TWI567784B - 半導體裝置基板之製造方法 - Google Patents
半導體裝置基板之製造方法 Download PDFInfo
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- TWI567784B TWI567784B TW104128244A TW104128244A TWI567784B TW I567784 B TWI567784 B TW I567784B TW 104128244 A TW104128244 A TW 104128244A TW 104128244 A TW104128244 A TW 104128244A TW I567784 B TWI567784 B TW I567784B
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- Prior art keywords
- film
- semiconductor device
- ruthenium
- group
- device substrate
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- 239000000758 substrate Substances 0.000 title claims description 90
- 239000004065 semiconductor Substances 0.000 title claims description 78
- 238000004519 manufacturing process Methods 0.000 title claims description 56
- -1 polysiloxane Polymers 0.000 claims description 147
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 109
- 229910052707 ruthenium Inorganic materials 0.000 claims description 109
- 239000000203 mixture Substances 0.000 claims description 86
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- 238000000034 method Methods 0.000 claims description 45
- 238000005468 ion implantation Methods 0.000 claims description 34
- 125000000962 organic group Chemical group 0.000 claims description 34
- 239000002904 solvent Substances 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 27
- 239000002253 acid Substances 0.000 claims description 26
- 238000001312 dry etching Methods 0.000 claims description 25
- 229910052731 fluorine Inorganic materials 0.000 claims description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 20
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- 229910052733 gallium Inorganic materials 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 15
- 239000011737 fluorine Substances 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 13
- 150000002500 ions Chemical class 0.000 claims description 13
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- 150000004706 metal oxides Chemical class 0.000 claims description 8
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- 229910052787 antimony Inorganic materials 0.000 claims description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 4
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- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical group C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 claims description 3
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- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
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- 239000007943 implant Substances 0.000 claims description 2
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- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 2
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- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims 2
- 239000000178 monomer Substances 0.000 description 80
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- 125000002178 anthracenyl group Chemical group C1(=CC=CC2=CC3=CC=CC=C3C=C12)* 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 125000001204 arachidyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 125000002619 bicyclic group Chemical group 0.000 description 1
- GPRLTFBKWDERLU-UHFFFAOYSA-N bicyclo[2.2.2]octane Chemical compound C1CC2CCC1CC2 GPRLTFBKWDERLU-UHFFFAOYSA-N 0.000 description 1
- 150000003519 bicyclobutyls Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 239000005380 borophosphosilicate glass Substances 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- BSDOQSMQCZQLDV-UHFFFAOYSA-N butan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] BSDOQSMQCZQLDV-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 125000004106 butoxy group Chemical group [*]OC([H])([H])C([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- UADDLHRDLMMBQG-UHFFFAOYSA-N butoxyboron Chemical compound [B]OCCCC UADDLHRDLMMBQG-UHFFFAOYSA-N 0.000 description 1
- PZRCTEHEHLNVEC-UHFFFAOYSA-N butoxyhydrazine Chemical compound CCCCONN PZRCTEHEHLNVEC-UHFFFAOYSA-N 0.000 description 1
- DOBSQSLSWMMIEM-UHFFFAOYSA-N butoxytin Chemical compound CCCCO[Sn] DOBSQSLSWMMIEM-UHFFFAOYSA-N 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004744 butyloxycarbonyl group Chemical group 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 229940075419 choline hydroxide Drugs 0.000 description 1
- HNEGQIOMVPPMNR-IHWYPQMZSA-N citraconic acid Chemical compound OC(=O)C(/C)=C\C(O)=O HNEGQIOMVPPMNR-IHWYPQMZSA-N 0.000 description 1
- 229940018557 citraconic acid Drugs 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 229940125904 compound 1 Drugs 0.000 description 1
- 229940125773 compound 10 Drugs 0.000 description 1
- 229940125797 compound 12 Drugs 0.000 description 1
- 229940125782 compound 2 Drugs 0.000 description 1
- 229940126214 compound 3 Drugs 0.000 description 1
- 229940125898 compound 5 Drugs 0.000 description 1
- AJEHNBIPLQJTNU-UHFFFAOYSA-N cyanomethyl acetate Chemical compound CC(=O)OCC#N AJEHNBIPLQJTNU-UHFFFAOYSA-N 0.000 description 1
