量%以上者為佳。
其次,亦可將水解縮合所使用之酸觸媒由反應混合物中去除。去除酸觸媒之方法,例如將水與含金屬氧化物之化合物混合,再由含金屬氧化物之化合物以有機溶劑萃取。此時所使用之有機溶劑,以可溶解含金屬氧化物之化合物,且與水混合時,可形成2層分離有機溶劑為佳。例如甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-1-丙醇、丙酮、四氫呋喃、甲苯、己烷、乙酸乙酯、環己酮、甲基-2-n-戊酮、丁二醇單甲基醚、丙二醇單甲基醚、乙二醇單甲基醚、丁二醇單乙基醚、丙二醇單乙基醚、乙二醇單乙基醚、丁二醇單丙基醚、丙二醇單丙基醚、乙二醇單丙基醚、丙二醇二甲基醚、二乙二醇二甲基醚、丙二醇單甲基醚乙酸酯、丙二醇單乙基醚乙酸酯、丙酮酸乙酯、乙酸丁酯、3-甲氧基丙酸甲酯、3-乙氧基丙酸乙酯、乙酸tert-丁酯、丙酸tert-丁酯、丙二醇單tert-丁基醚乙酸酯、γ-丁內酯、甲基異丁酮、環戊基甲基醚等,及其混合物等。
此外,亦可使用水溶性有機溶劑與水難溶性有機溶劑之混合物。例如甲醇+乙酸乙酯、乙醇+乙酸乙酯、1-丙醇+乙酸乙酯、2-丙醇+乙酸乙酯、丁二醇單甲基醚+乙酸乙酯、丙二醇單甲基醚+乙酸乙酯、乙二醇單甲基醚、丁二醇單乙基醚+乙酸乙酯、丙二醇單乙基醚+乙酸乙酯、乙二醇單乙基醚+乙酸乙酯、丁二醇單丙基醚+乙酸乙酯、丙二醇單丙基醚+乙酸乙酯、乙二醇單丙基醚+乙酸乙酯、甲醇+甲基異丁酮、乙醇+甲基異丁酮、1-丙醇+甲基異丁酮、2-丙醇+甲基異丁酮、丙二醇單甲基醚+甲基異丁酮、乙二醇單甲基醚、丙二醇單乙基醚+甲基異丁酮、乙二醇單乙基醚+甲基異丁酮、丙二醇單丙基醚+甲基異丁酮、乙二醇單丙基醚+甲基異丁酮、甲醇+環戊基甲基醚、乙醇+環戊基甲基醚、1-丙醇+環戊基甲基醚、2-丙醇+環戊基甲基醚、丙二醇單甲基醚+環戊基甲基醚、乙二醇單甲基醚+環戊基甲基醚、丙二醇單乙基醚+環戊基甲基醚、乙二醇單乙基醚+環戊基甲基醚、丙二醇單丙基醚+環戊基甲基醚、乙二醇單丙基醚+環戊基甲基醚、甲醇+丙二醇甲基醚乙酸酯、乙醇+丙二醇甲基醚乙酸酯、1-丙醇+丙二醇甲基醚乙酸酯、2-丙醇+丙二醇甲基醚乙酸酯、丙二醇單甲基醚+丙二醇甲基醚乙酸酯、乙二醇單甲基醚+丙二醇甲基醚乙酸酯、丙二醇單乙基醚+丙二醇甲基醚乙酸酯、乙二醇單乙基醚+丙二醇甲基醚乙酸酯、丙二醇單丙基醚+丙二醇甲基醚乙酸酯、乙二醇單丙基醚+丙二醇甲基醚乙酸酯等組合者為佳,但組合內容並不僅限定於前述內容。
又,一般可適當選擇水溶性有機溶劑與水難溶性有機溶劑之混合比例,但以相對於水難溶性有機溶劑100質量份,水溶性有機溶劑為使用0.1~1,000質量份,較佳為1~500質量份,更佳為2~100質量份。
隨後,使用中性水進行洗淨。該水,一般為使用通常稱為去離子水或超純水之水即可。該水之量,相對於含金屬氧化物之化合物溶液1L,為使用0.01~100L,較佳為0.05~50L,更佳為0.1~5L。其洗淨之方法,例如將兩者放置於同一容器中攪拌混合後,靜置使水層分離即可。洗淨次數,以1次以上即可,即使洗淨10次以上時,也僅能得到洗淨之效果而已,故較佳以1~5次左右為佳。
去除其他酸觸媒之方法,例如可使用離子交換樹脂之方法,或環氧乙烷、環氧丙烷等環氧化合物中和後予以去除之方法等。該些方法,可配合反應所使用之酸觸媒做適當之選擇亦可。
又,於去除上述觸媒之操作中,該酸觸媒為實際上被去除之意,係指其殘留量為相對於反應所使用之酸觸媒於含金屬氧化物之化合物於反應開始時所添加之量的10質量%以下,較佳為5質量%以下之意。
此時經由水洗操作,可使含金屬氧化物之化合物中之一部份移至水層,而可得到實質上與區分操作為相同效果之情形,故可依據水洗次數或洗淨水之量所得之觸媒去除效果與區分效果做適當之選擇即可。
無論殘留有酸觸媒之含金屬氧化物之化合物,及去除酸觸媒所得之含金屬氧化物之化合物溶液中,加入最後之溶劑,於減壓進行溶劑交換而可得含金屬氧化物之化合物溶液。此時之溶劑交換的溫度,依所應去除之反應溶劑或萃取溶劑之種類而有所不同,一般較佳為0~100℃,更佳為10~90℃,最佳為15~80℃。又,此時之減壓度,依所欲除之萃取溶劑之種類、排氣裝置、凝縮裝置及加熱溫度而有所不同,較佳為大氣壓以下,更佳為絕對壓為80kPa以下,更佳為絕對壓為50kPa以下。
此時,若改變溶劑時將會造成含金屬氧化物之化合物不安定之情形。其乃因最後的溶劑與含金屬氧化物之化合物之相性而發生,為防止該情形,可添加後述作為安定劑之(C)成份。添加量,相對於溶劑交換前之溶液中的含金屬氧化物之化合物100質量份為0~25質量份,較佳為0~15質量份,更佳為0~5質量份,添加之情形中,以添加0.5質量份以上為佳。溶劑交換前之溶液若有必要時,可添加(C)成份進行溶劑交換操作即可。
含金屬氧化物之化合物,於濃縮至某特定濃度以上時,則開始進行縮合反應,而變化為對有機溶劑不可能再溶解之狀態。因此,以適當濃度之溶液狀態下放置為佳。又,過於稀薄時,因溶劑之量過大而不具經濟性。此時之濃度以0.1~20質量%為佳。
含金屬氧化物之化合物溶液中所添加之最後的溶劑中,較佳者為醇系溶劑,特佳者為乙二醇、二乙二醇、三乙二醇、丙二醇、二丙二醇、丁二醇等之單烷基醚衍生物。具體而言,例如,丁二醇單甲基醚、丙二醇單甲基醚、乙二醇單甲基醚、丁二醇單乙基醚、丙二醇單乙基醚、乙二醇單乙基醚、丁二醇單丙基醚、丙二醇單丙基醚、乙二醇單丙基醚等為佳。
又,其他反應操作,例如於單體或單體之有機溶液中,添加水或含水有機溶劑,使其開始水解反應。此時,觸媒可添加於單體或單體之有機溶液中亦可,或添加於水或含水有機溶劑中亦可。反應溫度為0~100℃,較佳為10~80℃。又以滴下水時加熱至10~50℃,其後升溫至20~80℃以使其熟成之方法為佳。
使用有機溶劑之情形,以使用水溶性者為佳,例如甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-1-丙醇、丙酮、四氫呋喃、乙腈、丁二醇單甲基醚、丙二醇單甲基醚、乙二醇單甲基醚、丁二醇單乙基醚、丙二醇單乙基醚、乙二醇單乙基醚、丁二醇單丙基醚、丙二醇單丙基醚、乙二醇單丙基醚、丙二醇二甲基醚、二乙二醇二甲基醚、丙二醇單甲基醚乙酸酯、丙二醇單乙基醚乙酸酯、丙二醇單丙基醚等多元醇縮合物衍生物及其之混合物等。
有機溶劑之使用量,可與前述之量為相同即可。所得反應混合物之後處理,與前述之方法相同般進行後處理,而製得含金屬氧化物之化合物。
所得合金屬氧化物之化合物之分子量,除可選擇單體以外,亦可由聚合時反應條件之控制進行調整,重量平均分子量使用超過100,000以上時,依情況之不同,而會有發生異物或產生塗佈斑等情形,一般以使用100,000以下,更佳為200~50,000,最佳為使用300~30,000者為佳。又,上述重量平均分子量之數據,為使用RI作為檢測器之凝膠滲透色層分析法(GPC),標準物質使用聚苯乙烯,並以聚苯乙烯換算所得分子量表示者。
本發明之含金屬氧化物之膜形成用組成物,若於酸性條件下所製造之組成物時,其可含有2種以上組成及/或反應條件相異之含金屬氧化物之化合物。
本發明中,上述含金屬氧化物之化合物(A)中,可再添加熱交聯促進劑(B)、酸(C)及有機溶劑(D)以製得含金屬氧化物之膜形成用組成物。
本發明中,為更促進含金屬氧化物膜形成時之交聯反應,可使其含有(B)成份之熱交聯促進劑。前述成分,可列舉例如通式(3)或(4)所表示之化合物等。
La
Hb
X (3)
(式中,L為鋰、鈉、鉀、銣或銫,X為羥基,或碳數1~30之1價或2價以上之有機酸基,a為1以上之整數,b為0或1以上之整數,又,a+b為羥基或有機酸基之價數)。
Ma
Hb
A (4)
(式中,M為鋶、碘鎓或銨,較佳為三級鋶、二級碘鎓或四級銨,特別是以光分解性之物質,即,三芳基鋶化合物、二芳基碘鎓化合物為佳。A為上述X或非親核性對向離子,a、b係與上述為相同之內容)。
通式(3)所表示之化合物,例如鹼金屬有機酸鹽。例如,鋰、鈉、鉀、銣、銫之氫氧酸鹽、甲酸鹽、乙酸鹽、丙酸鹽、丁酸鹽、戊酸鹽、己酸鹽、庚酸鹽、辛酸鹽、壬酸鹽、癸酸鹽、油酸鹽、硬脂酸鹽、亞油酸鹽、亞麻酸鹽、苯甲酸鹽、苯二甲酸鹽、間苯二甲酸鹽、對苯二甲酸鹽、水楊酸鹽、三氟乙酸鹽、單氯乙酸鹽、二氯乙酸鹽、三氯乙酸鹽等1價之鹽、1價或2價之草酸鹽、丙二酸鹽、甲基丙二酸鹽、乙基丙二酸鹽、丙基丙二酸鹽、丁基丙二酸鹽、二甲基丙二酸鹽、二乙基丙二酸鹽、丁二酸鹽、甲基丁二酸鹽、戊二酸鹽、己二酸鹽、依康酸鹽、馬來酸鹽、富馬酸鹽、檸康酸鹽、檸檬酸鹽、碳酸鹽等。