- UCIYGNATMHQYCT-OWOJBTEDSA-N cyclodecene Chemical compound C1CCCC\C=C\CCC1 UCIYGNATMHQYCT-OWOJBTEDSA-N 0.000 description 1
- ARUKYTASOALXFG-UHFFFAOYSA-N cycloheptylcycloheptane Chemical compound C1CCCCCC1C1CCCCCC1 ARUKYTASOALXFG-UHFFFAOYSA-N 0.000 description 1
- FJFKIPQEUBVHPU-UHFFFAOYSA-N cyclohexyloxycyclohexane;titanium Chemical compound [Ti].C1CCCCC1OC1CCCCC1 FJFKIPQEUBVHPU-UHFFFAOYSA-N 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 239000012973 diazabicyclooctane Substances 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 229960005215 dichloroacetic acid Drugs 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- QAIDPMSYQQBQTK-UHFFFAOYSA-N diethylgallium Chemical compound CC[Ga]CC QAIDPMSYQQBQTK-UHFFFAOYSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 1
- OREAFAJWWJHCOT-UHFFFAOYSA-N dimethylmalonic acid Chemical compound OC(=O)C(C)(C)C(O)=O OREAFAJWWJHCOT-UHFFFAOYSA-N 0.000 description 1
- 125000005982 diphenylmethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 description 1
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 description 1
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- UARGAUQGVANXCB-UHFFFAOYSA-N ethanol;zirconium Chemical compound [Zr].CCO.CCO.CCO.CCO UARGAUQGVANXCB-UHFFFAOYSA-N 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- RSIHJDGMBDPTIM-UHFFFAOYSA-N ethoxy(trimethyl)silane Chemical compound CCO[Si](C)(C)C RSIHJDGMBDPTIM-UHFFFAOYSA-N 0.000 description 1
- FKDLBUPSJQZYFZ-UHFFFAOYSA-N ethoxy-ethyl-dimethylsilane Chemical compound CCO[Si](C)(C)CC FKDLBUPSJQZYFZ-UHFFFAOYSA-N 0.000 description 1
- WFSULZXQWNUZPF-UHFFFAOYSA-N ethoxyaluminum Chemical compound CCO[Al] WFSULZXQWNUZPF-UHFFFAOYSA-N 0.000 description 1
- LRANRHDJNHABBA-UHFFFAOYSA-N ethoxyarsenic Chemical compound CCO[As] LRANRHDJNHABBA-UHFFFAOYSA-N 0.000 description 1
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- 125000003754 ethoxycarbonyl group Chemical group C(=O)(OCC)* 0.000 description 1
- HIWDBXCAECYPGA-UHFFFAOYSA-N ethoxygallium Chemical compound CCO[Ga] HIWDBXCAECYPGA-UHFFFAOYSA-N 0.000 description 1
- FANAUDUYRDVPHX-UHFFFAOYSA-N ethoxytin Chemical compound CCO[Sn] FANAUDUYRDVPHX-UHFFFAOYSA-N 0.000 description 1
- 125000004672 ethylcarbonyl group Chemical group [H]C([H])([H])C([H])([H])C(*)=O 0.000 description 1
- UKFXDFUAPNAMPJ-UHFFFAOYSA-N ethylmalonic acid Chemical compound CCC(C(O)=O)C(O)=O UKFXDFUAPNAMPJ-UHFFFAOYSA-N 0.000 description 1
- LIWAQLJGPBVORC-UHFFFAOYSA-N ethylmethylamine Chemical compound CCNC LIWAQLJGPBVORC-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000007687 exposure technique Methods 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- CATSNJVOTSVZJV-UHFFFAOYSA-N heptan-2-one Chemical compound CCCCCC(C)=O CATSNJVOTSVZJV-UHFFFAOYSA-N 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- PNLSQMMDWXZWHO-UHFFFAOYSA-N hexoxyboron Chemical compound [B]OCCCCCC PNLSQMMDWXZWHO-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 125000003454 indenyl group Chemical group C1(C=CC2=CC=CC=C12)* 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 235000013847 iso-butane Nutrition 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- ZLVXBBHTMQJRSX-VMGNSXQWSA-N jdtic Chemical compound C1([C@]2(C)CCN(C[C@@H]2C)C[C@H](C(C)C)NC(=O)[C@@H]2NCC3=CC(O)=CC=C3C2)=CC=CC(O)=C1 ZLVXBBHTMQJRSX-VMGNSXQWSA-N 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
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- 238000001459 lithography Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- ZEIWWVGGEOHESL-UHFFFAOYSA-N methanol;titanium Chemical compound [Ti].OC.OC.OC.OC ZEIWWVGGEOHESL-UHFFFAOYSA-N 0.000 description 1
- IKGXNCHYONXJSM-UHFFFAOYSA-N methanolate;zirconium(4+) Chemical compound [Zr+4].[O-]C.[O-]C.[O-]C.[O-]C IKGXNCHYONXJSM-UHFFFAOYSA-N 0.000 description 1
- FTWKTOVWPKRLHM-UHFFFAOYSA-N methoxyaluminum Chemical compound CO[Al] FTWKTOVWPKRLHM-UHFFFAOYSA-N 0.000 description 1
- GHAMDDWKPOYZGV-UHFFFAOYSA-N methoxyarsenic Chemical compound CO[As] GHAMDDWKPOYZGV-UHFFFAOYSA-N 0.000 description 1
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- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- ZIYVHBGGAOATLY-UHFFFAOYSA-N methylmalonic acid Chemical compound OC(=O)C(C)C(O)=O ZIYVHBGGAOATLY-UHFFFAOYSA-N 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- PSHKMPUSSFXUIA-UHFFFAOYSA-N n,n-dimethylpyridin-2-amine Chemical compound CN(C)C1=CC=CC=N1 PSHKMPUSSFXUIA-UHFFFAOYSA-N 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical group CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- UMRZSTCPUPJPOJ-KNVOCYPGSA-N norbornane Chemical compound C1C[C@H]2CC[C@@H]1C2 UMRZSTCPUPJPOJ-KNVOCYPGSA-N 0.000 description 1
- 125000002868 norbornyl group Chemical group C12(CCC(CC1)C2)* 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 229960002446 octanoic acid Drugs 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- 125000004043 oxo group Chemical group O=* 0.000 description 1
- 125000005702 oxyalkylene group Chemical group 0.000 description 1
- 125000005740 oxycarbonyl group Chemical group [*:1]OC([*:2])=O 0.000 description 1
- AZCUJQOIQYJWQJ-UHFFFAOYSA-N oxygen(2-) titanium(4+) trihydrate Chemical compound [O-2].[O-2].[Ti+4].O.O.O AZCUJQOIQYJWQJ-UHFFFAOYSA-N 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- VOPZDTIRUBJGNT-UHFFFAOYSA-N pentoxyboron Chemical compound [B]OCCCCC VOPZDTIRUBJGNT-UHFFFAOYSA-N 0.000 description 1
- 125000001148 pentyloxycarbonyl group Chemical group 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 125000005561 phenanthryl group Chemical group 0.000 description 1
- IFFPHDYFQRRKPZ-UHFFFAOYSA-N phenol;titanium Chemical compound [Ti].OC1=CC=CC=C1.OC1=CC=CC=C1.OC1=CC=CC=C1.OC1=CC=CC=C1 IFFPHDYFQRRKPZ-UHFFFAOYSA-N 0.000 description 1
- AVKUWNUBPFREQI-UHFFFAOYSA-N phenoxyarsenic Chemical compound [As]OC1=CC=CC=C1 AVKUWNUBPFREQI-UHFFFAOYSA-N 0.000 description 1
- PIZWVRTVVYPAID-UHFFFAOYSA-N phenoxyboron Chemical compound [B]OC1=CC=CC=C1 PIZWVRTVVYPAID-UHFFFAOYSA-N 0.000 description 1
- CSRCVZZUZZRSEH-UHFFFAOYSA-M phenoxytin Chemical compound [Sn]OC1=CC=CC=C1 CSRCVZZUZZRSEH-UHFFFAOYSA-M 0.000 description 1
- 229960004838 phosphoric acid Drugs 0.000 description 1
- DLYUQMMRRRQYAE-UHFFFAOYSA-N phosphorus pentoxide Inorganic materials O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 description 1
- 239000001294 propane Chemical group 0.000 description 1
- PMBLYMFPRDUCBQ-UHFFFAOYSA-N propoxyboron Chemical compound [B]OCCC PMBLYMFPRDUCBQ-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000010421 standard material Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 125000000547 substituted alkyl group Chemical group 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 125000005931 tert-butyloxycarbonyl group Chemical group [H]C([H])([H])C(OC(*)=O)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 125000004192 tetrahydrofuran-2-yl group Chemical group [H]C1([H])OC([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 125000004187 tetrahydropyran-2-yl group Chemical group [H]C1([H])OC([H])(*)C([H])([H])C([H])([H])C1([H])[H] 0.000 description 1
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 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
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-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
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 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
- OPSWAWSNPREEFQ-UHFFFAOYSA-K triphenoxyalumane Chemical compound [Al+3].[O-]C1=CC=CC=C1.[O-]C1=CC=CC=C1.[O-]C1=CC=CC=C1 OPSWAWSNPREEFQ-UHFFFAOYSA-K 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
- 229940005605 valeric acid Drugs 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
-
- 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
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Description
本發明係關於在半導體裝置之製造步驟,於半導體裝置基板上形成電晶體、電路時之製造方法。
半導體裝置之高整合化係利用微影光源之短波長化及選擇相應之適當光阻組成物以獲致圖案尺寸之微細化而達成。但是由EUV曝光技術之延遲,造成光源之短波長化所致圖案尺寸之微細化鈍化。而最先進的半導體裝置的高整合化的相關研發,專注在以貫通配線實施半導體裝置之疊層化、3維電晶體形成等。尤其3維電晶體不只是半導體裝置之高整合化,關於高速動作且低耗電方面也受到重視。
習知的平面型電晶體之製造處理中,因為平面型電晶體形成用基板之凹凸較小,係以單層光阻處理、有機抗反射膜與單層光阻所為之圖案化(以下稱為2層處理)為主流。但是由FIN-FET結構構成之3維電晶體之製造處理因形成比較
立體的結構,故基板之凹凸比平面型大,越來越難以用習知的2層處理形成此結構。
而作為解決此問題之一方法,有人探討利用3層處理法形成圖案。3層處理法,係使光阻膜,亦即和光阻上層膜有不同蝕刻選擇性之光阻下層膜插入於光阻上層膜與有機下層膜之間,於光阻上層膜獲得圖案後,將上層光阻圖案作為蝕刻遮罩,利用乾蝕刻在光阻下層膜轉印圖案,然後將其作為蝕刻遮罩,利用乾蝕刻在有機下層膜轉印圖案,再將其作為蝕刻遮罩,利用乾蝕刻在被加工基板轉印圖案之方法。通常、對於光阻上層膜與有機下層膜兩者有良好蝕刻選擇性之含矽膜適合作為光阻下層膜(專利文獻1)。
具體的3層處理法,係以有適當厚度之有機下層膜將凹凸大的3維電晶體形成用基板予以平坦化,並為了將有機下層膜加工,插入含矽之光阻下層膜作為硬遮罩,並將於上層光阻形成之圖案作為蝕刻遮罩,而於含矽之光阻下層膜轉印圖案,將此轉印之圖案作為遮罩,可以將有機下層膜加工。此方法已廣泛使用於半導體裝置之配線步驟。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本特開2007-199653號公報
上述3層處理法使用於3維電晶體形成處理時,須將作為離子植入(離子注入)之遮罩使用後之含矽之光阻下層膜與有機下層膜(以下也將其稱為下層膜殘渣)以對於基板不造成損害地除去。於習知配線步驟,雖能將下層膜殘渣利用乾蝕刻除去,但是於電晶體形成步驟,將下層膜殘渣以乾蝕刻除去時會發生對於基板之損害,成為問題。
本發明有鑑於上述問題,目的為提供一種半導體裝置基板之製造方法,其使用含矽膜,將以乾蝕刻形成之有含矽膜之一部分或全部殘留之有機下層膜圖案作為離子注入之遮罩使用後,以剝離液輕易且對於半導體裝置基板不造成損害地進行濕式剝離。
為了解決上述課題,本發明提供一種半導體裝置基板之製造方法,包含以下步驟:(1)在半導體裝置製造用被加工體基板上形成有機下層膜,於該有機下層膜上塗佈含矽膜形成用組成物並加熱,以形成矽含量為1質量%以上30質量%以下之含矽膜;(2)在該含矽膜上塗佈含有因酸作用而改變極性而對於顯影液之溶解度改變之聚合物之光阻組成物,並形成光阻膜;(3)將該光阻膜曝光、顯影而形成光阻圖案;(4)將該光阻圖案作為乾蝕刻遮罩,利用乾蝕刻於前述含矽膜轉印圖案;(5)將該已轉印圖案之含矽膜作為乾蝕刻遮罩,利用乾蝕刻於前述有機下層膜轉印圖案,並於圖案轉印後使前述含矽膜之一部分或全部殘留於前述已轉印圖案之有機下層膜上;
(6)將前述已轉印圖案之有機下層膜作為遮罩,對於前述半導體裝置製造用被加工體基板注入離子;及(7)以剝離液將作為前述離子注入之遮罩使用之殘留前述含矽膜之一部分或全部之有機下層膜予以剝離。
若為如此之半導體裝置基板之製造方法,在使用了圖案密合性優異之含矽膜之半導體裝置基板之製造方法,能將離子注入使用之遮罩以剝離液輕易且對於半導體裝置基板不造成損害地進行濕式剝離。
此時,於前述(6)步驟,可將以前述含矽膜之一部分或全部及前述有機下層膜形成之圖案作為遮罩,對於前述半導體裝置製造用被加工體基板注入離子。
如此,本發明中,可以以將含矽膜及有機下層膜形成之圖案作為遮罩以進行離子注入。
又,此時於前述(7)步驟,宜將作為前述離子注入之遮罩使用之前述含矽膜之一部分或全部有殘留之有機下層膜同時以剝離液剝離較佳。
若如上述,同時剝離,能更有效率地進行剝離。
此時,前述剝離液宜使用含有過氧化氫者較佳。
若為如此之剝離液,特別適合含矽膜之剝離。
又,此時,前述剝離液宜使用含硫酸者較佳。
藉由使用含有硫酸的剝離液,可促進剝離。
此時,前述(7)步驟中,於以前述剝離液處理後,更以含氟離子之剝離液進行剝離較佳。
藉此,能更確實地將離子注入使用之遮罩予以剝離。
此時,於前述(7)步驟,以前述剝離液處理後,宜更以含氨之洗滌液洗滌較佳。
藉此,能將剝離後之半導體裝置基板所附著的雜質除去。
此時,前述半導體裝置製造用被加工體基板宜使用已形成半導體電路之一部分或全部之半導體裝置基板、或已於該半導體裝置基板成膜了金屬膜、非晶金屬膜、金屬碳化膜、金屬氧化膜、金屬氮化膜、金屬氧化碳化膜、及金屬氧化氮化膜中任一者的基板較佳。
此時,前述金屬宜包括矽、鈦、鎢、鉿、鋯、鉻、鍺、銅、銀、金、鋁、銦、鎵、砷、鈀、鐵、鉭、銥、鉬、或該等之合金較佳。
本發明,可理想地使用如此之半導體裝置製造用被加工體基板。
此時,前述離子注入之離子物種宜為硼、磷、砷、碳、氮、氧、氟、氬、矽、鎵、鍺、銦、及銻中任一者較佳。
若為如此之離子物種,適合作為注入之離子。
又,此時前述含矽膜形成用組成物宜使用至少含有聚矽氧烷及溶劑者較佳。
若為如此之含矽膜形成用組成物,能形成高品質之含矽膜,適合用在本發明。
此時,前述聚矽氧烷宜使用含有交聯性有機基者較佳。