具體而言,例如,甲酸鋰、乙酸鋰、丙酸鋰、丁酸鋰、戊酸鋰、己酸鋰、庚酸鋰、辛酸鋰、壬酸鋰、癸酸鋰、油酸鋰、硬脂酸鋰、亞油酸鋰、亞麻酸鋰、苯甲酸鋰、苯二甲酸鋰、間苯二甲酸鋰、對苯二甲酸鋰、水楊酸鋰、三氟乙酸鋰、單氯乙酸鋰、二氯乙酸鋰、三氯乙酸鋰、氫氧化鋰、草酸氫鋰、丙二酸氫鋰、甲基丙二酸氫鋰、乙基丙二酸氫鋰、丙基丙二酸氫鋰、丁基丙二酸氫鋰、二甲基丙二酸氫鋰、二乙基丙二酸氫鋰、丁二酸氫鋰、甲基丁二酸氫鋰、戊二酸氫鋰、己二酸氫鋰、依康酸氫鋰、馬來酸氫鋰、富馬酸氫鋰、檸康酸氫鋰、檸檬酸氫鋰、碳酸氫鋰、草酸鋰、丙二酸鋰、甲基丙二酸鋰、乙基丙二酸鋰、丙基丙二酸鋰、丁基丙二酸鋰、二甲基丙二酸鋰、二乙基丙二酸鋰、丁二酸鋰、甲基丁二酸鋰、戊二酸鋰、己二酸鋰、依康酸鋰、馬來酸鋰、富馬酸鋰、檸康酸鋰、檸檬酸鋰、碳酸鋰、甲酸鈉、乙酸鈉、丙酸鈉、丁酸鈉、戊酸鈉、己酸鈉、庚酸鈉、辛酸鈉、壬酸鈉、癸酸鈉、油酸鈉、硬脂酸鈉、亞油酸鈉、亞麻酸鈉、苯甲酸鈉、苯二甲酸鈉、間苯二甲酸鈉、對苯二甲酸鈉、水楊酸鈉、三氟乙酸鈉、單氯乙酸鈉、二氯乙酸鈉、三氯乙酸鈉、氫氧化鈉、草酸氫鈉、丙二酸氫鈉、甲基丙二酸氫鈉、乙基丙二酸氫鈉、丙基丙二酸氫鈉、丁基丙二酸氫鈉、二甲基丙二酸氫鈉、二乙基丙二酸氫鈉、丁二酸氫鈉、甲基丁二酸氫鈉、戊二酸氫鈉、己二酸氫鈉、依康酸氫鈉、馬來酸氫鈉、富馬酸氫鈉、檸康酸氫鈉、檸檬酸氫鈉、碳酸氫鈉、草酸鈉、丙二酸鈉、甲基丙二酸鈉、乙基丙二酸鈉、丙基丙二酸鈉、丁基丙二酸鈉、二甲基丙二酸鈉、二乙基丙二酸鈉、丁二酸鈉、甲基丁二酸鈉、戊二酸鈉、己二酸鈉、依康酸鈉、馬來酸鈉、富馬酸鈉、檸康酸鈉、檸檬酸鈉、碳酸鈉、甲酸鉀、乙酸鉀、丙酸鉀、丁酸鉀、戊酸鉀、己酸鉀、庚酸鉀、辛酸鉀、壬酸鉀、癸酸鉀、油酸鉀、硬脂酸鉀、亞油酸鉀、亞麻酸鉀、苯甲酸鉀、苯二甲酸鉀、間苯二甲酸鉀、對苯二甲酸鉀、水楊酸鉀、三氟乙酸鉀、單氯乙酸鉀、二氯乙酸鉀、三氯乙酸鉀、氫氧化鉀、草酸氫鉀、丙二酸氫鉀、甲基丙二酸氫鉀、乙基丙二酸氫鉀、丙基丙二酸氫鉀、丁基丙二酸氫鉀、二甲基丙二酸氫鉀、二乙基丙二酸氫鉀、丁二酸氫鉀、甲基丁二酸氫鉀、戊二酸氫鉀、己二酸氫鉀、依康酸氫鉀、馬來酸氫鉀、富馬酸氫鉀、檸康酸氫鉀、檸檬酸氫鉀、碳酸氫鉀、草酸鉀、丙二酸鉀、甲基丙二酸鉀、乙基丙二酸鉀、丙基丙二酸鉀、丁基丙二酸鉀、二甲基丙二酸鉀、二乙基丙二酸鉀、丁二酸鉀、甲基丁二酸鉀、戊二酸鉀、己二酸鉀、依康酸鉀、馬來酸鉀、富馬酸鉀、檸康酸鉀、檸檬酸鉀、碳酸鉀等例示。
通式(4)所表示之化合物,可列舉例如(Q-1)、(Q-2)及(Q-3)所表示之鋶化合物、碘鎓化合物、銨化合物等。
(式中,R204
、R205
、R206
分別為碳數1~12之直鏈狀、分支狀或環狀之烷基、烯基、酮烷基或酮烯基、碳數6~20之取代或無取代之芳基,或碳數7~12之芳烷基或芳基酮烷基,該些基之氫原子的一部份或全部可被烷氧基等所取代;又,R205
與R206
可與其鍵結之硫原子共同形成環亦可,形成環時,R205
、R206
分別表示碳數1~6之伸烷基;A-
為非親核性對向離子;R207
、R208
、R209
、R210
,與R204
、R205
、R206
相同般,其亦可為氫原子;R207
與R208
、R207
與R208
與R209
可與其鍵結之氮原子共同形成環亦可,形成環時,R207
與R208
及R207
與R208
與R209
表示碳數3~10之伸烷基)。
上述R204
、R205
、R206
、R207
、R208
、R209
、R210
可相互為相同或相異皆可,具體而言,烷基例如,甲基、乙基、丙基、異丙基、n-丁基、sec-丁基、tert-丁基、戊基、己基、庚基、辛基、環戊基、環己基、環庚基、環丙基甲基、4-甲基環己基、環己基甲基、降冰片烷基、金剛烷基等。烯基例如,乙烯基、烯丙基、丙烯基、丁烯基、己烯基、環己烯基等。酮烷基例如,2-酮基環戊基、2-酮基環己基等,2-酮基丙基、2-環戊基-2-酮基乙基、2-環己基-2-酮基乙基、2-(4-甲基環己基)-2-酮基乙基等。芳基例如,苯基、萘基等,或p-甲氧基苯基、m-甲氧基苯基、o-甲氧基苯基、乙氧基苯基、p-tert-丁氧基苯基、m-tert-丁氧基苯基等之烷氧基苯基、2-甲基苯基、3-甲基苯基、4-甲基苯基、乙基苯基、4-tert-丁基苯基、4-丁基苯基、二甲基苯基等之烷基苯基,甲基萘基、乙基萘基等之烷基萘基,甲氧基萘基、乙氧基萘基等之烷氧基萘基,二甲基萘基、二乙基萘基等之二烷基萘基,二甲氧基萘基、二乙氧基萘基等之二烷氧基萘基等。芳烷基例如苯甲基、苯基乙基、苯乙基等。芳基酮烷基例如,2-苯基-2-酮基乙基、2、(1-萘基)-2-酮基乙基、2-(2-萘基)-2-酮基乙基等之2-芳基-2-酮基乙基等。
A-
為氫氧離子、甲酸離子、乙酸離子、丙酸離子、丁
酸離子、戊酸離子、己酸離子、庚酸離子、辛酸離子、壬酸離子、癸酸離子、油酸離子、硬脂酸離子、亞油酸離子、亞麻酸離子、苯甲酸離子、p-甲基苯甲酸離子、p-t-丁基苯甲酸離子、苯二甲酸離子、間苯二甲酸離子、對苯二甲酸離子、水楊酸離子、三氟乙酸離子、單氯乙酸離子、二氯乙酸離子、三氯乙酸離子、氟化物離子、氯化物離子、溴化物離子、碘化物離子、硝酸離子、氯酸離子、過氯酸離子、溴酸離子、碘酸離子、草酸離子、丙二酸離子、甲基丙二酸離子、乙基丙二酸離子、丙基丙二酸離子、丁基丙二酸離子、二甲基丙二酸離子、二乙基丙二酸離子、丁二酸離子、甲基丁二酸離子、戊二酸離子、己二酸離子、依康酸離子、馬來酸離子、富馬酸離子、檸康酸離子、檸檬酸離子、碳酸離子等。
具體而言,例如,鋶化合物例如,甲酸三苯基鋶、乙酸三苯基鋶、丙酸三苯基鋶、丁酸三苯基鋶、戊酸三苯基鋶、己酸三苯基鋶、庚酸三苯基鋶、辛酸三苯基鋶、壬酸三苯基鋶、癸酸三苯基鋶、油酸三苯基鋶、硬脂酸三苯基鋶、亞油酸三苯基鋶、亞麻酸三苯基鋶、苯甲酸三苯基鋶、p-甲基苯甲酸三苯基鋶、p-t-丁基苯甲酸三苯基鋶、苯二甲酸三苯基鋶、間苯二甲酸三苯基鋶、對苯二甲酸三苯基鋶、水楊酸三苯基鋶、三氟乙酸三苯基鋶、單氯乙酸三苯基鋶、二氯乙酸三苯基鋶、三氯乙酸三苯基鋶、氫氧化三苯基鋶、草酸三苯基鋶、丙二酸三苯基鋶、甲基丙二酸三苯基鋶、乙基丙二酸三苯基鋶、丙基丙二酸三苯基鋶、丁基丙二酸三苯基鋶、二甲基丙二酸三苯基鋶、二乙基丙二酸三苯基鋶、丁二酸三苯基鋶、甲基丁二酸三苯基鋶、戊二酸三苯基鋶、己二酸三苯基鋶、依康酸三苯基鋶、馬來酸三苯基鋶、富馬酸三苯基鋶、檸康酸三苯基鋶、檸檬酸三苯基鋶、碳酸三苯基鋶、氯化三苯基鋶、溴化三苯基鋶、碘化三苯基鋶、硝酸三苯基鋶、氯酸三苯基鋶、過氯酸三苯基鋶、溴酸三苯基鋶、碘酸三苯基鋶、草酸雙三苯基鋶、丙二酸雙三苯基鋶、甲基丙二酸雙三苯基鋶、乙基丙二酸雙三苯基鋶、丙基丙二酸雙三苯基鋶、丁基丙二酸雙三苯基鋶、二甲基丙二酸雙三苯基鋶、二乙基丙二酸雙三苯基鋶、丁二酸雙三苯基鋶、甲基丁二酸雙三苯基鋶、戊二酸雙三苯基鋶、己二酸雙三苯基鋶、依康酸雙三苯基鋶、馬來酸雙三苯基鋶、富馬酸雙三苯基鋶、檸康酸雙三苯基鋶、檸檬酸雙三苯基鋶、碳酸雙三苯基鋶等。
又,碘鎓化合物,具體而言例如,甲酸二苯基碘鎓、乙酸二苯基碘鎓、丙酸二苯基碘鎓、丁酸二苯基碘鎓、戊酸二苯基碘鎓、己酸二苯基碘鎓、庚酸二苯基碘鎓、辛酸二苯基碘鎓、壬酸二苯基碘鎓、癸酸二苯基碘鎓、油酸二苯基碘鎓、硬脂酸二苯基碘鎓、亞油酸二苯基碘鎓、亞麻酸二苯基碘鎓、苯甲酸二苯基碘鎓、p-甲基苯甲酸二苯基碘鎓、p-t-丁基苯甲酸二苯基碘鎓、苯二甲酸二苯基碘鎓、間苯二甲酸二苯基碘鎓、對苯二甲酸二苯基碘鎓、水楊酸二苯基碘鎓、三氟乙酸二苯基碘鎓、單氯乙酸二苯基碘鎓、二氯乙酸二苯基碘鎓、三氯乙酸二苯基碘鎓、氫氧化二苯基碘鎓、草酸二苯基碘鎓、丙二酸二苯基碘鎓、甲基丙二酸二苯基碘鎓、乙基丙二酸二苯基碘鎓、丙基丙二酸二苯基碘鎓、丁基丙二酸二苯基碘鎓、二甲基丙二酸二苯基碘鎓、二乙基丙二酸二苯基碘鎓、丁二酸二苯基碘鎓、甲基丁二酸二苯基碘鎓、戊二酸二苯基碘鎓、己二酸二苯基碘鎓、依康酸二苯基碘鎓、馬來酸二苯基碘鎓、富馬酸二苯基碘鎓、檸康酸二苯基碘鎓、檸檬酸二苯基碘鎓、碳酸二苯基碘鎓、氯化二苯基碘鎓、溴化二苯基碘鎓、碘化二苯基碘鎓、硝酸二苯基碘鎓、氯酸二苯基碘鎓、過氯酸二苯基碘鎓、溴酸二苯基碘鎓、碘酸二苯基碘鎓、草酸雙二苯基碘鎓、丙二酸雙二苯基碘鎓、甲基丙二酸雙二苯基碘鎓、乙基丙二酸雙二苯基碘鎓、丙基丙二酸雙二苯基碘鎓、丁基丙二酸雙二苯基碘鎓、二甲基丙二酸雙二苯基碘鎓、二乙基丙二酸雙二苯基碘鎓、丁二酸雙二苯基碘鎓、甲基丁二酸雙二苯基碘鎓、戊二酸雙二苯基碘鎓、己二酸雙二苯基碘鎓、依康酸雙二苯基碘鎓、馬來酸雙二苯基碘鎓、富馬酸雙二苯基碘鎓、檸康酸雙二苯基碘鎓、檸檬酸雙二苯基碘鎓、碳酸雙二苯基碘鎓等。
又,銨化合物,具體而言例如,甲酸四甲基銨、乙酸四甲基銨、丙酸四甲基銨、丁酸四甲基銨、戊酸四甲基銨、己酸四甲基銨、庚酸四甲基銨、辛酸四甲基銨、壬酸四甲基銨、癸酸四甲基銨、油酸四甲基銨、硬脂酸四甲基銨、亞油酸四甲基銨、亞麻酸四甲基銨、苯甲酸四甲基銨、p-甲基苯甲酸四甲基銨、p-t-丁基苯甲酸四甲基銨、苯二甲酸四甲基銨、間苯二甲酸四甲基銨、對苯二甲酸四甲基銨、水楊酸四甲基銨、三氟乙酸四甲基銨、單氯乙酸四甲基銨、二氯乙酸四甲基銨、三氯乙酸四甲基銨、氫氧化四甲基銨、草酸四甲基銨、丙二酸四甲基銨、甲基丙二酸四甲基銨、乙基丙二酸四甲基銨、丙基丙二酸四甲基銨、丁基丙二酸四甲基銨、二甲基丙二酸四甲基銨、二乙基丙二酸四甲基銨、丁二酸四甲基銨、甲基丁二酸四甲基銨、戊二酸四甲基銨、己二酸四甲基銨、依康酸四甲基銨、馬來酸四甲基銨、富馬酸四甲基銨、檸康酸四甲基銨、檸檬酸四甲基銨、碳酸四甲基銨、氯化四甲基銨、溴化四甲基銨、碘化四甲基銨、硝酸四甲基銨、氯酸四甲基銨、過氯酸四甲基銨、溴酸四甲基銨、碘酸四甲基銨、草酸雙四甲基銨、丙二酸雙四甲基銨、甲基丙二酸雙四甲基銨、乙基丙二酸雙四甲基銨、丙基丙二酸雙四甲基銨、丁基丙二酸雙四甲基銨、二甲基丙二酸雙四甲基銨、二乙基丙二酸雙四甲基銨、丁二酸雙四甲基銨、甲基丁二酸雙四甲基銨、戊二酸雙四甲基銨、己二酸雙四甲基銨、依康酸雙四甲基銨、馬來酸雙四甲基銨、富馬酸雙四甲基銨、檸康酸雙四甲基銨、檸檬酸雙四甲基銨、碳酸雙四甲基銨、甲酸四丙基銨、乙酸四丙基銨、丙酸四丙基銨、丁酸四丙基銨、戊酸四丙基銨、己酸四丙基銨、庚酸四丙基銨、辛酸四丙基銨、壬酸四丙基銨、癸酸四丙基銨、油酸四丙基銨、硬脂酸四丙基銨、亞油酸四丙基銨、亞麻酸四丙基銨、苯甲酸四丙基銨、p-甲基苯甲酸四丙基銨、p-t-丁基苯甲酸四丙基銨、苯二甲酸四丙基銨、間苯二甲酸四丙基銨、對苯二甲酸四丙基銨、水楊酸四丙基銨、三氟乙酸四丙基銨、單氯乙酸四丙基銨、二氯乙酸四丙基銨、三氯乙酸四丙基銨、氫氧化四丙基銨、草酸四丙基銨、丙二酸四丙基銨、甲基丙二酸四丙基銨、乙基丙二酸四丙基銨、丙基丙二酸四丙基銨、丁基丙二酸四丙基銨、二甲基丙二酸四丙基銨、二乙基丙二酸四丙基銨、丁二酸四丙基銨、甲基丁二酸四丙基銨、戊二酸四丙基銨、己二酸四丙基銨、依康酸四丙基銨、馬來酸四丙基銨、富馬酸四丙基銨、檸康酸四丙基銨、檸檬酸四丙基銨、碳酸四丙基銨、氯化四丙基銨、溴化四丙基銨、碘化四丙基銨、硝酸四丙基銨、氯酸四丙基銨、過氯酸四丙基銨、溴酸四丙基銨、碘酸四丙基銨、草酸雙四丙基銨、丙二酸雙四丙基銨、甲基丙二酸雙四丙基銨、乙基丙二酸雙四丙基銨、丙基丙二酸雙四丙基銨、丁基丙二酸雙四丙基銨、二甲基丙二酸雙四丙基銨、二乙基丙二酸雙四丙基銨、丁二酸雙四丙基銨、甲基丁二酸雙四丙基銨、戊二酸雙四丙基銨、己二酸雙四丙基銨、依康酸雙四丙基銨、馬來酸雙四丙基銨、富馬酸雙四丙基銨、檸康酸雙四丙基銨、檸檬酸雙四丙基銨、碳酸雙四丙基銨、甲酸四丁基銨、乙酸四丁基銨、丙酸四丁基銨、丁酸四丁基銨、戊酸四丁基銨、己酸四丁基銨、庚酸四丁基銨、辛酸四丁基銨、壬酸四丁基銨、癸酸四丁基銨、油酸四丁基銨、硬脂酸四丁基銨、亞油酸四丁基銨、亞麻酸四丁基銨、苯甲酸四丁基銨、p-甲基苯甲酸四丁基銨、p-t-丁基苯甲酸四丁基銨、苯二甲酸四丁基銨、間苯二甲酸四丁基銨、對苯二甲酸四丁基銨、水楊酸四丁基銨、三氟乙酸四丁基銨、單氯乙酸四丁基銨、二氯乙酸四丁基銨、三氯乙酸四丁基銨、氫氧化四丁基銨、草酸四丁基銨、丙二酸四丁基銨、甲基丙二酸四丁基銨、乙基丙二酸四丁基銨、丙基丙二酸四丁基銨、丁基丙二酸四丁基銨、二甲基丙二酸四丁基銨、二乙基丙二酸四丁基銨、丁二酸四丁基銨、甲基丁二酸四丁基銨、戊二酸四丁基銨、己二酸四丁基銨、依康酸四丁基銨、馬來酸四丁基銨、富馬酸四丁基銨、檸康酸四丁基銨、檸檬酸四丁基銨、碳酸四丁基銨、氯化四丁基銨、溴化四丁基銨、碘化四丁基銨、硝酸四丁基銨、氯酸四丁基銨、過氯酸四丁基銨、溴酸四丁基銨、碘酸四丁基銨、草酸雙四丁基銨、丙二酸雙四丁基銨、甲基丙二酸雙四丁基銨、乙基丙二酸雙四丁基銨、丙基丙二酸雙四丁基銨、丁基丙二酸雙四丁基銨、二甲基丙二酸雙四丁基銨、二乙基丙二酸雙四丁基銨、丁二酸雙四丁基銨、甲基丁二酸雙四丁基銨、戊二酸雙四丁基銨、己二酸雙四丁基銨、依康酸雙四丁基銨、馬來酸雙四丁基銨、富馬酸雙四丁基銨、檸康酸雙四丁基銨、檸檬酸雙四丁基銨、碳酸雙四丁基銨等例示。
又,上述熱交聯促進劑可單獨使用1種或將2種以上組合使用皆可。熱交聯促進劑之添加量,相對於基礎聚合物(上述方法所得之(A)成份的含金屬氧化物之化合物)100質量份,較佳為添加0.01~50質量份,更佳為0.1~40質量份。
為確保本發明之熱硬化性含金屬氧化物之膜形成用組成物的安定性時,必須添加(C)成份之碳數為1~30之1價或2價以上的有機酸。此時所添加之酸,例如甲酸、乙酸、丙酸、丁酸、戊酸、己酸、庚酸、辛酸、壬酸、癸酸、油酸、硬脂酸、亞油酸、亞麻酸、苯甲酸、苯二甲酸、間苯二甲酸、對苯二甲酸、水楊酸、三氟乙酸、單氯乙酸、二氯乙酸、三氯乙酸、草酸、丙二酸、甲基丙二酸、乙基丙二酸、丙基丙二酸、丁基丙二酸、二甲基丙二酸、二乙基丙二酸、丁二酸、甲基丁二酸、戊二酸、己二酸、依康酸、馬來酸、富馬酸、檸康酸、檸檬酸等。特別是以草酸、馬來酸、甲酸、乙酸、丙酸、檸檬酸等為佳。又,為保持安定性,亦可將2種以上之酸混合使用亦可。添加量,相對於組成物中所含之金屬氧化物100質量份,為0.001~25質量份,較佳為0.01~15質量份,更佳為0.1~5質量份。
或,上述有機酸換算為組成物之pH時,較佳以可達成0≦pH≦7,更佳為0.3≦pH≦6.5,最佳為0.5≦pH≦6之方式添加為宜。
含有本發明之含金屬氧化物之化合物的組成物中,(D)成份為與製造前述含金屬氧化物之化合物時所使用之成分為相同之有機溶劑,較佳為水溶性有機溶劑,特別是使用乙二醇、二乙二醇、三乙二醇、丙二醇、二丙二醇、丁二醇、戊二醇等單烷基醚衍生物為佳。具體而言,例如,可使用由丁二醇單甲基醚、丙二醇單甲基醚、乙二醇單甲基醚、丁二醇單乙基醚、丙二醇單乙基醚、乙二醇單乙基醚、丁二醇單丙基醚、丙二醇單丙基醚、乙二醇單丙基醚等所選出之有機溶劑。其使用量將於後說明。
又,本發明中,可含有通式(5)所表示之水解性矽化合物經水解縮合所得之含矽之化合物。
R6 m6
R7 m7
R8 m8
Si(OR9
)(4-m6-m7-m8)
(5)
(式中,R9
為碳數1~6之烷基,R6
、R7
、R8
分別為氫原子,或碳數1~30之1價之有機基,m6、m7、m8為0或1;m6+m7+m8為0~3之整數)。
該式(5)所使用之R6
、R7
、R8
、R9
、m6、m7、m8為對應於通式(1)之R1
、R2
、R3
、R、m1、m2、m3,且其例示亦為完全相同。
該些含矽之化合物(E)的製造方法,例如與(A)的製造方法為相同之方法。
此外,本發明所可使用之含矽之化合物(E),可於鹼觸媒下使單體水解縮合而製得。較佳之含矽之化合物的製造方法,例如以下所例示者,但並不僅限定於該方法。
作為起始物質之單體,可使用前述通式(5)所表示之單體,具體而言,例如上述段落[0065]~[0071]所表示之內容。
含矽之化合物(E),可使單體於鹼性觸媒之存在下,進行水解縮合而可製得。
此時所使用之鹼觸媒,例如甲基胺、乙基胺、丙基胺、丁基胺、乙烯二胺、六伸甲基二胺、二甲基胺、二乙基胺、乙基甲基胺、三甲基胺、三乙基胺、三丙基胺、三丁基胺、環己基胺、二環己基胺、單乙醇胺、二乙醇胺、二甲基單乙醇胺、單甲基二乙醇胺、三乙醇胺、二氮雜二環辛烷、二氮雜二環環壬烯、二氮雜二環十一烯、六伸甲基四胺、苯胺、N,N-二甲基苯胺、吡啶、N,N-二甲基胺基吡啶、吡咯、六氫吡啶、吡咯烷、哌啶、甲吡啶、氫氧化四甲基銨、氫氧化膽鹼、氫氧化四丙基銨、氫氧化四丁基銨、氨、氫氧化鋰、氫氧化鈉、氫氧化鉀、氫氧化鋇、氫氧化鈣等。觸媒之使用量,相對於矽單體1莫耳為10-6
~10莫耳,較佳為10-5
~5莫耳,更佳為10-4
~1莫耳。
該些單體經由水解縮合而得到含矽之化合物時之水量,以相對於鍵結於單體之水解性取代基1莫耳添加0.1~50莫耳為佳。添加超過50莫耳時,僅造成反應所使用之裝置過大而已,而不具經濟效應。
操作方法為,於觸媒水溶液中添加單體使水解縮合反應開始。此時,可於觸媒水溶液中加入有機溶劑亦可,或將單體稀釋於有機溶劑中亦可,或兩者皆可。反應溫度為0~100℃,較佳為5~80℃。以單體滴下時保持5~80℃之溫度,其後再於20~80℃下熟成之方法為佳。
可加入觸媒水溶液中之有機溶劑,或可稀釋單體之有機溶劑,例如甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-1-丙醇、丙酮、乙腈、四氫呋喃、甲苯、己烷、乙酸乙酯、環己酮、甲基-2-n-戊酮、丙二醇單甲基醚、乙二醇單甲基醚、丙二醇單乙基醚、乙二醇單乙基醚、丙二醇二甲基醚、二乙二醇二甲基醚、丙二醇單甲基醚乙酸酯、丙二醇單乙基醚乙酸酯、丙酮酸乙基、乙酸丁基、3-甲氧基丙酸甲基、3-乙氧基丙酸乙基、乙酸tert-丁基、丙酸tert-丁基、丙二醇單tert-丁基醚乙酸酯、γ-丁內酯及其混合物等。
該些溶劑中較佳者為水可溶性之溶劑。例如,甲醇、乙醇、1-丙醇、2-丙醇等之醇類,乙二醇、丙二醇等之多元醇,丙二醇單甲基醚、乙二醇單甲基醚、丙二醇單乙基醚、乙二醇單乙基醚、丙二醇單丙基醚、乙二醇單丙基醚等多元醇縮合物衍生物,丙酮、乙腈、四氫呋喃等。
其中,最佳者為沸點為100℃以下者。
又,有機溶劑之使用量,相對於單體1莫耳以使用0~1,000ml為佳。有機溶劑之使用量過多時,將造成反應容器過大而不具經濟效應。
其後,必要時可進行觸媒之中和反應,以減壓去除水解縮合反應所生成之醇,得反應混合物水溶液。此時,中和時所使用酸性物質之量,以相對於觸媒所使用之鹼的0.1~2當量為佳。只要該酸性物質於水中可顯示出酸性之物質時,可為任意之物質皆可。
隨後,必須將反應混合物中經水解縮合反應所生成之醇去除。此時反應混合物之加熱溫度,依與所添加之有機溶劑發生反應之醇的種類而有所不同,較佳為0~100℃,更佳為10~90℃,最佳為15~80℃。又,此時之減壓度,依所欲去除之有機溶劑及醇之種類、排氣裝置、凝縮裝置及加熱溫度而有所不同,較佳為於大氣壓以下,更佳為於絕對壓之80kPa以下,最佳為於絕對壓之50kPa以下。雖無法正確得知此時所去除之醇量,但以去除所生成之醇等的約80質量%以上者為佳。