如上,藉由含有交聯性有機基,能形成密合性更良好的含矽膜。
此時,前述交聯性有機基宜為環氧基、苯酚基、及萘酚基中之任一者較佳。
若為如此之交聯性有機基,能確實地形成密合性良好的含矽膜。
此時,前述聚矽氧烷宜使用含有鹵化有機基者較佳。
如上,藉由含有鹵化有機基,能更確實地將離子注入使用之遮罩予以剝離。
此時,前述鹵化有機基之鹵素宜為氟或氯較佳。
若為如此之鹵化有機基,能更確實地將離子注入使用之遮罩予以剝離。
此時,前述含矽膜形成用組成物可使用更含有因熱、光、或此兩者之作用而產生酸之酸產生劑者。
此時,前述含矽膜形成用組成物可使用更含有含氟之有機化合物。
此時,前述含矽膜形成用組成物可使用更含有交聯劑者。
如上,本發明使用之含矽膜形成用組成物也可含有該等添加劑。
如上,若為發明之半導體裝置基板之製造方法,藉由調整含矽膜中之矽含量成預定之範圍,即使有含矽膜之一部分或全部殘留在有機下層膜上,仍可利用例如剝離液和有機下層膜同時剝離並除去。所以,當將以含矽膜與有機下層膜形成之圖案作為離子注入之遮罩時,能於離子注入後以剝離液輕易且不對於半導體裝置基板造成損害地進行濕式剝離。如上,因能對於以3層處理進行離子注入後之基板不造成損害地加工,故本發明特別適合3維電晶體之製造。
1‧‧‧半導體裝置製造用被加工體基板
2‧‧‧有機下層膜
3‧‧‧含矽膜
4‧‧‧光阻膜
4’‧‧‧光阻圖案
圖1(0)~(7)顯示本發明之半導體裝置基板之製造方法之一例之流程圖。
如上述,尋求開發:於使用含矽膜之半導體裝置基板之製造方法,能將離子注入使用之遮罩以剝離液輕易且不對於半導體裝置基板造成損害地進行濕式剝離之半導體裝置基板之製造方法。
本案發明人等為了解決上述課題而努力研究,發現:將殘留含矽膜之有機下層膜作為遮罩實施離子注入,且之後去除遮罩(下層膜殘渣)之方法中,設含矽膜之矽含量為1質量%以上30質量%以下,並於離子注入後以剝離液處理,則可輕易且對於基板不造成損害地進行濕式剝離,乃完成本發明。
亦即,本發明係一種半導體裝置基板之製造方法,包含以下步驟:(1)於半導體裝置製造用被加工體基板上形成有機下層膜,在該有機下層膜上塗佈含矽膜形成用組成物並加熱,以形成矽含量為1質量%以上30質量%以下之含矽膜;(2)在含矽膜上塗佈含有因酸作用而改變極性並改變對於顯影液之溶解度之聚合物之光阻組成物,而形成光阻膜;(3)將該光阻膜曝光、顯影而形成光阻圖案;(4)將該光阻圖案作為乾蝕刻遮罩,利用乾蝕刻於前述含矽膜轉印圖案;(5)將該已轉印圖案之含矽膜作為乾蝕刻遮罩,利用乾蝕刻於前述有機下層膜轉印圖案,並於圖案轉印後使前述含矽膜之一部分或全部殘留於前述已轉印圖案之有機下層膜上;(6)將前述已轉印圖案之有機下層膜作為遮罩,對於前述半導體裝置製造用被加工體基板注入離子;及
(7)以剝離液將作為前述離子注入之遮罩使用之殘留前述含矽膜之一部分或全部之有機下層膜予以剝離。
以下針對本發明詳細說明,但本發明不限於此等。
又,本說明書中,Me表示甲基,Et表示乙基,Ac表示乙醯基。
[半導體裝置製造用被加工體基板]
本發明中,就半導體裝置製造用被加工體基板(被加工體)而言,宜使用已形成半導體電路之一部分或全部之半導體裝置基板,或在該半導體裝置基板已成膜金屬膜、非晶金屬膜、金屬碳化膜、金屬氧化膜、金屬氮化膜、金屬氧化碳化膜、及金屬氧化氮化膜中任一膜作為被加工層(被加工部分)的基板較佳。
半導體裝置基板一般使用矽基板,但無特殊限定,可使用Si、非晶矽(α-Si)、p-Si、SiO2、SiN、SiON、W、TiN、Al等和被加工層為不同的材質者。
作為構成被加工體之金屬,可使用包括矽、鈦、鎢、鉿、鋯、鉻、鍺、銅、銀、金、鋁、銦、鎵、砷、鈀、鐵、鉭、銥、鉬、或該等之合金者,含如此之金屬之被加工層,可使用例如:Si、SiO2、SiN、SiON、SiOC、p-Si、α-Si、TiN、BPSG、SOG、Cr、CrO、CrON、MoSi、W、W-Si、Al、Cu、Al-Si等及各種低介電膜及其蝕刻阻擋膜,膜厚為50~10,000nm較理想、100~5,000nm更理想。
[有機下層膜]
本發明中,在半導體裝置製造用被加工體基板上形成之有機下層膜只要是利用公知方法、材料形成者即可,只要能以後述剝離液剝離者即可,並無特殊限定。有機下層膜之膜厚不特別限定,約100nm至500nm較佳。
[含矽膜]
本發明中,在有機下層膜上形成之含矽膜只要是藉由將含矽膜形成用組成物塗佈並加熱而形成者即可,但含矽膜中之矽含量必須為1質量%以上30質量%以下。針對矽含量將於後述。
本發明中,含矽膜形成用組成物宜使用至少含有聚矽氧烷與溶劑者較佳。
本發明使用之含矽膜形成用組成物含有之聚矽氧烷,宜含有下列通式(A-1)表示之化合物、其水解物、其縮合物、其水解縮合物中之1種以上較佳。
R1A A1R2A A2R3A A3Si(OR0A)(4-A1-A2-A3) (A-1)
(式中,R0A為碳數1~6之烴基,R1A、R2A、R3A為氫原子或1價之有機基。又,A1、A2、A3為0或1,0≦A1+A2+A3≦3。)
作為聚矽氧烷之原料(起始物質)之通式(A-1)表示之水解性矽化合物(烷氧基矽烷)可列舉如下。
四烷氧基矽烷可列舉四甲氧基矽烷、四乙氧基矽烷、四丙氧基矽烷、四異丙氧基矽烷等。
作為三烷氧基矽烷,可列舉:三甲氧基矽烷、三乙氧基矽烷、三丙氧基矽烷、三異丙氧基矽烷、甲基三甲氧基矽烷、甲基三乙氧基矽烷、甲基三丙氧基矽烷、甲基三異丙氧基矽烷、乙基三甲氧基矽烷、乙基三乙氧基矽烷、乙基三丙氧基矽烷、乙基三異丙氧基矽烷、乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、乙烯基三丙氧基矽烷、乙烯基三異丙氧基矽烷、丙基三甲氧基矽烷、丙基三乙氧基矽烷、丙基三丙氧基矽烷、丙基三異丙氧基矽烷、異丙基三甲氧基矽烷、異丙基三乙氧基矽烷、異丙基三丙氧基矽烷、異丙基三異丙氧基矽烷、丁基三甲氧基矽烷、丁基三乙氧基矽烷、丁基三丙氧基矽烷、丁基三異丙氧基矽烷、第二丁基三甲氧基矽烷、第二丁基三乙氧基矽烷、第二丁基三丙氧基矽烷、第二丁基三異丙氧基矽烷、第三丁基三甲氧基矽烷、第三丁基三乙氧基矽烷、第三丁基三丙氧基矽烷、第三丁基三異丙氧基矽烷、環丙基三甲氧基矽烷、環丙基三乙氧基矽烷、環丙基三丙氧基矽烷、環丙基三異丙氧基矽烷、環丁基三甲氧基矽烷、環丁基三乙氧基矽烷、環丁基三丙氧基矽烷、環丁基三異丙氧基矽烷、環戊基三甲氧基矽烷、環戊基三乙氧基矽烷、環戊基三丙氧基矽烷、環戊基三異丙氧基矽烷、環己基三甲氧基矽烷、環己基三乙氧基矽烷、環己基三丙氧基矽烷、環己基三異丙氧基矽烷、環己烯基三甲氧基矽烷、環己烯基三乙氧基矽烷、環己烯基三丙氧基矽烷、環己烯基三異丙氧基矽烷、環己烯基乙基三甲氧基矽烷、環己烯基乙基三乙氧基矽烷、環己烯基乙基三丙氧基矽烷、環己烯基乙基三異丙氧基矽烷、環辛基三甲氧基矽烷、環辛基三乙氧基矽烷、環辛基三丙氧基矽烷、環辛基三異丙氧基矽烷、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、環戊二烯基丙基三丙氧基矽烷、環戊二烯基丙基三異丙氧基矽烷、雙環庚烯基三甲氧基矽烷、雙環庚烯基三乙氧基矽烷、雙環庚烯基三丙氧基矽烷、雙環庚烯基三異丙氧基矽烷、雙環庚基三甲氧基矽烷、雙環庚基三乙氧基矽烷、雙環庚基三丙氧基矽烷、雙環庚基三異丙氧基矽烷、
金剛烷基三甲氧基矽烷、金剛烷基三乙氧基矽烷、金剛烷基三丙氧基矽烷、金剛烷基三異丙氧基矽烷、苯基三甲氧基矽烷、苯基三乙氧基矽烷、苯基三丙氧基矽烷、苯基三異丙氧基矽烷、苄基三甲氧基矽烷、苄基三乙氧基矽烷、苄基三丙氧基矽烷、苄基三異丙氧基矽烷、甲苯基三甲氧基矽烷、甲苯基三乙氧基矽烷、甲苯基三丙氧基矽烷、甲苯基三異丙氧基矽烷、大茴香基三甲氧基矽烷、大茴香基三乙氧基矽烷、大茴香基三丙氧基矽烷、大茴香基三異丙氧基矽烷、苯乙基三甲氧基矽烷、苯乙基三乙氧基矽烷、苯乙基三丙氧基矽烷、苯乙基三異丙氧基矽烷、萘基三甲氧基矽烷、萘基三乙氧基矽烷、萘基三丙氧基矽烷、萘基三異丙氧基矽烷等。
作為二烷氧基矽烷,可列舉: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、二甲基二丙氧基矽烷、二甲基二異丙氧基矽烷、二乙基二甲氧基矽烷、二乙基二乙氧基矽烷、二乙基二丙氧基矽烷、二乙基二異丙氧基矽烷、二丙基二甲氧基矽烷、二丙基二乙氧基矽烷、二丙基二丙氧基矽烷、二丙基二異丙氧基矽烷、二異丙基二甲氧基矽烷、二異丙基二乙氧基矽烷、二異丙基二丙氧基矽烷、二異丙基二異丙氧基矽烷、二丁基二甲氧基矽烷、二丁基二乙氧基矽烷、二丁基二丙氧基矽烷、二丁基二異丙氧基矽烷、二第二丁基二甲氧基矽烷、二第二丁基二乙氧基矽烷、二第二丁基二丙氧基矽烷、二第二丁基二異丙氧基矽烷、二第三丁基二甲氧基矽烷、二第三丁基二乙氧基矽烷、二第三丁基二丙氧基矽烷、二第三丁基二異丙氧基矽烷、二環丙基二甲氧基矽烷、二環丙基二乙氧基矽烷、二環丙基二丙氧基矽烷、二環丙基二異丙氧基矽烷、二環丁基二甲氧基矽烷、二環丁基二乙氧基矽烷、二環丁基二丙氧基矽烷、二環丁基二異丙氧基矽烷、二環戊基二甲氧基矽烷、二環戊基二乙氧基矽烷、二環戊基二丙氧基矽烷、二環戊基二異丙氧基矽
烷、二環己基二甲氧基矽烷、二環己基二乙氧基矽烷、二環己基二丙氧基矽烷、二環己基二異丙氧基矽烷、二環己烯基二甲氧基矽烷、二環己烯基二乙氧基矽烷、二環己烯基二丙氧基矽烷、二環己烯基二異丙氧基矽烷、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、二環己烯基乙基二丙氧基矽烷、二環己烯基乙基二異丙氧基矽烷、二環辛基二甲氧基矽烷、二環辛基二乙氧基矽烷、二環辛基二丙氧基矽烷、二環辛基二異丙氧基矽烷、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丙氧基矽烷、二環戊二烯基丙基二異丙氧基矽烷、雙(雙環庚烯基)二甲氧基矽烷、雙(雙環庚烯基)二乙氧基矽烷、雙(雙環庚烯基)二丙氧基矽烷、雙(雙環庚烯基)二異丙氧基矽烷、雙(雙環庚基)二甲氧基矽烷、雙(雙環庚基)二乙氧基矽烷、雙(雙環庚基)二丙氧基矽烷、雙(雙環庚基)二異丙氧基矽烷、二金剛烷基二甲氧基矽烷、二金剛烷基二乙氧基矽烷、二金剛烷基二丙氧基矽烷、二金剛烷基二異丙氧基矽烷、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、二苯基二丙氧基矽烷、二苯基二異丙氧基矽烷等。
作為單烷氧基矽烷,可列舉: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、二甲基苯基甲氧基矽烷、二甲基苯基乙氧基矽烷、二甲基苄基甲氧基矽烷、二甲基苄基乙氧基矽烷、二甲基苯乙基甲氧基矽烷、二甲基苯乙基乙氧基矽烷等。
此外,作為通式(A-1)表示之化合物,可列舉下列結構表示之在矽上含有水解性基者:就OR0A而言,為1~3個甲氧基、乙氧基、丙氧基、丁氧基、戊氧基、環戊氧基、己氧基、環己氧基、苯氧基。又,以下,結構式中之(Si)代表和Si之鍵結部位。
【化4】
本發明使用之含矽膜形成用組成物含有之聚矽氧烷,宜含有鹵化有機基較佳。如上藉由含有鹵化有機基,能更確實地將離子注入使用之遮罩予以剝離。又,鹵化有機基之鹵素宜為氟及氯較佳。
通式(A-1)中之R1A A1R2A A2R3A A3表示之有機基之中,該有機基之氫原子取代為鹵素原子者可列舉如下。
R1A、R2A、R3A表示之有機基之其他例,可列舉有1個以上的碳-氧單鍵或碳-氧雙鍵的有機基。具體而言,為具有選自於由環氧基、酯基、烷氧基、羥基構成之群組中之1種以上之基的有機基。其例可列舉下列通式(A-2)表示者。
(P-Q1-(Sa)v1-Q2-)u-(T)v2-Q3-(Sb)v3-Q4- (A-2)
(通式(A-2)中,P為氫原子,