其次,為去除水解縮合時所使用之觸媒,需使用有機溶劑萃取含矽之化合物。此時所使用之有機溶劑,只要可溶解含矽之化合物,與水混合時可分離為2層者為佳。例如甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-1-丙醇、丙酮、四氫呋喃、甲苯、己烷、乙酸乙酯、環己酮、甲基-2-n-戊酮、丙二醇單甲基醚、乙二醇單甲基醚、丙二醇單乙基醚、乙二醇單乙基醚、丙二醇單丙基醚、乙二醇單丙基醚、丙二醇二甲基醚、二乙二醇二甲基醚、丙二醇單甲基醚乙酸酯、丙二醇單乙基醚乙酸酯、丙酮酸乙基、乙酸丁基、3-甲氧基丙酸甲基、3-乙氧基丙酸乙基、乙酸tert-丁基、丙酸tert-丁基、丙二醇單tert-丁基醚乙酸酯、γ-丁內酯、甲基異丁酮、環戊基甲基醚等及其混合物。
此外,也可使用水溶性有機溶劑與水難溶性有機溶劑之混合物。例如以甲醇+乙酸乙酯、乙醇+乙酸乙酯、1-丙醇+乙酸乙酯、2-丙醇+乙酸乙酯、丙二醇單甲基醚+乙酸乙酯、乙二醇單甲基醚、丙二醇單乙基醚+乙酸乙酯、乙二醇單乙基醚+乙酸乙酯、丙二醇單丙基醚+乙酸乙酯、乙二醇單丙基醚+乙酸乙酯、甲醇+甲基異丁酮、乙醇+甲基異丁酮、1-丙醇+甲基異丁酮、2-丙醇+甲基異丁酮、丙二醇單甲基醚+甲基異丁酮、乙二醇單甲基醚、丙二醇單乙基醚+甲基異丁酮、乙二醇單乙基醚+甲基異丁酮、丙二醇單丙基醚+甲基異丁酮、乙二醇單丙基醚+甲基異丁酮、甲醇+環戊基甲基醚、乙醇+環戊基甲基醚、1-丙醇+環戊基甲基醚、2-丙醇+環戊基甲基醚、丙二醇單甲基醚+環戊基甲基醚、乙二醇單甲基醚、丙二醇單乙基醚+環戊基甲基醚、乙二醇單乙基醚+環戊基甲基醚、丙二醇單丙基醚+環戊基甲基醚、乙二醇單丙基醚+環戊基甲基醚、甲醇+丙二醇甲基醚乙酸酯、乙醇+丙二醇甲基醚乙酸酯、1-丙醇+丙二醇甲基醚乙酸酯、2-丙醇+丙二醇甲基醚乙酸酯、丙二醇單甲基醚+丙二醇甲基醚乙酸酯、乙二醇單甲基醚、丙二醇單乙基醚+丙二醇甲基醚乙酸酯、乙二醇單乙基醚+丙二醇甲基醚乙酸酯、丙二醇單丙基醚+丙二醇甲基醚乙酸酯、乙二醇單丙基醚+丙二醇甲基醚乙酸酯等組合為佳,但組合併不僅限定於上述內容。
又,水溶性有機溶劑與水難溶性有機溶劑之混合比例,雖可適度選擇,一般以相對於難溶性有機溶劑100質量份,水溶性有機溶劑為0.1~1,000質量份,較佳為1~500質量份,更佳為2~100質量份。
隨後,以中性水洗淨。該水,一般為使用通常稱為去離子水或超純水之水即可。該水之量,相對於含矽之化合物溶液1L,為使用0.01~100L,較佳為0.05~50L,更佳為0.1~5L。其洗淨之方法,例如將兩者放置於同一容器中攪拌混合後,靜置使水層分離即可。洗淨次數,以1次以上即可,即使洗淨10次以上時,也僅能得到洗淨之效果而已,故較佳以1~5次左右為佳。
於洗淨後之含矽之化合物溶液中加入最後的溶劑,於減壓下進行溶劑交換而得含矽之化合物溶液。此時溶劑交換之溫度,依所欲去除之萃取溶劑的種類而有所不同,較佳為0~100℃,更佳為10~90℃,最佳為15~80℃。又,此時之減壓度,依所欲去除之萃取溶劑之種類、排氣裝置、凝縮裝置及加熱溫度而有所不同,較佳為大氣壓以下,更佳為絕對壓之80kPa以下,最佳為絕對壓之50kPa以下。
作為加入含矽之化合物溶液中之最後的溶劑,較佳者為例如醇系溶劑,特佳者例如乙二醇、二乙二醇、三乙二醇、丙二醇、二丙二醇、丁二醇等單烷基醚衍生物。具體而言,例如,丁二醇單甲基醚、丙二醇單甲基醚、乙二醇單甲基醚、丁二醇單乙基醚、丙二醇單乙基醚、乙二醇單乙基醚、丁二醇單丙基醚、丙二醇單丙基醚、乙二醇單丙基醚等為佳。
又,其他反應操作,係於單體或單體之有機溶液中,添加水或含水有機溶劑,以開始水解反應。此時,觸媒可添加於單體或單體之有機溶液中,或添加於水或含水有機溶劑中亦可。反應溫度為0~100℃,較佳為10~80℃。又以滴下水時加熱至10~50℃,其後升溫至20~80℃以使其熟成之方法為佳。
使用有機溶劑之情形,以水溶性之溶劑為佳,例如甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-1-丙醇、丙酮、四氫呋喃、乙腈、丙二醇單甲基醚、乙二醇單甲基醚、丙二醇單乙基醚、乙二醇單乙基醚、丙二醇單丙基醚、乙二醇單丙基醚、丙二醇二甲基醚、二乙二醇二甲基醚、丙二醇單甲基醚乙酸酯、丙二醇單乙基醚乙酸酯、丙二醇單丙基醚等多元醇縮合物衍生物及其混合物等。
有機溶劑之使用量,與前述之量為相同。所得反應混合物之後處理,可與前述方法為相同般進行後處理,得含矽之化合物(E)。
所得含矽之化合物(E)之分子量,除可選擇單體以外,亦可由聚合時反應條件之控制進行調整,重量平均分子量使用超過1,000,000以上時,依情況之不同,而會有發生異物或產生塗佈斑等情形,一般以使用800,000以下,更佳為200~500,000,最佳為300~300,000之單體為宜。又,上述重量平均分子量之數據,為使用RI或光散射式檢測器作為檢測器之凝膠滲透色層分析法(GPC),標準物質使用聚苯乙烯,並以聚苯乙烯換算所得分子量表示者。
所得含矽之化合物(E)之添加比,相對於(A)成份雖可為任意之添加比,但較佳為配合所得之膜的性能,以質量比為(A)>(E)者為佳。
本發明中,組成物可添加水亦可。添加水時,含金屬氧化物之化合物會形成水和物,而可提高微影蝕刻性能。組成物之溶劑成份中,水的含有率超過0質量%未達50質量%,更佳為0.3~30質量%,最佳為0.5~20質量%。各別之成份,於添加量過多時,將會使塗佈膜之均勻性惡化,最差之情形將會發生彈出現象。又,添加量過少時,將會造成微影蝕刻性能降低,而為不佳。
包含水之全溶劑之使用量,相對於(A)成份之基礎聚合物100質量份為500~100,000質量份,特別是以400~50,000質量份為佳。
本發明中,可使用光酸發生劑。本發明所使用之光酸發生劑,例如
(A-I)下述通式(P1a-1)、(P1a-2)或(P1b)之鎓鹽、
(A-II)下述通式(P2)之重氮甲烷衍生物、
(A-III)下述通式(P3)之乙二肟衍生物、
(A-IV)下述通式(P4)之雙碸衍生物、
(A-V)下述通式(P5)之N-羥基醯亞胺化合物之磺酸酯、
(A-VI)p-酮磺酸衍生物、
(A-VII)二碸衍生物、
(A-VIII)硝基苯甲基磺酸酯衍生物、
(A-IX)磺酸酯衍生物
等。
(式中,R101a
、R101b
、R101c
分別為碳數1~12之直鏈狀、分支狀或環狀之烷基、烯基、酮烷基或酮烯基、碳數6~20之取代或無取代之芳基,或碳數7~12之芳烷基或芳基酮烷基,該些基中之氫原子的一部份或全部可被烷氧基等所取代亦可。又,R101b
與R101c
可與其鍵結之硫原子共同形成環亦可,形成環時,R101b
、R101c
分別表示碳數1~6之伸烷基。K-
為非親核性對向離子)。
上述R101a
、R101b
、R101c
可相互為相同或相異皆可、具體而言,烷基例如,甲基、乙基、丙基、異丙基、n-丁基、sec-丁基、tert-丁基、戊基、己基、庚基、辛基、環戊基、環己基、環庚基、環丙基甲基、4-甲基環己基、環己基甲基、降冰片烷基、金剛烷基等。烯基例如,乙烯基、烯丙基、丙烯基、丁烯基、己烯基、環己烯基等。酮烷基例如,2-酮基環戊基、2-酮基環己基、2-酮基丙基、2-環戊基-2-酮基乙基、2-環己基-2-酮基乙基、2-(4-甲基環己基)-2-酮基乙基等。芳基例如,苯基、萘基等,或,p-甲氧基苯基、m-甲氧基苯基、o-甲氧基苯基、乙氧基苯基、p-tert-丁氧基苯基、m-tert-丁氧基苯基等之烷氧基苯基、2-甲基苯基、3-甲基苯基、4-甲基苯基、乙基苯基、4-tert-丁基苯基、4-丁基苯基、二甲基苯基等之烷基苯基、甲基萘基、乙基萘基等之烷基萘基、甲氧基萘基、乙氧基萘基等之烷氧基萘基,二甲基萘基、二乙基萘基等之二烷基萘基,二甲氧基萘基、二乙氧基萘基等之二烷氧基萘基等。芳烷基例如,苯甲基、苯基乙基、苯乙基等。芳基酮烷基例如,2-苯基-2-酮基乙基、2-(1-萘基)-2-酮基乙基、2-(2-萘基)-2-酮基乙基等之2-芳基-2-酮基乙基等。K-
之非親核性對向離子例如有氯化物離子、溴化物離子等鹵化物離子,三氟甲烷磺酸酯、1,1,1-三氟乙烷磺酸酯、九氟丁烷磺酸酯等氟烷基磺酸酯,甲苯磺酸酯、苯磺酸酯、4-氟苯基磺酸酯、1,2,3,4,5-五氟苯基磺酸酯等芳基磺酸酯、甲磺醯酯、丁烷磺酸酯等烷基磺酸酯等
(式中,R102a
、R102b
係分別表示碳數1至8之直鏈狀、分支狀或環狀之烷基。R103
為碳數1至10之直鏈狀、分支狀或環狀之伸烷基。R104a
、R104b
係分別為碳數3至7之2-酮基烷基。K-
為非親核性對向離子)。
上述R102a
、R102b
之具體例為甲基、乙基、丙基、異丙基、n-丁基、sec-丁基、tert-丁基、戊基、己基、庚基、辛基、環戊基、環己基、環丙基甲基、4-甲基環己基、環己基甲基等。R103
之具體例為伸甲基、伸乙基、伸丙基、伸丁基、伸戊基、伸己基、伸庚基、伸辛基、伸壬基、1,4-伸環己基、1,2-伸環己基、1,3-伸環戊基、1,4-伸環辛基、1,4-伸環己二甲基等。R104a
、R104b
例如有2-氧代丙基、2-氧代環戊基、2-氧代環己基、2-氧代環庚基等。K-
例如與式(P1a-1)、(P1a-2)及(P1a-3)所說明之內容為相同者。
(式中,R105
、R106
為碳數1至12之直鏈狀、分支狀或環狀之烷基或鹵化烷基、碳數6至20之取代或無取代之取代或無取代之芳基或鹵化芳基或碳數7至12之芳烷基)。
R105
、R106
之烷基例如甲基、乙基、丙基、異丙基、n-丁基、sec-丁基、tert-丁基、戊基、己基、庚基、辛基、戊基、環戊基、環己基、環庚基、降冰片基、金剛烷基等。R105
、R106
之鹵化烷基例如有三氟甲基、1,1,1-三氟乙基、1,1,1-三氯乙基、九氟丁基等。R105
、R106
之芳基例如有苯基、p-甲氧苯基、m-甲氧苯基、o-甲氧苯基、乙氧苯基、p-tert-丁氧苯基、m-tert-丁氧苯基等之烷氧苯基、2-甲基苯基、3-甲基苯基、4-甲基苯基、乙基苯基、4-tert-丁基苯基、4-丁基苯基、二甲基苯基等之烷基苯基。R105
、R106
之鹵化芳基例如有氟苯基、氯苯基、1,2,3,4,5-五氟苯基等。R105
、R106
之芳烷基例如苯甲基、苯乙基等。
(式中R107
、R108
、R109
為碳數1至12之直鏈狀、分支狀或環狀之烷基或鹵化烷基、碳數6至20之芳基或鹵化芳基或碳數7至12之芳烷基。R108
、R109
可相互鍵結並與其鍵結之碳原子共同形成環狀構造,形成環狀構造時,R108
、R109
係分別為碳數1至6之直鏈狀、分支狀之伸烷基)。
R107
、R108
、R109
之烷基、鹵化烷基、芳基、鹵化芳基、芳烷基例如有與R105
、R106
所說明者相同的基。又,R108
、R109
之伸烷基例如有伸甲基、伸乙基、伸丙基、伸丁基、伸己基等。
(式中,R101
a、R101b
係與上述為相同之內容)。
(式中,R110
為碳數6至10之伸芳基、碳數1至6之伸烷基或碳數2至6之伸烯基,這些基所含之氫原子之一部份或全部可被碳數1至4之直鏈狀或分支狀之烷基或烷氧基、硝基、乙醯基或苯基所取代。R111
為碳數1至8之直鏈狀、分支狀或取代之烷基、烯基或烷氧基烷基、苯基或萘基,這些基之氫原子之一部份或全部可被碳數1至4之烷基或烷氧基;碳數1至4之烷基、烷氧基、硝基或乙醯基所取代之苯基;碳數3至5之雜芳基;或可被氯原子、氟原子所取代)。
其中,R110
之伸芳基例如1,2-伸苯基、1,8-伸萘基等;伸烷基例如伸甲基、伸乙基、伸丙基、伸丁基、苯基伸乙基、降冰片烷-2,3-二基等;伸烯基例如1,2-伸乙烯基、1-苯基-1,2-伸乙烯基、5-降冰片烯-2,3-二基等。R111
之烷基係與R101a
至R101c
相同者,烯基例如有乙烯基、1-丙烯基、烯丙基、1-丁烯基、3-丁烯基、異戊烯基、1-戊烯基、3-戊烯基、4-戊烯基、二甲基烯丙基、1-己烯基、3-己烯基、5-己烯基、1-庚烯基、3-庚烯基、6-庚烯基、7-辛烯基等;烷氧烷基例如甲氧甲基、乙氧甲基、丙氧甲基、丁氧甲基、戊氧甲基、己氧甲基、庚氧甲基、甲氧乙基、乙氧乙基、丙氧乙基、丁氧乙基、戊氧乙基、己氧乙基、甲氧丙基、乙氧丙基、丙氧丙基、丁氧丙基、甲氧丁基、乙氧丁基、丙氧丁基、甲氧戊基、乙氧戊基、甲氧己基、甲氧庚基等。
又,可再被取代之碳數1至4之烷基例如有甲基、乙基、丙基、異丙基、n-丁基、異丁基、tert-丁基等,碳數1至4之烷氧基例如甲氧基、乙氧基、丙氧基、異丙氧基、正丁氧基、異丁氧基、tert-丁氧基等;可被碳數1至4之烷基、烷氧基、硝基或乙醯基所取代之苯基例如有苯基、甲苯基、對tert-丁氧苯基、對乙醯苯基、對硝基苯基等;碳數3至5之雜芳基例如吡啶基、呋喃基等。
具體而言,例如,可列舉例如下述之光酸發生劑。三氟甲烷磺酸二苯基碘鎓、三氟甲烷磺酸(p-tert-丁氧基苯基)苯基碘鎓、p-甲苯磺酸二苯基碘鎓、p-甲苯磺酸(p-tert-丁氧基苯基)苯基碘金翁、三氟甲烷磺酸三苯基鋶、三氟甲烷磺酸(p-tert-丁氧基苯基)二苯基鋶、三氟甲烷磺酸雙(p-tert-丁氧基苯基)苯基鋶、三氟甲烷磺酸三(p-tert-丁氧基苯基)鋶、p-甲苯磺酸三苯基鋶、p-甲苯磺酸(p-tert-丁氧基苯基)二苯基鋶、p-甲苯磺酸雙(p-tert-丁氧基苯基)苯基鋶、p-甲苯磺酸三(p-tert-丁氧基苯基)鋶、九氟丁烷磺酸三苯基鋶、丁烷磺酸三苯基鋶、三氟甲烷磺酸三甲基鋶、p-甲苯磺酸三甲基鋶、三氟甲烷磺酸環己基甲基(2-酮基環己基)鋶、p-甲苯磺酸環己基甲基(2-酮基環己基)鋶、三氟甲烷磺酸二甲基苯基鋶、p-甲苯磺酸二甲基苯基鋶、三氟甲烷磺酸二環己基苯基鋶、p-甲苯磺酸二環己基苯基鋶、三氟甲烷磺酸三萘基鋶、三氟甲烷磺酸環己基甲基(2-酮基環己基)鋶、三氟甲烷磺酸(2-降冰片基)甲基(2-酮基環己基)鋶、乙撐雙[甲基(2-酮基環戊基)鋶三氟甲烷磺酸酯]、1,2’-萘基羰甲基四氫噻吩鎓三氟甲烷磺酸酯(triflate)等之鎓鹽。
雙(苯磺醯基)重氮甲烷、雙(p-甲苯磺醯基)重氮甲烷、雙(二甲苯磺醯基)重氮甲烷、雙(環己基磺醯基)重氮甲烷、雙(環戊基磺醯基)重氮甲烷、雙(n-丁基磺醯基)重氮甲烷、雙(異丁基磺醯基)重氮甲烷、雙(sec-丁基磺醯基)重氮甲烷、雙(n-丙基磺醯基)重氮甲烷、雙(異丙基磺醯基)重氮甲烷、雙(tert-丁基磺醯基)重氮甲烷、雙(n-戊基磺醯基)重氮甲烷、雙(異戊基磺醯基)重氮甲烷、雙(sec-戊基磺醯基)重氮甲烷、雙(tert-戊基磺醯基)重氮甲烷、1-環己基磺醯基-1-(tert-丁基磺醯基)重氮甲烷、1-環己基磺醯基-1-(tert-戊基磺醯基)重氮甲烷、1-tert-戊基磺醯基-1-(tert-丁基磺醯基)重氮甲烷等之重氮甲烷衍生物。
雙-O-(p-甲苯磺醯基)-α-二甲基乙二肟、雙-O-(p-甲苯磺醯基)-α-二苯基乙二肟、雙-O-(p-甲苯磺醯基)-α-二環己基乙二肟、雙-O-(p-甲苯磺醯基)-2,3-戊二酮乙二肟、雙-O-(p-甲苯磺醯基)-2-甲基-3,4-戊二酮乙二肟、雙-O-(n-丁烷磺醯基)-α-二甲基乙二肟、雙-O-(n-丁烷磺醯基)-α-二苯基乙二肟、雙-O-(n-丁烷磺醯基)-α-二環己基乙二肟、雙-O-(n-丁烷磺醯基)-2,3-戊二酮乙二肟、雙-O-(n-丁烷磺醯基)-2-甲基-3,4-戊二酮乙二肟、雙-O-(甲烷磺醯基)-α-二甲基乙二肟、雙-O-(三氟甲烷磺醯基)-α-二甲基乙二肟、雙-O-(1,1,1-三氟乙烷磺醯基)-α-二甲基乙二肟、雙-O-(tert-丁烷磺醯基)-α-二甲基乙二肟、雙-O-(全氟辛烷磺醯基)-α-二甲基乙二肟、雙-O-(環己烷磺醯基)-α-二甲基乙二肟、雙-O-(苯磺醯基)-α-二甲基乙二肟、雙-O-(p-氟苯磺醯基)-α-二甲基乙二肟、雙-O-(p-tert-丁基苯磺醯基)-α-二甲基乙二肟、雙-O-(二甲苯磺醯基)-α-二甲基乙二肟、雙-O-(樟腦磺醯基)-α-二甲基乙二肟等之乙二肟衍生物。
雙萘基磺醯基甲烷、雙三氟甲基磺醯基甲烷、雙甲基磺醯基甲烷、雙乙基磺醯基甲烷、雙丙基磺醯基甲烷、雙異丙基磺醯基甲烷、雙-p-甲苯磺醯基甲烷、雙苯磺醯基甲烷等之雙碸衍生物。
2-環己基羰基-2-(p-甲苯磺醯基)丙烷、2-異丙基羰基-2-(p-甲苯磺醯基)丙烷等之β-酮磺酸衍生物。
二苯基二碸、二環己基二碸等之二碸衍生物。
p-甲苯磺酸2,6-二硝基苯甲基、p-甲苯磺酸2,4-二硝基苯甲基等之硝基苯甲基磺酸酯衍生物。
1,2,3-三(甲烷磺醯基氧代基)苯、1,2,3-三(三氟甲烷磺醯基氧代基)苯、1,2,3-三(p-甲苯磺醯基氧代基)苯等之磺酸酯衍生物。
N-羥基琥珀醯亞胺甲烷磺酸酯、N-羥基琥珀醯亞胺三氟甲烷磺酸酯、N-羥基琥珀醯亞胺乙烷磺酸酯、N-羥基琥珀醯亞胺1-丙烷磺酸酯、N-羥基琥珀醯亞胺2-丙烷磺酸酯、N-羥基琥珀醯亞胺1-戊烷磺酸酯、N-羥基琥珀醯亞胺1-辛烷磺酸酯、N-羥基琥珀醯亞胺p-甲苯磺酸酯、N-羥基琥珀醯亞胺p-甲氧基苯磺酸酯、N-羥基琥珀醯亞胺2-氯乙烷磺酸酯、N-羥基琥珀醯亞胺苯磺酸酯、N-羥基琥珀醯亞胺-2,4,6-三甲基苯磺酸酯、N-羥基琥珀醯亞胺1-萘磺酸酯、N-羥基琥珀醯亞胺2-萘磺酸酯、N-羥基-2-苯基琥珀醯亞胺甲烷磺酸酯、N-羥基馬來醯亞胺甲烷磺酸酯、N-羥基馬來醯亞胺乙烷磺酸酯、N-羥基-2-苯基馬來醯亞胺甲烷磺酸酯、N-羥基戊二醯亞胺甲烷磺酸酯、N-羥基戊二醯亞胺苯磺酸酯、N-羥基鄰苯二甲醯亞胺甲烷磺酸酯、N-羥基鄰苯二甲醯亞胺苯磺酸酯、N-羥基鄰苯二甲醯亞胺三氟甲烷磺酸酯、N-羥基鄰苯二甲醯亞胺p-甲苯磺酸酯、N-羥基萘二甲醯亞胺甲烷磺酸酯、N-羥基萘二甲醯亞胺苯磺酸酯、N-羥基-5-降冰片烯-2,3-二羧基醯亞胺甲烷磺酸酯、N-羥基-5-降冰片烯-2,3-二羧基醯亞胺三氟甲烷磺酸酯、N-羥基-5-降冰片烯-2,3-二羧基醯亞胺p-甲苯磺酸酯等之N-羥基醯亞胺化合物之磺酸酯衍生物等。