羥基、碳數1~4之烷氧基、碳數1~6之烷基羰基氧基、或碳數1~6之烷基羰基,Q1、Q2、Q3、及Q4各自獨立地為-CqH(2q-p)Pp-(式中,P同上述,p為0~3之整數,q為0~10之整數(惟q=0代表單鍵。)。),u為0~3之整數,Sa與Sb各自獨立地表示-O-、-CO-、-OCO-、-COO-、或-OCOO-。v1、v2、及v3各自獨立地表示0或1。和此等為同時,T代表由也可含雜原子之脂環或芳香環構成之2價基,T之也可含氧原子等雜原子之脂環或芳香環之例如以下所示。於T,Q2與Q3鍵結之位置不特別限定,可考量立體要因所致之反應性、反應使用之市售試藥之取得性等而適當選擇。)
通式(A-2)表示之具有1個以上之碳-氧單鍵或碳-氧雙鍵之有機基之理想例可列舉如下。
又,本發明使用之含矽膜形成用組成物含有之聚矽氧烷宜含有交聯性有機基。亦即,上述有機基之中,含有交聯性有機基者尤佳。如上,藉由含有交聯性有機基,能形成密合性更良好的含矽膜。又,交聯性有機基,例如環氧基、苯酚基、及萘酚基等為較佳。
又,通式(A-1)中之R1A、R2A、R3A表示之有機基也可以為含有矽-矽鍵之有機基。具體而言可列舉下列結構。
本發明使用之含矽膜形成用組成物含有之聚矽氧烷,除了上述通式(A-1)表示之化合物以外,也可以含有下列通式(A-3)表示之水解性金屬化合物作為原料。
L’(OR4A)A4(OR5A)A5(O)A6 (A-3)
(式中,R4A及R5A為氫原子或碳數1~30之有機基,A4+A5+A6為依L’之種類決定之價數,A4、A5、A6為0以上之數,L’為周期表之III族、IV族、或V族之元素且排除碳。)
通式(A-3)表示之水解性金屬化合物可列舉如下。
L’為硼時,作為通式(A-3)表示之化合物可列舉: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、硼酸、氧化硼等。
L’為鋁時,作為通式(A-3)表示之化合物可列舉: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鋁、二丁氧基乙基乙醯乙酸鋁、丙氧基雙乙基乙醯乙酸鋁、丁氧基雙乙基乙醯乙酸鋁、2,4-戊烷二酮酸鋁、2,2,6,6-四甲基-3,5-庚烷二酮酸鋁等。
L’為鎵時,作為通式(A-3)表示之化合物可列舉: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鎵、二丁氧基乙基乙醯乙酸鎵、丙氧基雙乙基乙醯乙酸鎵、丁氧基雙乙基乙醯乙酸鎵、2,4-戊烷二酮酸鎵、2,2,6,6-四甲基-3,5-庚烷二酮酸鎵等。
L’為釔時,作為通式(A-3)表示之化合物可列舉: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釔、二丁氧基乙基乙醯乙酸釔、丙氧基雙乙基乙醯乙酸釔、丁氧基雙乙基乙醯乙酸釔、2,4-戊烷二酮酸釔、2,2,6,6-四甲基-3,5-庚烷二酮酸釔等。
L’為鍺時,作為通式(A-3)表示之化合物可列舉: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。
L’為鈦時,作為通式(A-3)表示之化合物可列舉: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鈦、二丁氧基雙乙基乙醯乙酸鈦、二丙氧基雙2,4-戊烷二酮酸鈦、二丁氧基雙2,4-戊烷二酮酸鈦等。
L’為鉿時,作為通式(A-3)表示之化合物可以列舉: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鉿、二丁氧基雙乙基乙醯乙酸鉿、二丙氧基雙2,4-戊烷二酮酸鉿、二丁氧基雙2,4-戊烷二酮酸鉿等。
L’為錫時,通式(A-3)表示之化合物可列舉: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-戊烷二酮酸錫、2,2,6,6-四甲基-3,5-庚烷二酮酸錫。
L’為砷時,作為通式(A-3)表示之化合物可列舉:甲氧基砷、乙氧基砷、丙氧基砷、丁氧基砷、苯氧基砷等。
L’為銻時,作為通式(A-3)表示之化合物可列舉: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。
L’為鈮時,作為通式(A-3)表示之化合物可列舉:甲氧基鈮、乙氧基鈮、丙氧基鈮、丁氧基鈮、苯氧基鈮等。
L’為鉭時,作為通式(A-3)表示之化合物可列舉:甲氧基鉭、乙氧基鉭、丙氧基鉭、丁氧基鉭、苯氧基鉭等。
L’為鉍時,作為通式(A-3)表示之化合物可列舉:甲氧基鉍、乙氧基鉍、丙氧基鉍、丁氧基鉍、苯氧基鉍等。
L’為磷時,作為通式(A-3)表示之化合物可列舉:亞磷酸三甲酯、亞磷酸三乙酯、亞磷酸三丙酯、磷酸三甲酯、磷酸三乙酯、磷酸三丙酯、五氧化二磷等。
L’為釩時,作為通式(A-3)表示之化合物可列舉:雙(2,4-戊烷二酮酸)氧化釩、2,4-戊烷二酮酸釩、三丁氧基氧化釩、三丙氧基氧化釩等。
L’為鋯時,作為通式(A-3)表示之化合物可列舉: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-戊烷二酮酸)鋯、二丙氧基雙(2,2,6,6-四甲基-3,5-庚烷二酮酸)鋯等。
可選擇該等化合物中的1種以上,於反應前或反應中混合成用以形成聚矽氧烷之反應原料(單體)。
本發明使用之含矽膜形成用組成物含有之聚矽氧烷,例如可將上述通式(A-1)表示之化合物與視需要之上述通式(A-3)表示之化合物,使用選自無機酸、脂肪族磺酸、及芳香族磺酸中之1種以上之化合物作為酸觸媒,進行水解縮合以製造。
此時可使用之酸觸媒可列舉:氟酸、鹽酸、氫溴酸、硫酸、硝酸、過氯酸、磷酸、甲烷磺酸、苯磺酸、甲苯磺酸等。觸媒之使用量相對於單體1莫耳為10-6~10莫耳較理想,更佳為10-5~5莫耳,又更佳為10-4~1莫耳。
從該等單體利用水解縮合獲得聚矽氧烷時之水之量,宜為鍵結於單體之水解性取代基每1莫耳為0.01~100莫耳,更佳為0.05~50莫耳,又更佳為0.1~30莫耳。添加量若為100莫耳以下,反應使用的裝置不會變得過大,為經濟的。
操作方法係於觸媒水溶液添加單體使水解縮合反應開始。此時,可以於觸媒水溶液中添加有機溶劑,也可以將單體以有機溶劑稀釋,也可進行兩者。反應溫度宜為0~100℃,更佳為5~80℃。宜為單體之滴加時保持溫度為5~80℃,之後使其於20~80℃熟成之方法較佳。
可添加於觸媒水溶液、或能將單體稀釋之有機溶劑,宜為甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-1-丙醇、乙二醇、丙二醇、丙酮、乙腈、四氫呋喃、甲苯、己烷、乙酸乙酯、環己酮、甲基戊酮、丁二醇單甲醚、丙二醇單甲醚、乙二醇單甲醚、丁二醇單乙醚、丙二醇單乙醚、乙二醇單乙醚、丁二醇單丙醚、丙二醇單丙醚、乙二醇單丙醚、丙二醇二甲醚、二乙二醇二甲醚、丙二醇單甲醚乙酸酯、丙二醇單乙醚乙酸酯、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、乙酸第三丁酯、丙酸第三丁酯、丙二醇單第三丁醚乙酸酯、γ-丁內酯及該等之混合物等為較佳。
該等溶劑之中較理想者為水溶性者。例如:甲醇、乙醇、1-丙醇、2-丙醇等醇類;乙二醇、丙二醇等多元醇;丁二醇單甲醚、丙二醇單甲醚、乙二醇單甲醚、丁二醇單乙醚、丙二醇單乙醚、乙二醇單乙醚、丁二醇單丙醚、丙二醇單丙醚、乙二醇單丙醚等多元醇縮合物衍生物;丙酮、乙腈、四氫呋喃等。其中特別理想者為沸點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,尤其0~500mL為較佳。若為如此的使用量,反應容器不會變得太大,為經濟的。
之後視須要進行觸媒之中和反應,將於水解縮合反應生成的醇減壓除去,獲得反應混合物水溶液。此時,中和可使用之鹼性物質之量,宜相對於觸媒使用之酸為0.1~2當量為較佳。此鹼性物質只要是在水中呈鹼性者即可,可以為任意物質。
然後,宜從反應混合物將水解縮合反應生成的醇等副生物去除較佳。此時,將反應混合物加熱的溫度取決於添加之有機溶劑及於反應產生之醇等的種類,較佳為0~100℃,更佳為10~90℃,又更佳為15~80℃。又,此時之減壓度取決於待除去之有機溶劑及醇等的種類、排氣裝置、冷凝裝置、及加熱溫度而異,較佳為大氣壓以下,更佳為絕對壓力80kPa以下,又更佳為絕對壓力50kPa以下。此時難正確知曉除去之醇量,但希望能去除生成之醇等的約80質量%以上。
然後,也可從反應混合物去除水解縮合使用的酸觸媒。去除酸觸媒之方法係將水與聚矽氧烷混合並將聚矽氧烷以有機溶劑萃取。此時使用的有機溶劑宜為能溶解聚矽氧烷,且若和水混合則分層為2層者較佳。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、甲基戊酮、丁二醇單甲醚、丙二醇單甲醚、乙二醇單甲醚、丁二醇單乙醚、丙二醇單乙醚、乙二醇單乙醚、丁二醇單丙醚、丙二醇單丙醚、乙二醇單丙醚、丙二醇二甲醚、二乙二醇二甲醚、丙二醇單甲醚乙酸酯、丙二醇單乙醚乙酸酯、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、乙酸第三丁酯、丙酸第三丁酯、丙二醇單第三丁醚乙酸酯、γ-丁內酯、甲基異丁酮、環戊基甲醚等、及該等之混合物。
又,也可以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、丁二醇單甲醚+乙酸乙酯、丙二醇單甲醚+乙酸乙酯、乙二醇單甲醚+乙酸乙酯、丁二醇單乙醚+乙酸乙酯、丙二醇單乙醚+乙酸乙酯、乙二醇單乙醚+乙酸乙酯、丁二醇單丙醚+乙酸乙酯、丙二醇單丙醚+乙酸乙酯、乙二醇單丙醚+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、丙二醇單甲醚+甲基異丁酮、乙二醇單甲醚+甲基異丁酮、丙二醇單乙醚+甲基異丁酮、乙二醇單乙醚+甲基異丁酮、丙二醇單丙醚+甲基異丁酮、乙二醇單丙醚+甲基異丁酮、甲醇+環戊基甲醚、乙醇+環戊基甲醚、1-丙醇+環戊基甲醚、2-丙醇+環戊基甲醚、丙二醇單甲醚+環戊基甲醚、乙二醇單甲醚+環戊基甲醚、丙二醇單乙醚+環戊基甲醚、乙二醇單乙醚+環戊基甲醚、丙二醇單丙醚+環戊基甲醚、乙二醇單丙醚+環戊基甲醚、甲醇+丙二醇甲醚乙酸酯、乙醇+丙二醇甲醚乙酸酯、1-丙醇+丙二醇甲醚乙酸酯、2-丙醇+丙二醇甲醚乙酸酯、丙二醇單甲醚+丙二醇甲醚乙酸酯、乙二醇單甲醚+丙二醇甲醚乙酸酯、丙二醇單乙醚+丙二醇甲醚乙酸酯、乙二醇單乙醚+丙二醇甲醚乙酸酯、丙二醇單丙醚+丙二醇甲醚乙酸酯、乙二醇單丙醚+丙二醇甲醚乙酸酯等之組合為較佳,但組合不限於此等。
又,水溶性有機溶劑與水難溶性有機溶劑之混合比例可適當選擇,但相對於水難溶性有機溶劑100質量份,水溶性有機溶劑宜為0.1~1,000質量份,更佳為1~500質量份,又更佳為2~100質量份。
然後也可以用中性水洗滌。此水可使用通常稱為去離子水、超純水者。此水之量相對於聚矽氧烷溶液1L宜為0.01~100L,更佳為0.05~50L,又更佳為0.1~5L。此洗滌方法可為將兩者放入同一容器並混合後,靜置並將水層。洗滌次數只要是1次以上即可,因為即使洗滌10次以上仍無法獲得相應於洗滌次數的效果,較佳為1~5次左右。
此外,去除酸觸媒之方法,可列舉利用離子交換樹脂之方法、以環氧乙烷、環氧丙烷等環氧化合物中和後除去之方法。該等方法可以配合反應使用的酸觸媒適當選擇。
由於此時之水洗操作,聚矽氧烷一部分會進入水層,有時獲得實質上與區分操作為同等的效果,所以水洗次數或洗滌水之量,評估觸媒去除效果及區分效果適當選擇即可。
又尚有酸觸媒殘留之聚矽氧烷溶液、及已去除酸觸媒之聚矽氧烷溶液,均可添加最後的溶劑並於減壓進行溶劑交換而獲得聚矽氧烷溶液。此時之溶劑交換之溫度,取決於待除去之反應溶劑或萃取溶劑之種類而不同,較佳為0~100℃,更佳為10~90℃,又更佳為15~80℃。又,此時之減壓度因應於待除去之萃取溶劑之種類、排氣裝置、冷凝裝置及加熱溫度而異,較佳為於大氣壓力以下,更佳為於絕對壓力80kPa以下,又更佳為絕對壓力50kPa以下。