其中,特別是以三氟甲烷磺酸三苯基鋶、三氟甲烷磺酸(p-tert-丁氧基苯基)二苯基鋶、三氟甲烷磺酸三(p-tert-丁氧基苯基)鋶、p-甲苯磺酸三苯基鋶、p-甲苯磺酸(p-tert-丁氧基苯基)二苯基鋶、p-甲苯磺酸三(p-tert-丁氧基苯基)鋶、三氟甲烷磺酸三萘基鋶、三氟甲烷磺酸環己基甲基(2-酮基環己基)鋶、三氟甲烷磺酸(2-降冰片基)甲基(2-酮基環己基)鋶、1,2’-萘基羰基甲基四氫塞吩鎓三氟甲烷磺酸酯等之鎓鹽,雙(苯磺醯基)重氮甲烷、雙(p-甲苯磺醯基)重氮甲烷、雙(環己基磺醯基)重氮甲烷、雙(n-丁基磺醯基)重氮甲烷、雙(異丁基磺醯基)重氮甲烷、雙(sec-丁基磺醯基)重氮甲烷、雙(n-丙基磺醯基)重氮甲烷、雙(異丙基磺醯基)重氮甲烷、雙(tert-丁基磺醯基)重氮甲烷等之重氮甲烷衍生物,雙-O-(p-甲苯磺醯基)-α-二甲基乙二肟、雙-O-(n-丁烷磺醯基)-α-二甲基乙二肟等之乙二肟衍生物,雙萘基磺醯基甲烷等之雙碸衍生物,N-羥基琥珀醯亞胺甲烷磺酸酯、N-羥基琥珀醯亞胺三氟甲烷磺酸酯、N-羥基琥珀醯亞胺1-丙烷磺酸酯、N-羥基琥珀醯亞胺2-丙烷磺酸酯、N-羥基琥珀醯亞胺1-戊烷磺酸酯、N-羥基琥珀醯亞胺p-甲苯磺酸酯、N-羥基萘二甲醯亞胺甲烷磺酸酯、N-羥基萘二甲醯亞胺苯磺酸酯等之N-羥基醯亞胺化合物之磺酸酯衍生物為較佳使用者。
又,上述光酸發生劑可單獨使用1種或將2種以上組合使用亦可。酸發生劑之添加量,相對於(A)成份之基礎聚合物(上述方法所得之含金屬氧化物之化合物)100質量份,較佳為0.01~50質量份,更佳為0.05~40質量份。
此外,安定劑之具有使用環狀醚作為取代基之1價或2價以上之醇,特別是添加以下構造所表示之醚化合物時,可提高含金屬氧化物之膜形成用組成物之安定性。前述物質,例如下述所揭示之化合物等。
其中,R90a
為,氫原子、碳數1~10之直鏈狀、分支狀或環狀之1價烴基,R91
O-(CH2
CH2
O)n1
-(CH2
)n2
-(其中,0≦n1≦5、0≦n2≦3、R91
為氫原子或甲基),或R92
O-[CH(CH3
)CH2
O]n3
-(CH2
)n4
-(其中,0≦n3≦5、0≦n4≦3、R92
為氫原子或甲基),R90b
為,羥基、具有1個或2個以上之羥基的碳數1~10之直鏈狀、分支狀或環狀之1價烴基,HO-(CH2
CH2
O)n5
-(CH2
)n6
-(其中,1≦n5≦5、1≦n6≦3),或HO-[CH(CH3
)CH2
O]n7
-(CH2
)n8
-(其中,1≦n7≦5、1≦n8≦3)。
又,上述安定劑可單獨使用1種或將2種以上組合使用亦可。安定劑之添加量,相對於(A)成份之基礎聚合物(上述方法所得之含金屬氧化物之化合物)100質量份,較佳為0.001~50質量份,更佳為0.01~40質量份。又,該些安定劑可單獨使用1種或將2種以上混合使用亦可。其中,較佳之構造為冠醚衍生物與具有橋頭位置為氧原子之二環環作為取代基之化合物。
添加該些安定劑時,可使酸之電荷更為安定化,而期待可促使組成物中之含金屬氧化物之化合物的安定化。
此外,本發明中,必要時可添加界面活性劑。其中,界面活性劑以非離子性者為佳,例如全氟烷基聚氧乙烯乙醇、氟化烷基酯、全氟烷基胺氧化物、全氟烷基環氧乙烷加成物、含氟有機矽氧烷系化合物等。例如Fluorad「FC-430」、「FC-431」、「FC-4430」(皆為住友3M(股)製)、Surflon「S-141」、「S-145」、「KH-10」、「KH-20」、「KH-30」、「KH-40」(皆為旭硝子(股)製)、優妮坦「DS-401」、「DS-403」、「DS-451」(皆為大金工業(股)製)、美格氟「F-8151」(大日本油墨工業(股)製)、「X-70-092」、「X-70-093」(皆為信越化學工業(股)製)等。較佳者為,Fluorad「FC-4430」、「KH-20」、「KH-30」、「X-70-093」等。
又,界面活性劑之添加量,可使用不妨礙本發明之效果的範圍下之通常量,一般為相對於(A)成份之基礎聚合物100質量份,使用0~10質量份,特別是0~5質量份為佳。
本發明之有效作為蝕刻遮罩用之含金屬氧化物膜,可與使用含金屬氧化物之膜形成用組成物製造光阻膜之相同方法般,使用旋轉塗佈法等於基板上製作。旋轉塗佈後,使溶劑蒸發,為防止與上層光阻膜間之混合(Mixing),且促進交聯反應等目的而以進行燒焙為佳。燒焙溫度為於50~500℃之範圍内,以10~300秒之範圍内為佳。更佳之溫度範圍為,依所製造之裝置構造而有所不同,為避免裝置受到熱傷害,一般以400℃以下為佳。
又,本發明中,於被加工基板之被加工部份之上,介由下層膜而形成上述含矽之膜,於其上形成光阻膜,而可進行圖型之形成。
該情形,被加工基板之被加工部份,例如k值為3以下之低介電率絕緣膜、一次加工之低介電率絕緣膜、含有氮及/或氧之無機膜、金屬膜等。又,下層膜以有機膜為佳,又,形成光阻膜之光阻組成物以不含矽之化學増幅型光阻組成物為佳。
更詳細而言,被加工基板可為於基礎基板上形成被加工層(被加工部份)之物。基礎基板,並未有特別限定,其可使用Si、非晶質矽(α-Si)、p-Si、SiO2
、SiN、SiON、W、TiN、Al等與被加工層相異之材質亦可。被加工層,可使用Si、SiO2
、SiN、SiON、p-Si、α-Si、W、W-Si、Al、Cu、Al-Si等,及各種低介電膜及其蝕刻阻滯(Stopper)膜,通常可形成50~10,000nm,特別是100~5,000nm之厚度。
本發明中,上述含金屬氧化物膜與上層之光阻膜之間可形成市售之有機抗反射膜。此時,抗反射膜之構造可為具有芳香族取代基之化合物。該抗反射膜於以乾式蝕刻轉印上層光阻膜之圖型時,必須不會對上層光阻膜產生蝕刻負擔方可。例如,相對於上層光阻膜,其厚度為80%以下,較佳為50%以下之膜厚時,乾式蝕刻時僅會產生極小之負擔。
該情形,抗反射膜其最低之反射以調整為2%以下,較佳為1%以下,更佳為0.5%以下為宜。
本發明之含金屬氧化物膜於使用ArF準分子雷射光所進行之曝光製程之情形中,上層之光阻膜,均可使用通常ArF準分子雷射光用之光阻組成物。ArF準分子雷射光用光阻組成物已知具有多數候選組成物,為正型時,為經由酸之作用使酸不穩定基分解,而形成可溶於鹼水溶液之樹脂,與控制光酸發生劑及控制酸之擴散所使用之鹼性物質為主要成份,於負型時,為經由酸之作用而與交聯劑產生反應而形成不溶於鹼水溶液之樹脂,與光酸發生劑、交聯劑及控制酸之擴散之鹼性物質為主要成份,使用何種樹脂時,其特性將會有所差異。將所有公知之樹脂作大區分時,例如有聚(甲基)丙烯酸系、COMA(Cyclo Olefin Maleic Anhydride)系、COMA-(甲基)丙烯酸摻合物系、ROMP(式中,Ring Opening Methathesis Polymerization)系、聚降冰片烯系等,其中,又以使用聚(甲基)丙烯酸系樹脂之光阻組成物,其於側鏈導入脂環式骨架而可確保耐蝕刻性,故其解析性能相較於其他樹脂系更為優良。
使用聚(甲基)丙烯酸系樹脂之ArF準分子雷射用光阻組成物,其多數之內容皆為公知,於作為正型用時,皆為為確保主要機能之耐蝕刻性所使用之單位、經由酸之作用而分解變化為鹼可溶性之單位、確保密著性之單位等之組合,或必要時,含有以1個單位兼具有2個以上上述之機能的單位予以組合而構成聚合物。其中,基於酸使鹼溶解性產生變化之單位,例如,具有具金剛烷骨架之酸不穩定基的(甲基)丙烯酸酯(特開平9-73173號公報),或,具有具降冰片烷或四環十二烷骨架之酸不穩定基的(甲基)丙烯酸酯(特開2003-84438號公報),其可提供高解析性與耐蝕刻性,而為最佳使用者。又,為確保密著性之單位,例如,具有具內酯環之降冰片烷側鏈的(甲基)丙烯酸酯(國際公開第00/01684號公報)、具有氧雜降冰片烷側鏈之(甲基)丙烯酸酯(特開2000-159758號公報),或具有羥基金剛烷基側鏈之(甲基)丙烯酸酯(特開平8-12626號公報)等可提供良好之耐蝕刻性與高解析性,而為最佳使用者。又,例如具有鄰位為被氟取代而顯示出酸性之醇作為官能基之單位(例如,Polym. Mater. Sci. Eng. 1997. 77. pp449)包含於聚合物內時,可提供抑制聚合物膨潤之物性,且可提供高解析性,故特別於近年來極注目之植入(immersion)法中,作為對應之光阻聚合物而受到注目,聚合物中含有氟時,將會造成耐蝕刻性降低等問題。本發明之含金屬氧化物膜,對於前述不易確保耐蝕刻性之有機光阻組成物而言,特別是可有效使用者。
本發明之含金屬氧化物膜之使用例中,於製作含金屬氧化物膜層後,可於其上使用光阻組成物溶液製作光阻層,但以與含金屬氧化物膜層相同般,使用旋轉塗佈法為宜。光阻組成物於旋轉塗佈後,進行預燒焙,其以80~180℃、10~300秒之範圍內進行為佳。隨後進行曝光,曝光後燒焙(PEB)、顯影,而得光阻圖型。
本發明之含金屬氧化物膜作為蝕刻遮罩使用時,已使用含有氟龍(Flon)系氣體等含有氟之氣體為主成份的氣體進行蝕刻。本發明之含金屬氧化物膜對前述氣體具有蝕刻速度更快,上層之光阻膜的膜消減極小等特徵。
又,使用本發明之含金屬氧化物膜之多層光阻法,可於本發明之含金屬氧化物膜與被加工基板之間設置下層膜。下層膜作為被加工基板之蝕刻遮罩時,下層膜以具有芳香族骨架之有機膜為佳,下層膜為犧牲膜之情形等,除有機膜以外,只要矽含量為15質量%以下之膜時,也可為含矽之材料。
本發明之含金屬氧化物膜之其他使用例,例如將下層膜作為被加工基板之蝕刻遮罩之使用有機膜之多層光阻法。該有機膜,為於形成圖型之光阻圖型轉印於含金屬氧化物膜後,再將該圖型再一次轉印所得之膜,含金屬氧化物膜除應具有可於顯示高耐蝕刻性之蝕刻條件進行蝕刻加工之特性以外,對被加工基板進行蝕刻加工之條件也被要求應具有高耐蝕刻性之特性。
作為該些下層膜之有機膜,已知有多數被作為3層光阻法用,或使用矽光阻組成物之2層光阻法用之下層膜,例如除特開2005-128509號公報記載之4,4’-(9H-茀-9-茚)雙酚酚醛清漆樹脂(分子量11,000)以外,由酚醛清漆樹脂開始之多數之樹脂,已知皆被作為2層光阻法或3層光阻法之光阻下層膜材料,該些皆可使用於本發明中。又,通常欲提高較酚醛清漆為更高耐熱性之情形,可導入4,4’-(9H-茀-9-茚)雙酚酚醛清漆樹脂等多環式骨架,又,可選擇聚醯亞胺系樹脂(例如,特開2004-153125號公報)。
上述有機膜,可使用組成物溶液,依與光阻組成物相同之旋轉塗佈法等形成於基板上。使用旋轉塗佈法等形成光阻下層膜後,為使有機溶劑蒸發,以進行燒焙處理為佳。燒焙溫度為80~300℃之範圍内,以10~300秒之範圍内為較佳使用者。
又,並未有特別限定,但因蝕刻加工條件不同,下層膜之厚度以10nm以上,特別是50nm以上,又以50,000nm以下為佳,本發明之含金屬氧化物膜之厚度以1nm以上、200nm以下,光阻膜之厚度以1nm以上、300nm以下為佳。
使用本發明之含金屬氧化物膜之3層光阻法,係如以下所述。於該製程中,首先於被加工基板上使用旋轉塗佈法等製作有機膜。該有機膜,於對被加工基板蝕刻之際具有作為遮罩之作用,故期待其具有高耐蝕刻性,於尋求不會與上層之含金屬氧化物膜產生混合,故於旋轉塗佈後,以熱或酸進行交聯者為佳。於其上依前述方法依序形成本發明之組成物所得之含金屬氧化物膜、光阻膜。光阻膜,依以往之方法,使用對應於光阻膜之光源,例如使用KrF準分子雷射光,或ArF準分子雷射光、F2
雷射光、或EUV光,進行圖型曝光,並配合各個光阻膜之條件進行加熱處理後,以顯影液進行顯影操作而可得光阻圖型。其次,將該光阻圖型作為蝕刻遮罩,對光阻膜,以較含金屬氧化物膜之蝕刻速度為更優位之高乾式蝕刻條件,例如使用氟系氣體電漿之乾式蝕刻進行蝕刻。其結果,對光阻膜側邊蝕刻下幾乎不會使圖型變化產生任何影響下,即可得到含金屬氧化物膜圖型。其次,對上述所得到之具有轉印有光阻圖型之含金屬氧化物膜圖型之基板,以下層有機膜之蝕刻速度為更優位之高乾式蝕刻條件,例如使用含有氧之氣體電漿的反應性乾式蝕刻,或含有氫-氮之氣體電漿進行反應性乾式蝕刻,以對下層有機膜進行蝕刻加工。經由該蝕刻步驟而得到下層有機膜之圖型,同時最上層之光阻層,通常為消失掉。此外,其中所得之下層有機膜作為蝕刻遮罩,對被加工基板之乾式蝕刻,例如,使用氟系乾式蝕刻或氯系乾式蝕刻時,可使被加工基板於具有良好精確度下進行蝕刻加工。
以下,將以合成例及實施例與比較例對本發明作具體之說明,但本發明並不受該些記載所限定。又,下述例中,%表示質量%,分子量測定為依GPC所進行者。
於丙二醇甲基醚40g、甲烷磺酸1g及去離子水50g之混合物中,添加苯基三甲氧基矽烷10g、2-(3,4-環氧環己基)乙基三甲氧基矽烷20g、四丁氧基鍺10g及丙二醇甲基醚35g之混合物,於無任何處理下,保持12小時、40℃,經水解縮合後,將副產物之醇減壓餾除。於其中,加入乙酸乙酯800ml及丙二醇甲基醚300ml,使水層分液。殘留之有機層中,加入離子交換水100ml後,進行攪拌、靜置、分液。重複3次此一操作。殘留之有機層中加入丙二醇甲基醚200ml,減壓濃縮後得含金屬氧化物之化合物1的丙二醇甲基醚溶液100g(聚合物濃度20%)。所得溶液使用離子色層分析法對甲烷磺酸離子進行分析結果,得知並未檢測出。該物質使用聚苯乙烯換算分子量測定結果,Mw=3,000。
於丙二醇甲基醚40g、甲烷磺酸1g及去離子水50g之混合物中,添加苯基三甲氧基矽烷10g、2-(3,4-環氧環己基)乙基三甲氧基矽烷20g、四丁氧基鈦10g、2,4-戊二酮20g及丙二醇甲基醚35g之混合物,於無任何處理下,保持12小時、30℃,經水解縮合後,將副產物之醇減壓餾除。殘留之溶液中加入丙二醇甲基醚200ml,再經減壓濃縮得含金屬氧化物之化合物2之丙二醇甲基醚溶液120g(聚合物濃度20%)。該物質使用聚苯乙烯換算分子量測定結果,Mw=8,000。
於丙二醇乙基醚40g、鹽酸1g及去離子水50g之混合物中,添加苯基三甲氧基矽烷10g、2-(3,4-環氧環己基)乙基三甲氧基矽烷20g、四丙氧基鉿10g及丙二醇乙基醚35g之混合物,於無任何處理下,保持12小時、10℃,經水解縮合後,將副產物之醇減壓餾除。於殘留之溶液中加入丙二醇乙基醚200ml,更經減壓濃縮得含金屬氧化物之化合物3之丙二醇乙基醚溶液100g(聚合物濃度20%)。該物質使用聚苯乙烯換算分子量測定結果,Mw=5,000。
於離子交換水260g、35%鹽酸1g之混合物中,於室溫下加入四甲氧基矽烷70g、甲基三甲氧基矽烷25g、下述式[i]之矽烷化合物25g、三甲氧基鋁10g及苯基三甲氧基矽烷10g之混合物。於無任何處理下,於8小時室溫下進行水解縮合後,將副產物之甲醇減壓餾除。於其中,加入乙酸乙酯800ml及丙二醇丙基醚300ml,使水層分液。殘留之有機層中,加入離子交換水100ml後,進行攪拌、靜置、分液。重複3次此一操作。殘留之有機層中加入丙二醇單丙基醚200ml,經減壓濃縮後得含金屬氧化物之化合物4之丙二醇單丙基醚溶液300g(聚合物濃度20%)。所得之溶液使用離子色層分析法分析氯離子結果,得知並未檢測出。該物質使用聚苯乙烯換算分子量測定結果,Mw=2,500。
於乙醇200g、離子交換水100g、甲烷磺酸3g之混合物中,於室溫下加入四甲氧基矽烷40g、甲基三甲氧基矽烷10g、硼酸三甲酯50g及苯基三甲氧基矽烷10g之混合物。於無任何處理下,於8小時室溫下進行水解縮合後,將副產物之甲醇減壓餾除。於其中,加入乙酸乙酯800ml及乙二醇單丙基醚300ml,將水層分液。殘留之有機層中,加入離子交換水100ml後,進行攪拌、靜置、分液。重複3次此一操作。殘留之有機層中,加入乙二醇單丙基醚200ml,經減壓濃縮後得含金屬氧化物之化合物5之乙二醇單丙基醚溶液300g(聚合物濃度20%)。所得之溶液使用離子色層分析對甲烷磺酸離子進行分析結果,得知反應所使用之物質中,99%已被去除。該物質使用聚苯乙烯換算分子量測定結果,Mw=2,100。
於乙醇200g、離子交換水100g、甲烷磺酸3g之混合物中,於室溫下加入四甲氧基矽烷40g、甲基三甲氧基矽烷10g、2-(3,4-環氧環己基)乙基三甲氧基矽烷20g及苯基三甲氧基矽烷10g之混合物。於無任何處理下,於8小時室溫下進行水解縮合後,將副產物之甲醇減壓餾除。於其中,加入乙酸乙酯800ml及乙二醇單丙基醚300ml,將水層分液。殘留之有機層中,加入離子交換水100ml後,進行攪拌、靜置、分液。重複3次此一操作。殘留之有機層中,加入乙二醇單丙基醚200ml,經減壓濃縮後得含金屬氧化物之化合物6之乙二醇單丙基醚溶液300g(聚合物濃度20%)。所得之溶液使用離子色層分析法對甲烷磺酸離子進行分析結果,得知反應所使用之物質中,99%已被去除。該物質使用聚苯乙烯換算分子量測定結果,Mw=3,500。
將乙醇500g、離子交換水250g、25%氫氧化四甲基銨2.5g加入1,000ml玻璃燒瓶中,將該混合物於55℃下攪拌,於其中以2小時時間滴入四乙氧基矽烷97g、甲基三甲氧基矽烷73g之混合液。於55℃下攪拌1小時後,冷卻至室溫,加入20%馬來酸水溶液3g。隨後,於此溶液中,加入丙二醇單丙基醚1,000ml後,將溶液濃縮至900ml為止。隨後,加入乙酸乙酯2,000ml,使用離子交換水300ml洗淨2次,進行分液,隨後,將乙酸乙酯減壓濃縮得含矽之化合物7之丙二醇單丙基醚溶液900g(聚合物濃度7%)。該物質使用聚苯乙烯換算分子量測定結果,Mw=約10萬。
將離子交換水260g、65%硝酸5g加入1,000ml玻璃燒瓶中,再於室溫下加入四乙氧基矽烷70g、甲基三甲氧基矽烷70g及苯基三甲氧基矽烷10g之混合物。於無任何處理下,於8小時室溫下進行水解縮合後,將甲醇及副產物之乙醇減壓餾除。於其中,加入乙酸乙酯800ml及丙二醇單丙基醚300ml,將水層分液。殘留之有機層中加入1%馬來酸水溶液100ml後,進行攪拌、靜置、分液。重複2次此一操作後,加入離子交換水100ml後,進行攪拌、靜置、分液。重複3次此一操作。殘留之有機層中加入丙二醇單丙基醚200ml,經減壓濃縮後得含矽之化合物8之丙二醇單丙基醚溶液300g(聚合物濃度21%)。該物質使用聚苯乙烯換算分子量測定結果,Mw=2,000。