此時,由於改變溶劑有時會使得聚矽氧烷變得不安定。此現象係由於最終的溶劑與聚矽氧烷的相容性而發生,為防止此現象,也可加入後述成分作為安定劑。加入量,相對於溶劑交換前之溶液中之聚矽氧烷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,但添加時以0.5質量份以上為較佳。視需要,也可對於溶劑交換前之溶液加入安定劑並進行溶劑交換操作。
又,聚矽氧烷溶液的濃度為0.1~20質量%較佳。若為如此的濃度,聚矽氧烷不會進行縮合反應而變成不能再溶於有機溶劑的狀態。又,藉由為如此的濃度,溶劑之量為適量,故有經濟性。
加入聚矽氧烷溶液的最終溶劑宜為醇系溶劑,特別理想者為:乙二醇、二乙二醇、三乙二醇、丙二醇、二丙二醇、丁二醇等單烷醚衍生物。具體而言,丁二醇單甲醚、丙二醇單甲醚、乙二醇單甲醚、丁二醇單乙醚、丙二醇單乙醚、乙二醇單乙醚、丁二醇單丙醚、丙二醇單丙醚、乙二醇單丙醚等。
該等溶劑只要是主成分即可,也可以加入非醇系溶劑作為輔助溶劑。此輔助溶劑可列舉:丙酮、四氫呋喃、甲苯、己烷、乙酸乙酯、環己酮、甲基戊酮、丙二醇二甲醚、二乙二醇二甲醚、丙二醇單甲醚乙酸酯、丙二醇單乙醚乙酸酯、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、乙酸第三丁酯、丙酸第三丁酯、丙二醇單第三丁醚乙酸酯、γ-丁內酯、甲基異丁酮、環戊基甲醚等。
又,就其他反應操作而言,係於單體或單體之有機溶液添加水或含水有機溶劑並使水解反應開始。此時,觸媒可添加到單體或單體之有機溶液,也可以添加到水或含水有機溶劑。反應溫度為0~100℃,較佳為10~80℃。水滴加時,宜加熱到10~50℃,之後使其升溫到20~80℃並使其熟成之方法為較佳。
使用有機溶劑時宜為水溶性者,可以列舉:甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-1-丙醇等醇類;丁二醇單甲醚、丙二醇單甲醚、乙二醇單甲醚、丁二醇單乙醚、丙二醇單乙醚、乙二醇單乙醚、丁二醇單丙醚、丙二醇單丙醚、乙二醇單丙醚、丙二醇二甲醚、二乙二醇二甲醚、丙二醇單甲醚乙酸酯、丙二醇單乙醚乙酸酯、丙二醇單丙醚等多元醇縮合物衍生物;丙酮、四氫呋喃、乙腈等、及該等之混合物等。
有機溶劑之使用量可和上述為同量。對於獲得之反應混合物以和上述同樣的方法進行後處理,可獲得聚矽氧烷。
又,本發明使用之含矽膜形成用組成物含有之聚矽氧烷,亦可將例如上述通式(A-1)表示之化合物、及視需要之上述通式(A-3)表示之化合物於鹼觸媒存在下進行水解縮合以製造。
此時可使用之鹼觸媒可列舉:甲胺、乙胺、丙胺、丁胺、乙二胺、六亞甲基二胺、二甲胺、二乙胺、乙基甲胺、三甲胺、三乙胺、三丙胺、三丁胺、環己胺、二環己胺、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、二氮雜雙環辛烷、二氮雜雙環環壬烯、二氮雜雙環十一烯、六亞甲基四胺、苯胺、N,N-二甲基苯胺、吡啶、N,N-二甲胺基吡啶、吡咯、哌、吡
咯啶、哌啶、甲基吡啶、四甲基氫氧化銨、氫氧化膽鹼、四丙基氫氧化銨、四丁基氫氧化銨、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單體1莫耳,通常為10-6莫耳~10莫耳,較佳為10-5莫耳~5莫耳,更佳為10-4莫耳~1莫耳。
從該等單體利用水解縮合獲得聚矽氧烷時之水之量,宜就鍵結於單體之水解性取代基每1莫耳添加0.1~50莫耳較佳。添加量為50莫耳以下的話,反應使用的裝置不會變得過大,有經濟性。
操作方法係於觸媒水溶液添加單體使水解縮合反應開始。此時可於觸媒水溶液中添加有機溶劑,也可將單體以有機溶劑稀釋,也可實施兩者。反應溫度宜為0~100℃,更佳為5~80℃。單體滴加時保持溫度為5~80℃,於之後20~80℃熟成之方法為較佳。
能加到鹼觸媒水溶液、或能稀釋單體之有機溶劑,可使用與能添加在酸觸媒水溶液時例示之有機溶劑為同樣者。有機溶劑之使用量,宜相對於單體1莫耳為0~1,000ml,尤其0~500mL較佳。若為如此的使用量,反應使用的裝置不會變得過大,有經濟性。
之後視須要實施觸媒之中和反應,將於水解縮合反應生成之醇減壓除去,獲得反應混合物水溶液。此時中和能使用之酸性物質之量,相對於觸媒使用之鹼性物質宜為0.1~2當量為較佳。此酸性物質只要是在水中呈酸性者即可,可為任意物質。
然後,宜從反應混合物將在水解縮合反應生成之醇等副生物利用減壓除去等予以去除較佳。此時將反應混合物加熱之溫度及減壓度可以和使用酸觸媒時相同。
之後,可以從反應混合物將水解縮合使用的鹼觸媒去除。就去除鹼觸媒之方法,係將水和聚矽氧烷混合並將聚矽氧烷以有機溶劑萃取。此時使用之有機溶劑,可以使用與除去酸觸媒時使用者所具體例示之上述有機溶劑為同樣者。
又,也可以使用水溶性有機溶劑與水難性有機溶劑之混合物。此時使用之水溶性有機溶劑與水難性有機溶劑之混合物可使用與除去酸觸媒時使用者所具體例示之上述混合物為同樣者。
水溶性有機溶劑與水難溶性有機溶劑之混合比例可和除去酸觸媒時使用的混合比例相同。
然後也可以用中性水洗滌。此水可使用通常稱為去離子水、超純水者。此時之水之量、洗滌方法、洗滌次數,設為和使用酸觸媒時相同即可。
由於此時之水洗操作,聚矽氧烷一部分會進入水層,有時獲得實質上與區分操作為同等的效果,所以水洗次數或洗滌水之量,評估觸媒去除效果及區分效果適當選擇即可。
又尚有鹼觸媒殘留之聚矽氧烷溶液、及已去除鹼觸媒之聚矽氧烷溶液,均可添加最後的溶劑並於減壓進行溶劑交換而獲得聚矽氧烷溶液。此時之溶劑交換之溫度、減壓度、及最終的聚矽氧烷溶液之濃度,可設為和使用酸觸媒時相同。
又,加到聚矽氧烷溶液之最終溶劑也可使用和使用酸觸媒時相同者。
又,和使用酸觸媒時同樣,也可以添加安定劑。
又,就其他反應操作而言,於單體或單體之有機溶液中添加水或含水有機溶劑,使水解反應開始。此時,觸媒可添加到單體或單體之有機溶液,也可添加到水或含水有機溶劑。反應溫度為0~100℃,較佳為10~80℃。宜為水滴加時加熱到10~50℃,之後使其升溫到20~80℃並使其熟成之方法較佳。
又,使用有機溶劑時,可使用和使用酸觸媒時為同樣者。
獲得之聚矽氧烷之分子量不只可藉由單體之選擇,也可藉由控制聚合時之反應條件以調整,宜使用重量平均分子量為100,000以下,更佳為200~50,000,又更佳為300~30,000者。重量平均分子量若為100,000以下,無發生異物、塗佈斑之虞。
又,關於上述重量平均分子量之數據,係以RI作為檢測器,以四氫呋喃作為溶離溶劑,利用凝膠滲透層析(GPC),使用聚苯乙烯作為標準物質,以聚苯乙烯換算來表示分子量。
(其他添加成分)
本發明之含矽膜形成用組成物中,為了改善安定性,宜添加碳數1~30之1元或2元以上之有機酸較佳。作為如此的有機酸可列舉甲酸、乙酸、丙酸、丁酸、戊酸、己酸、庚酸、辛酸、壬酸、癸酸、油酸、硬脂酸、亞麻油酸、次亞麻油酸、苯甲酸、鄰苯二甲酸、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、琥珀酸、甲基琥珀
酸、戊二酸、己二酸、衣康酸、馬來酸、富馬酸、檸康酸、檸檬酸等。尤其草酸、馬來酸、甲酸、乙酸、丙酸、檸檬酸等較佳。又,為了確保安定性,也可混用2種以上的酸。添加量相對於組成物所含之聚矽氧烷100質量份宜為0.001~25質量份,更佳為0.01~15質量份,又更佳為0.1~5質量份。
或,宜摻合上述有機酸,使換算為組成物之pH成為較佳為0≦pH≦7,更佳為0.3≦pH≦6.5,又更佳為0.5≦pH≦6。
又,本發明之含矽膜形成用組成物中也可以添加水。若添加水,聚矽氧烷會水合,故微影性能提高。組成物之溶劑成分中,水之含有率較佳為超過0質量%且未達50質量%,更佳為0.3~30質量%,又更佳為0.5~20質量%。
含水之全部溶劑之使用量,宜相對於基礎聚合物(聚矽氧烷)100質量份為100~100,000質量份,更佳為200~50,000質量份。藉由為如此的添加量,能使微影性能提高,且塗佈膜之均勻性不易惡化,所以能抑制眼孔(eye hole)發生。
又,本發明之含矽膜形成用組成物中也可添加因熱、光或此兩者之作用而產生酸之酸產生劑。如此的酸產生劑,具體而言可列舉如日本特開2007-199653號公報之(0061)段落至(0084)段落記載之酸產生劑。
本發明使用之含矽膜形成用組成物中也可添加含氟之有機化合物。具體而言可列舉如以下的化合物。
含氟之有機物只要是可溶於含矽膜形成用組成物使用之溶劑者即可,並無特殊限定,例如含有下列通式(F1)~(F4)表示之重複單元中之1種以上較佳。
【化13】
式中,RF1、RF7、RF9、RF14各自獨立地為氫原子、甲基、氟原子、或三氟甲基。
RF2~RF6各自獨立地表示氫原子、氟原子、三氟甲基、-C(CF3)2ORF16、或1個以上之氫原子亦可取代為氟原子之碳數1~5之烷基或烷氧基,且RF2~RF6中之1者以上為氟原子或含氟之基。RF2~RF6為1個以上之氫也可取代為氟原子之碳數1~5之烷氧基時,具體例可列舉甲氧基、乙氧基、正丙基氧基、異丙基氧基、環戊基氧基正丁氧基、第二丁氧基、第三丁氧基、環丁氧基、正戊基氧基、環戊基氧基,此等基之一部分或全部氫原子也可取代為氟原子。
RF16、RF8、RF13各自獨立地表示氫原子、或碳數1~22之直鏈狀、分支狀或環狀之1價有機基。1價有機基可使用各種羥基之保護基,例如:甲基、乙基、丙基、異丙基、正丁基、第二丁基、第三丁基、第三戊基、正戊基、正己基、正庚基、正辛基、正壬基、正癸基、二十基、環丙基、環丁基、環戊基、環戊基甲基、環戊基乙基、環戊基丁基、環己基、環己基甲基、環己基乙基、環己基丁基、甲基環己基甲基、乙基環己基甲基、乙基環己基乙基、雙環[2.2.1]庚基
等1價烴基。又,此等1價烴基之氫原子之一部分也可取代為鹵素原子,構成之-CH2-也可取代為-O-或-C(=O)-。
又,作為RF16、RF8、RF13,可列舉下列通式(R1-1)、(R1-2)表示之基、碳數4~20,尤其碳數4~15之三級烷基、各烷基各為碳數1~5之三烷基矽基、碳數4~20,尤其碳數4~15之側氧基烷基、碳數1~10之醯基等。
在此,破折線代表鍵結手(以下同)。RL01、RL02表示氫原子、或碳數1~18,較佳為碳數1~10之直鏈狀、分支狀或環狀之烷基,具體而言可列舉:甲基、乙基、丙基、異丙基、正丁基、第二丁基、第三丁基、環戊基、環己基、2-乙基己基、正辛基、降莰基、三環癸基、四環十二基、金剛烷基等。RL03表示碳數1~18,較佳為碳數1~10之也可以有氧原子等雜原子之一價烴基,可列舉直鏈狀、分支狀或環狀之烷基、該等氫原子之一部分取代成羥基、烷氧基、側氧基、胺基、烷胺基等者,具體而言可列舉下列取代烷基等。
【化15】
RL01與RL02、RL01與RL03、RL02與RL03也可彼此鍵結並與此等所鍵結之碳原子、氧原子一起形成環,形成環時,RL01、RL02、RL03各代表碳數1~18,較佳為碳數1~10之直鏈狀或分支狀之伸烷基。
RL04表示碳數4~20,較佳為碳數4~15之三級烷基,各烷基各為碳數1~6之三烷基矽基、碳數4~20之側氧基烷基、或上述通式(R1-1)表示之基,就三級烷基而言,具體可列舉第三丁基、第三戊基、1,1-二乙基丙基、2-環戊基丙-2-基、2-環己基丙-2-基、2-(雙環[2.2.1]庚-2-基)丙-2-基、2-(金剛烷-1-基)丙-2-基、1-乙基環戊基、1-丁基環戊基、1-乙基環己基、1-丁基環己基、1-乙基-2-環戊烯基、1-乙基-2-環己烯基、2-甲基-2-金剛烷基、2-乙基-2-金剛烷基等,作為三烷基矽基,具體可列舉三甲基矽基、三乙基矽基、二甲基-第三丁基矽基等,作為側氧基烷基,具體可列舉3-側氧基環己基、4-甲基-2-側氧基烷-4-基、5-甲基-2-側氧基四氫呋喃-5-基等,作為醯基,具體可列舉甲醯基、乙醯基、乙基羰基、三甲基乙醯基、甲氧基羰基、乙氧基羰基、第三丁氧基羰基、三氟乙醯基、三氯乙醯基等。y為0~6之整數。
上式(R1-1)表示之保護基之中,直鏈狀或分支狀者可具體列舉下列之基。
【化16】
上式(R1-1)表示之保護基中,環狀者具體可列舉:四氫呋喃-2-基、2-甲基四氫呋喃-2-基、四氫哌喃-2-基、2-甲基四氫哌喃-2-基等。
作為上式(R1-2)表示之保護基,具體可列舉:第三丁氧基羰基、第三丁氧基羰基甲基、第三戊氧基羰基、第三戊氧基羰基甲基、1,1-二乙基丙氧基羰基、1,1-二乙基丙氧基羰基甲基、1-乙基環戊氧基羰基、1-乙基環戊氧基羰基甲基、1-乙基-2-環戊烯氧基羰基、1-乙基-2-環戊烯氧基羰基甲基、1-乙氧基乙氧基羰基甲基、2-四氫哌喃氧羰基甲基、2-四氫呋喃氧基羰基甲基等。
LF1代表單鍵或-C(=O)O-。mf代表0或1。
LF2表示碳數1~15之直鏈狀、分支狀或環狀之2價或3價之烴基。LF2,例如:從甲烷、乙烷、丙烷、正丁烷、正戊烷、正己烷、正庚烷、正辛烷、正壬烷、正癸烷、2-甲基丙烷、2-甲基丁烷、2,2-二甲基丙烷、2-甲基戊烷、2-甲基己烷、2-甲基庚烷、環戊烷、環己烷、甲基環戊烷、甲基環己烷、乙基環戊烷、甲基環庚烷、乙基環己烷、1-甲基金剛烷、2-甲基金剛烷、1-乙基金剛烷、2-乙基金剛烷等烴取走2個或3個氫原子而得者。
nf表示1或2。
RF10~RF12各自獨立地表示氫原子、羥基、鹵素原子、或碳數1~16之直鏈狀、分支狀或環狀之1價有機基。RF10~RF12為任意組且可至少其中兩者彼此鍵結並與此等所鍵結之碳原子一起形成環。
碳數1~16之直鏈狀、分支狀或環狀之1價有機基,例如:甲基、乙基、丙基、異丙基、正丁基、第二丁基、第三丁基、第三戊基、正戊基、正己基、正庚基、正辛基、正壬基、正癸基、環丙基、環丁基、環戊基、環戊基甲基、環戊基乙基、環戊基丁基、環己基、環己基甲基、環己基乙基、環己基丁基、甲基環己基甲基、乙基環己基甲基、乙基環己基乙基、雙環[2.2.1]庚基、雙環[2.2.1]庚基甲基、雙環[2.2.1]庚基乙基、雙環[2.2.1]庚基丁基、甲基雙環[2.2.1]庚基甲基、乙基雙環[2.2.1]庚基甲基、乙基雙環[2.2.1]庚基乙基、雙環[2.2.2]辛基、雙環[2.2.2]辛基甲基、雙環[2.2.2]辛基乙基、雙環[2.2.2]辛基丁基、甲基雙環[2.2.2]辛基甲基、乙基雙環[2.2.2]辛基甲基、乙基雙環[2.2.2]辛基乙基、三環[5.2.1.02,6]癸基、三環[5.2.1.02,6]癸基甲基、三環[5.2.1.02,6]癸基乙基、三環[5.2.1.02,6]癸基丁基、甲基三環[5.2.1.02,6]癸基甲基、乙基三環[5.2.1.02,6]癸基甲基、乙基三環[5.2.1.02,6]癸基乙基、金剛烷基、金剛烷基甲基、金剛烷基乙基、金剛烷基丁基、甲基金剛烷基甲基、乙基金剛烷基甲基、乙基金剛烷基乙基、四環[4.4.0.12,5.17,10]十二基、四環[4.4.0.12,5.17,10]十二基甲基、四環[4.4.0.12,5.17,10]十二基乙基、四環[4.4.0.12,5.17,10]十二基丁基、四環[4.4.0.125.1710十二基甲基乙基、四環[4.4.0.12,5.17,10]十二基甲基、乙基四環[4.4.0.12,5.17,10]十二基乙基等直鏈狀、分支狀或環狀之烷基、苯基、甲基苯基、萘基、蒽基、菲基等芳基、苄基、二苯基甲基、苯乙基等芳烷基等一價之烴基、甲氧基、乙氧基、丙氧基等烷氧基、
甲醯基氧基、乙醯氧基等醯氧基,該等基中之氫原子之一部分也可以取代為鹵素原子、烷基、芳基、烷氧基、烷氧基羰基、側氧基、烷氧基烷基、醯氧基、醯氧基烷基、烷氧基烷氧基等。
RF10~RF12為任意組合且也可至少其中2個彼此鍵結並與此等所鍵結之碳原子一起形成環。形成環之組合之典型例可列舉:RF10與RF11、RF10與RF12、RF11與RF12。於此情形,形成之環可列舉環丙烷、環丁烷、環戊烷、環己烷、雙環[2.2.1]庚烷、雙環[2.2.2]辛烷、三環[5.2.1.02,6]癸烷、金剛烷、四環[4.4.0.12,5.17,10]十二烷等碳數3~12之脂環族烴,也可為包括此等的烴的縮合環。又,該等脂環族烴之氫原子之一部分也可以取代成羥基、鹵素原子、烷基、芳基、烷氧基、烷氧基羰基、側氧基、烷氧基烷基、醯氧基、醯氧基烷基、烷氧基烷氧基等。
of表示0或1。
RF15表示有1個以上之氫取代成氟原子的碳數2~15的烴基。RF15,例如:乙基、丙基、異丙基、正丁基、第二丁基、第三丁基、第三戊基、正戊基、正己基、正庚基、正辛基、正壬基、正癸基、環丙基、環丁基、環戊基、環戊基甲基、環戊基乙基、環戊基丁基、環己基、環己基甲基、環己基乙基、環己基丁基、甲基環己基甲基、乙基環己基甲基、乙基環己基乙基、雙環[2.2.1]庚基、金剛烷基中之氫原子之一部分或全部取代成氟原子而得的基。
上述通式(F1)表示之重複單元之具體例列舉如下但不限於此等。
【化17】
【化18】
【化19】
(式中,RF1同上述。)
上述通式(F2)表示之重複單元之具體例列舉如下但不限於此等。
【化20】
(式中,RF7同上述。)
上述通式(F3)表示之重複單元之具體例列舉如下但不限於此等。
(式中,RF9同上述。)
上述通式(F4)表示之重複單元之具體例列舉如下但不限於此等。
(式中,RF14同上述。)
又,為了使上述含氟之有機化合物向溶劑之溶解性及剝離性改善,也可導入1種以上之基於上述以外之含碳-碳雙鍵之單體的重複單元。該等單元可列舉具有以下所示之羥基、烷氧基、羧基、酯基、及醚結構中任一者以上之重複單元,但不限於此等。
【化23】
【化24】
(式中,R01表示氫原子、甲基、氟原子、羥甲基、或三氟甲基。)
又,本發明使用之含矽膜形成用組成物中,視需要可添加交聯劑。如此之交聯劑,具體可列舉日本特開2007-199653號公報之(0056)段落至(0059)段落記載之交聯劑。
又,本發明使用之含矽膜形成用組成物中,視需要可更添加含有交聯性有機基之聚矽氧烷。如此之聚矽氧烷,具體而言可列舉通式(A-1)、(A-2)表示之化合物之中帶有環氧基之單體、帶有苯酚性羥基之單體、鍵結了三級烷基之帶有苯酚性羥基之單體予以水解縮合而得之聚矽氧烷。
又,本發明使用之含矽膜形成用組成物中,視需要可添加界面活性劑。如此之界面活性劑,具體而言可列舉在日本特開2009-126940號公報之(0185)段落記載之界面活性劑。
又,本發明使用之含矽膜形成用組成物中,視需要可添加熱交聯促進劑。如此之熱交聯促進劑,具體而言可列舉日本特開2007-302873號公報記載之熱交聯促進劑。
又,上述熱交聯促進劑可單獨使用1種或組合使用2種以上。熱交聯促進劑之添加量相對於基礎聚合物(上述聚矽氧烷)100質量份宜為0.01~50質量份,更佳為0.1~40質量份。
又,本發明使用之含矽膜形成用組成物中,視需要也可添加熱交聯用酸產生劑。如此之熱交聯用酸產生劑,具體而言可列舉日本特開2007-226204號公報記載之熱交聯用酸產生劑。
又,上述熱交聯用酸產生劑可單獨使用1種或組合使用2種以上。熱交聯用酸產生劑之添加量相對於基礎聚合物(上述聚矽氧烷)100質量份較佳為0.001~20質量份,更佳為0.01~10質量份。
在此,含矽膜中之矽含量定義如下。
通式(A-1)表示之水解性矽化合物作為單體時,添加足夠水而使其完全水解縮合時,獲得之聚矽氧烷之反應如下。
R1A A1R2A A2R3A A3Si(OR0A)(4-A1-A2-A3)+((4-A1-A2-A3)/2)H2O→R1A A1R2A A2R3A A3SiO((4-A1-A2-A3)/2)
在此,R1A A1R2A A2R3A A3部分之式量若令為Rw,則水解縮合獲得之聚矽氧烷之式量Rs以下式表示。
Rs=Rw+28.1+16.0×((4-A1-A2-A3)/2)
因此聚矽氧烷中之矽含量S1(質量%)以下式表示。
S1=(28.1/Rs)×100
將2種以上之單體混合而獲得聚矽氧烷時,若令單體1之Rs為Rs1、莫耳比為Rm1、單體2之Rs為Rs2、莫耳比為Rm2、單體n之Rs為Rsn、莫耳比為Rmn,聚矽氧烷中之矽含量S1(質量%)以下式表示。
又,若相相對於上述聚矽氧烷100g,在組成物添加之含氟之有機化合物與交聯劑之質量各令為RFw、RXw,則含矽膜中之矽含有率S(質量%)以下式表示。
S=S1/(100+RFw+RXw)
如上述,本發明中,含矽膜中之矽含量需為1質量%以上30質量%以下,更佳為5質量%以上25質量%以下。若矽含量超過30質量%,在利用剝離液所為之濕式剝離步驟,在基板上會殘留剝離不完全時之殘渣。另一方面,矽含量若少於1質量%,和光阻膜、有機下層膜之乾蝕刻選擇性惡化,於3層光阻處理難形成圖案。
本發明之含矽膜,能使用上述含矽膜形成用組成物,和光阻膜同樣以旋塗法等在有機下層膜上成膜。旋塗後,藉由使溶劑蒸發而防止和光阻膜混合,並未了促進交聯反應,會進行烘烤。烘烤溫度為50~500℃之範圍內較理想,烘烤
時間為10~300秒之範圍內為較佳。特別理想的溫度範圍取決於製造之裝置之結構,但為了減少對於裝置之熱損害,400℃以下為較佳。
又,含矽膜之膜厚不特別限定,約20nm至100nm較佳。
[光阻膜]
本發明中形成在含矽膜上之光阻膜,只要是塗佈含有因酸作用而改變極性而使得對於顯影液之溶解度變化之聚合物之光阻組成物而形成者即可。如此之光阻組成物可使用公知者。又,光阻膜之膜厚不特別限定,宜為約100nm至200nm較佳。
<半導體裝置基板之製造方法>
以下針對本發明之半導體裝置基板之製造方法參照圖式詳細說明。圖1係顯示本發明之半導體裝置基板之製造方法之一例之流程圖。
圖1之半導體裝置基板之製造方法中,首先準備半導體裝置製造用被加工體基板1(圖1(0)),作為(1)步驟,在半導體裝置製造用被加工體基板1之上形成有機下層膜2(圖1(1a)),並於有機下層膜2上塗佈含矽膜組成物並加熱,以形成含矽膜3(圖1(1b))。此時使含矽膜3中之矽含量為1質量%以上30質量%以下。然後,作為(2)步驟,在含矽膜3上塗佈光阻組成物並形成光阻膜4(圖1(2))。然後,作為(3)步驟,將光阻膜4曝光(圖1(3a))並顯影而形成光阻圖案4’(圖1(3b))。然後,作為(4)步驟,將光阻圖案4’作為乾蝕刻遮罩,利用乾蝕刻在含矽膜3轉印圖案(圖1(4))。然後,作為(5)步驟,將已轉印圖案之含矽膜3作為乾蝕刻遮罩,利用乾蝕刻在有機下層膜2轉印圖案(圖1(5))。此時調整乾蝕刻條件,使含矽膜3之一部分或全部殘留在有機下層膜2上。然後,作為(6)步驟,將以含矽膜3之
一部分或全部與有機下層膜2形成之圖案作為遮罩,對於半導體裝置製造用被加工體基板1注入離子(圖1(6))。然後,作為(7)步驟,將作為遮罩使用之殘留有含矽膜3之一部分或全部之有機下層膜2以剝離液同時剝離並除去(圖1(7))。
(3)步驟之曝光可使用公知方法進行,曝光光例如可使用KrF雷射、ArF雷射等。
又,(3)步驟之顯影可使用公知方法進行。顯影液,例如可使用鹼顯影液、有機溶劑顯影液,可以配合使用之光阻組成物適當選擇。
又,能以(6)步驟之離子注入進行注入之離子物種宜為硼、磷、砷、碳、氮、氧、氟、氬、矽、鎵、鍺、銦、及銻中之任一者較佳。
又,本發明中,於如上述(6)步驟,可將以含矽膜之一部分或全部與有機下層膜形成之圖案作為遮罩,對於半導體裝置製造用被加工體基板注入離子。
又,考量剝離之效率,如上述(7)步驟將作為離子注入之遮罩使用之殘留有含矽膜之一部分或全部之有機下層膜同時以剝離液剝離較佳,但當然也可分別剝離。