將上述合成例所得之含金屬氧化物之化合物1~6、含矽之化合物7、8、酸、熱交聯促進劑、溶劑、添加劑依表1所示比例混合,使用0.1μm之氟樹脂製過濾器過濾結果,分別製得含金屬氧化物之膜形成用組成物溶液,將其命為Sol.1~18。
TPSOAc:乙酸三苯基鋶(光分解性熱交聯促進劑)
TPSOH:氫氧化三苯基鋶(光分解性熱交聯促進劑)
TPSCl:氯化三苯基鋶(光分解性熱交聯促進劑)
TPSMA:馬來酸單(三苯基鋶)(光分解性熱交聯促進劑)
TPSN:硝酸三苯基鋶(光分解性熱交聯促進劑)
TMAOAc:乙酸四甲基銨(非光分解性熱交聯促進劑)
TPSNf:三苯基鋶九氟丁烷磺酸酯(光酸發生劑)
首先,將作為下層膜材料之含有4,4’-(9H-茀-9-茚)雙酚酚醛清漆樹脂(分子量11,000)(特開2005-128509號公報)之組成物(樹脂28質量份,溶劑(PGMEA)100質量份)迴轉塗佈於Si晶圓上,於200℃下加熱1分鐘後成膜,形成膜厚300nm之下層有機膜。作為此下層有機膜材料,除上述之外,例如由酚醛清漆樹脂為中心之多數樹脂,已知皆可作為多層光阻法之下層膜材料,故其皆可使用。
其次,將Sol.1~18迴轉塗佈,於200℃加熱1分鐘後成膜,形成膜厚100nm之含金屬氧化物膜。
隨後,為形成上層光阻膜,而將作為ArF準分子雷射光曝光用光阻組成物(式中,稱為Resistl)之下述物質溶解於含有FC-430(住友3M(股)製)0.1%之PGMEA(丙二醇單甲基醚乙酸酯)溶液中,再使用0.1μm之氟樹脂製過濾器經過濾而製得。
Mw=6,800
(Me為甲基,Et為乙基。) 10質量份
光酸發生劑:三苯基鋶九氟丁烷磺酸酯 0.2質量份
鹼性化合物:三乙醇胺 0.02質量份
將該組成物塗佈於含金屬氧化物之中間層之上,經130℃、60秒鐘燒焙後,形成膜厚200nm之光阻層。
其次,使用ArF曝光裝置((股)理光製;S305B、NA0.68、σ0.85、2/3輪體照明、Cr遮罩)進行曝光,再於110℃下進行90秒鐘之燒焙(PEB),使用2.38%氫氧化四甲基銨(TMAH)水溶液進行顯影,得正型之圖型。觀察所得圖型之90nml/S之圖型形狀之結果記載如表2所示。
無論任一實施例中,皆得到未在基板附近出現邊緣捲曲或凹陷、混合(Intermixing)現象之圖型。
其次,進行耐乾式蝕刻性之試驗。將上述組成物Sol.1~18迴轉塗佈,於200℃加熱1分鐘後成膜,製得膜厚100nm之含金屬氧化物膜Film1~18。將該些膜,與下層膜及光阻膜依下述之蝕刻條件(1)實施蝕刻試驗。其結果如表3所示。
(1)使用CHF3
/CF4
系氣體之蝕刻試驗裝置:東京電子(股)製乾式蝕刻裝置TE-8500P蝕刻條件(1):
反應室壓力 40.0Pa
RF能量 1,300W
間隙 9mm
CHF3
氣體流量 30ml/min
CF4
氣體流量 30ml/min
Ar氣體流量 100ml/min
處理時間 10sec
隨後,依表4所示般,將O2
系氣體之乾式蝕刻速度依下述所示蝕刻條件(2)進行調查。其與下層膜或上層光阻膜相比較時,為十分遲緩,得知將含金屬氧化物之中間層作為蝕刻遮罩對下層進行圖型轉印為可能者。
蝕刻條件(2):
反應室壓力 60.0Pa
RF能量 600W
Ar氣體流量 40ml/min
O2
氣體流量 60ml/min
間隙 9mm
處理時間 20sec
隨後,進行保存安定性試驗。將上述所得之含金屬氧化物之膜形成用組成物(Sol.1~18)於30℃下保管3個月後,依上述方法再度進行塗佈,進行成膜性是否會產生變化之試驗。其結果如表5所示。
由表5之結果,確認無論任一實施例之組成物中,皆具有30℃、3個月以上,換算為室溫為具有6個月以上之保存安定性。
由以上結果得知,本發明之組成物、含金屬氧化物膜,為具有優良之安定性、微影蝕刻特性者。使用該些組成物,可以最先端之高NA曝光機形成圖型與並可以蝕刻對基板進行加工。
Claims (20)
- 一種熱硬化性含金屬氧化物之膜形成用組成物,其特徵為,含有(A)通式(1)所表示之1種或2種以上之水解性矽化合物與通式(2)所表示之1種或2種以上之水解性金屬化合物經水解縮合所得之含金屬氧化物之化合物,R1 m1 Si(OR)(4-m1) (1)(式中,R為碳數1~3之烷基,R1 為由甲基、乙基、苯基及下式所示基中選出之基
- 如申請專利範圍第1項之熱硬化性含金屬氧化物之膜形成用組成物,其尚含有(E)通式(5)所表示之1種或2種以上之水解性矽化合物經水解縮合所得之含矽之化合物,R6 m6 Si(OR9 )(4-m6) (5)(式中,R9 為碳數1~6之烷基,R6 為甲基、乙基或苯基,m6為0或1)。
- 如申請專利範圍第1或2項之熱硬化性含金屬氧化物之膜形成用組成物,其為含有使用由無機酸及磺酸衍生物中選出之1種以上之化合物作為酸觸媒,以使通式(1)及(2)之化合物經水解縮合所得之含金屬氧化物之化合物。
- 如申請專利範圍第3項之熱硬化性含金屬氧化物之膜形成用組成物,其為含有可經由從上述之水解縮合所得之含金屬氧化物之化合物的反應混合物中,實質上去除上述酸觸媒之步驟所得之含金屬氧化物之化合物。
- 如申請專利範圍第1或2項之熱硬化性含金屬氧化物之膜形成用組成物,其中上述以通式(1)表示之水解 性含矽化合物為由四甲氧基矽烷、甲基三甲氧基矽烷、苯基三甲氧基矽烷、2-(3,4-環氧環己基)乙基三甲氧基矽烷、及以下式
- 如申請專利範圍第1或2項之熱硬化性含金屬氧化物之膜形成用組成物,其中,以通式(2)所示之水解性金屬化合物為由四丁氧基鍺、四丁氧基鈦、四丙氧基鉿、三甲氧基鋁、及硼酸三甲酯中選出。
- 如申請專利範圍第1或2項之熱硬化性含金屬氧化物之膜形成用組成物,其中,通式(1)所表示之化合物與通式(2)所表示之化合物之莫耳比為(1)>(2)。
- 如申請專利範圍第1或2項之熱硬化性含金屬氧化物之膜形成用組成物,其中,上述(C)成分為由草酸、馬來酸、甲酸、乙酸、丙酸、及檸檬酸中選出。
- 如申請專利範圍第1或2項之熱硬化性含金屬氧化物之膜形成用組成物,其中,上述(D)成分為由乙二醇、二乙二醇、三乙二醇、丙二醇、二丙二醇、丁二醇、及戊二醇之單烷基醚中選出。
- 如申請專利範圍第1或2項之熱硬化性含金屬氧化物之膜形成用組成物,其尚包含水。
- 如申請專利範圍第1或2項之熱硬化性含金屬氧 化物之膜形成用組成物,其尚含有光酸發生劑。
- 如申請專利範圍第1或2項之熱硬化性含金屬氧化物之膜形成用組成物,其尚含有具有以環狀醚作為取代基之1價或2價以上之醇。
- 一種由申請專利範圍第1~12項中任一項之組成物所形成之含金屬氧化物膜,其特徵為,於被加工基板上形成有機膜,於其上形成含金屬氧化物膜,再於其上使用不含矽之化學增幅型光阻組成物形成光阻膜,對該光阻膜進行圖型加工後,使用該光阻膜圖型對含金屬氧化物膜進行圖型加工,以加工後之含金屬氧化物膜圖型作為蝕刻遮罩對下層之有機膜進行圖型加工,更將加工後之有機膜作為蝕刻遮罩對被加工基板進行蝕刻之多層光阻法中所使用之含金屬氧化物膜。
- 一種基板,其特徵為,依序形成有機膜,與該有機膜上由申請專利範圍第1~12項中任一項之組成物所形成之含金屬氧化物膜,與於其上之光阻膜所得者。
- 如申請專利範圍第14項之基板,其中,含金屬氧化物膜與光阻膜之間介有有機抗反射膜。
- 如申請專利範圍第14或15項之基板,其中,上述有機膜為具有芳香族骨架之膜。
- 一種圖型形成方法,其為基板上形成圖型之方法,其特徵為,準備如申請專利範圍第14項之基板,使該基板之光阻膜的圖型電路區域曝光後,以顯影液顯影於光阻膜上形成光阻圖型,使用形成該光阻圖型之光阻膜作為 蝕刻遮罩,對含金屬氧化物膜進行乾式蝕刻,以形成圖型之含金屬氧化物膜作為蝕刻遮罩,對有機膜進行蝕刻,以形成圖型之有機膜作為遮罩對基板進行蝕刻,而於基板上形成圖型。
- 一種圖型形成方法,其為基板上形成圖型之方法,其特徵為,準備如申請專利範圍第15項之基板,使該基板之光阻膜的圖型電路區域曝光後,以顯影液顯影於光阻膜上形成光阻圖型,使用形成該光阻圖型之光阻膜作為蝕刻遮罩,對有機抗反射膜及含金屬氧化物膜進行乾式蝕刻,以形成圖型之含金屬氧化物膜作為蝕刻遮罩,對有機膜進行蝕刻,以形成圖型之有機膜作為遮罩對基板進行蝕刻,而於基板上形成圖型。
- 如申請專利範圍第17或18項之圖型形成方法,其中,上述有機膜為具有芳香族骨架之膜。
- 如申請專利範圍第17或18項之圖型形成方法,其於光阻圖型之形成中,為使用光微影蝕刻法,該光微影蝕刻法為使用波長300nm以下之光。
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JP4793592B2 (ja) | 2011-10-12 |
US8026038B2 (en) | 2011-09-27 |
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US20090136869A1 (en) | 2009-05-28 |
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