又,(7)步驟之剝離使用之剝離液宜使用含有過氧化氫者較佳。如此之剝離液特別適合含矽膜之濕式剝離。又,此時為了促進剝離,添加酸或鹼並調整pH更理想。此pH調整劑可列舉鹽酸、硫酸等無機酸、乙酸、草酸、酒石酸、檸檬
酸、乳酸等有機酸、氨、乙醇胺、氫氧化四甲基銨等含氮之鹼、EDTA(乙二胺4乙酸)等含氮之有機酸化合物等,尤其硫酸較佳。
更具體而言,作為對於半導體裝置基板不造成損害的剝離液,使用例如半導體製造處理一般使用之稱為SC1之含過氧化氫之氨水溶液、稱為SC2之含過氧化氫之鹽酸、及稱為SPM之硫酸過水等為宜。
又,(7)步驟之剝離,具體而言,例如:準備0℃~200℃,更佳為5℃~180℃之剝離液,將欲處理之已形成殘留有含矽膜之有機下層膜之被加工體基板浸漬於其中即可。又,若有必要,可利用在表面噴塗剝離液之邊使被加工體基板旋轉邊塗佈剝離液等常法的步驟而輕易地將含矽膜除去。
又,於(7)步驟,藉由以剝離液處理後,進一步以含有氟離子之剝離液予以剝離,能更確實度將離子注入使用之遮罩剝離。
又,於(7)步驟,藉由以剝離液處理後,進一步以含氨之洗滌液洗滌,能將剝離後之半導體裝置基板所附著之殘渣除去。
基板上之殘渣數目可以用顯微鏡檢查。若考慮基板上之晶片之良率,殘渣數目宜為50個以下較理想,10個以下更理想。
如上,依本發明之半導體裝置基板之製造方法,藉由將含矽膜中之矽含量調整成預定之範圍,即使含矽膜有一部分或全部殘留於有機下層膜上,也能以剝離液和有機下層膜一起剝離並除去。所以,即使是將以含矽膜與有機下層膜形成之圖案作為離子注入之遮罩時,仍能於離子注入後以剝離液輕易地且對於
半導體裝置基板不造成損害地進行濕式剝離。如上,能以3層處理對於離子注入後之基板不造成損害地進行加工,本發明特別適合3維電晶體之製造。
[實施例]
以下舉合成例、實驗例、比較實驗例、實施例、及比較例對於本發明具體說明,但本發明不限於該等記載。又,下列例中,%代表質量%,分子量測定係利用GPC實施。
[含矽化合物之合成]
(合成例1)
於乙醇400g、25%氫氧化四甲基銨5g、及去離子水200g之混合物中,添加單體[化100]19.8g及單體[化110]98.6g之混合物,於40℃保持並使其水解縮合4小時。反應結束後,加入乙酸2g使其中和,將副生醇以減壓餾去。於其中,添加乙酸乙酯1,200mL及丙二醇甲醚乙酸酯(以下稱為PGMEA)400g,將水層分液除去。於殘留的有機層加入離子交換水300mL並攪拌、靜置、分液。重複此處理3次。於殘留的有機層中加入PGMEA 500g後,減壓濃縮而獲得含矽化合物1(矽含量17%)之PGMEA溶液850g(化合物濃度9.9%)。測定其之聚苯乙烯換算分子量的結果為Mw=6,500。
(合成例2)
於乙醇400g、25%氫氧化四甲基銨5g、及去離子水200g之混合物中添加單體[化100]19.8g、單體[化110]73.9g、及單體[化111]23.6g之混合物,於40℃保持並使其水解縮合4小時。反應結束後加入乙酸2g使其中和,將副生醇以減壓餾去。於其中加入乙酸乙酯1,200mL及PGMEA400g,將水層分液除去。於殘留
的有機層加入離子交換水300mL並攪拌、靜置、分液。重複此處理3次。於殘留的有機層加入PGMEA 500g後,減壓濃縮而獲得含矽化合物2(矽含量17%)之PGMEA溶液860g(化合物濃度9.6%)。測定其之聚苯乙烯換算分子量的結果為Mw=6,600。
(合成例3)
於乙醇400g、25%氫氧化四甲基銨5g、及去離子水200g之混合物中添加單體[化100]19.8g、單體[化103]20.9g及單體[化110]73.9g之混合物,於40℃保持並使其水解縮合8小時。反應結束後添加乙酸2g,使其中和,將副生醇以減壓餾去。於其中添加乙酸乙酯1,200mL及PGMEA400g,將水層分液除去。於殘留的有機層加入離子交換水300mL並攪拌、靜置、分液。重複此處理3次。於殘留的有機層添加PGMEA 300g後,減壓濃縮而獲得含矽化合物3(矽含量19%)之PGMEA溶液670g(化合物濃度10.8%)。測定其之聚苯乙烯換算分子量的結果為Mw=8,800。
(合成例4)
於乙醇400g、25%氫氧化四甲基銨5g、及去離子水200g之混合物中添加單體[化104]21.2g、單體[化110]86.2g、及單體[化116]18.6g之混合物,於40℃保持並使其水解縮合8小時。反應結束後添加乙酸2g,使其中和,將副生醇以減壓餾去。於其中添加乙酸乙酯1,200mL及PGMEA400g,將水層分液除去。於殘留的有機層加入離子交換水300mL並攪拌、靜置、分液。重複此處理3次。於殘留的有機層中添加PGMEA 500g後,減壓濃縮而獲得含矽化合物4(矽含量16%)之PGMEA溶液920g(化合物濃度9.8%)。測定其之聚苯乙烯換算分子量的結果為Mw=7,400。
(合成例5)
於乙醇400g、25%氫氧化四甲基銨5g、及去離子水200g之混合物中添加單體[化100]19.8g、單體[化110]61.6g、及單體[化112]41.8g之混合物,於40℃保持並使其水解縮合8小時。反應結束後添加乙酸2g,使其中和,將副生醇以減壓餾去。於其中添加乙酸乙酯1,200mL及PGMEA400g,將水層分液除去。於殘留的有機層加入離子交換水300mL並攪拌、靜置、分液。重複此處理3次。於殘留的有機層中添加PGMEA 500g後,減壓濃縮而獲得含矽化合物5(矽含量16%)之PGMEA溶液940g(化合物濃度9.4%)。測定其之聚苯乙烯換算分子量的結果為Mw=7,200。
(合成例6)
於甲醇120g、70%硝酸1g、及去離子水60g之混合物中添加單體[化113]94.6g及單體[化114]41.2g之混合物,於40℃保持並使其水解縮合12小時。反應結束後添加丙二醇單乙醚(以下稱為PGEE)300g,將副生醇及過量的水以減壓餾去。於其中加入乙酸乙酯1,200mL,將水層分液除去。於殘留的有機層加入離子交換水300mL並攪拌、靜置、分液。重複此處理3次。於殘留的有機層加入PGEE 600g後,減壓濃縮而獲得含矽化合物6(矽含量14%)之PGEE溶液940g(化合物濃度9.4%)。測定其之聚苯乙烯換算分子量的結果為Mw=1,600。
(合成例7)
於甲醇120g、70%硝酸0.1g、及去離子水60g之混合物中添加單體[化100]9.9g、單體[化101]13.6g、及單體[化113]94.6g之混合物,於40℃保持並使其水解縮合12小時。反應結束後加入PGEE300g,將副生醇及過量的水以減壓
餾去。於其中加入乙酸乙酯1,200mL,將水層分液除去。於殘留的有機層加入離子交換水300mL並攪拌、靜置、分液。重複此處理3次。於殘留的有機層加入PGEE 600g後,減壓濃縮而獲得含矽化合物7(矽含量17%)之PGEE溶液860g(化合物濃度9.8%)。測定其之聚苯乙烯換算分子量的結果為Mw=2,500。
(合成例8)
於甲醇200g、70%硝酸0.2g、及去離子水100g之混合物中添加單體[化105]11.4g、單體[化113]67.6g、及單體[化116]74.5g之混合物,於40℃保持並使其水解縮合12小時。反應結束後加入PGEE300g,將副生醇及過量的水以減壓餾去。於其中添加乙酸乙酯1,200mL,將水層分液除去。於殘留的有機層加入離子交換水300mL並攪拌、靜置、分液。重複此處理3次。於殘留的有機層添加PGEE 800g後,減壓濃縮而獲得含矽化合物8(矽含量13%)之PGEE溶液1,070g(化合物濃度10.3%)。測定其之聚苯乙烯換算分子量的結果為Mw=1,500。
(合成例9)
於甲醇120g、70%硝酸0.1g、及去離子水60g之混合物中添加單體[化100]9.9g、單體[化101]13.6g、單體[化102]30.4g、及單體[化114]41.2g之混合物,於40℃保持並使其水解縮合12小時。反應結束後加入PGEE300g,將副生醇及過量的水以減壓餾去。於其中加入乙酸乙酯1,200mL,將水層分液除去。於殘留的有機層加入離子交換水300mL並攪拌、靜置、分液。重複此處理3次。於殘留的有機層加入PGEE 400g後,減壓濃縮而獲得含矽化合物9(矽含量25%)之PGEE溶液630g(化合物濃度8.9%)。測定其之聚苯乙烯換算分子量的結果為Mw=3,100。
(合成例10)
於甲醇120g、70%硝酸0.1g、及去離子水60g之混合物中添加單體[化100]5.0g、單體[化101]17.0g、單體[化102]34.2g、單體[化116]18.6g、單體[化117]2.5g、及單體[化118]5.2g之混合物,於40℃保持並使其水解縮合12小時。反應結束後添加PGEE200g,將副生醇及過量的水以減壓餾去。於其中添加乙酸乙酯1,000mL,將水層分液除去。於殘留的有機層中加入離子交換水250mL並攪拌、靜置、分液。重複此處理3次。於殘留的有機層中加入PGEE 200g後,減壓濃縮而獲得含矽化合物10(矽含量29%)之PGEE溶液380g(化合物濃度10.9%)。測定其之聚苯乙烯換算分子量的結果為Mw=2,500。
(合成例11)
於甲醇120g、70%硝酸0.1g、及去離子水60g之混合物添加單體[化100]9.9g、單體[化101]13.6g、單體[化102]30.4g、及單體[化115]29.8g之混合物,於40℃保持並使其水解縮合12小時。反應結束後加入PGEE300g,將副生醇及過量的水以減壓餾去。於其中加入乙酸乙酯1,200mL,將水層分液除去。於殘留的有機層加入離子交換水300mL並攪拌、靜置、分液。重複此處理3次。於殘留的有機層中加入PGEE 200g後、減壓濃縮而獲得含矽化合物11(矽含量31%)之PGEE溶液430g(化合物濃度10.4%)。測定其之聚苯乙烯換算分子量的結果為Mw=2,900。
(合成例12)
於甲醇120g、70%硝酸0.1g、及去離子水60g之混合物中添加單體[化100]5.0g、單體[化101]20.4g、單體[化102]38.1g、單體[化117]2.5g、及單體[化118]5.2g之混合物,於40℃保持並使其水解縮合12小時。反應結束後添加
PGEE200g,將副生醇及過量的水以減壓餾去。於其中添加乙酸乙酯800mL,將水層分液除去。於殘留的有機層加入離子交換水200mL並攪拌、靜置、分液。重複此處理3次。於殘留的有機層中加入PGEE 200g後,減壓濃縮而獲得含矽化合物12(矽含量38%)之PGEE溶液290g(化合物濃度11.0%)。測定其之聚苯乙烯換算分子量的結果為Mw=3,200。
以下揭示合成例使用之單體。
[含矽膜形成用組成物溶液之製備]
將上述合成例獲得之含矽化合物、添加劑、溶劑以表1A及表1B所示之比例混合,以0.1μm之氟樹脂製濾器過濾,以分別製備含矽膜形成用組成物溶液,各命名為Sol.1~25。
【表1A】
【表1B】
TPSMA:馬來酸單(三苯基鋶)
BnTBATf:三氟甲烷磺酸苄基三丁基銨
含氟之聚合物:
紫外線吸收劑:
[實驗例‧比較實驗例]
(圖案化試驗)
於矽晶圓上以膜厚200nm形成信越化學工業(股)製旋塗式碳膜ODL-50(碳含量80質量%)。於其上塗佈含矽膜形成用組成物溶液Sol.1~25,於200℃加熱60秒,而形成膜厚35nm之含矽膜Film1~25。
然後,在Film1~25上塗佈表2記載之正顯影用ArF光阻溶液(PR-1),於110℃烘烤60秒,形成膜厚250nm之光阻層(光阻膜)。
然後,將其以ArF曝光裝置(Nikon(股)製;NSR-S307E,NA0.85、σ0.85、0.93/0.85)曝光,於110℃烘烤(PEB)90秒,以2.38質量%四甲基氫氧化銨(TMAH)水溶液顯影30秒,獲得120nm 1:1之正型之線與間距圖案。以日立先端科技(股)製電子顯微鏡(CG4000)觀測得到之圖案之圖案崩塌,以日立製作所(股)製電子顯微鏡(S-9380)觀測剖面形狀。結果示於表3。
ArF光阻聚合物1:分子量(Mw)=6,800
分散度(Mw/Mn)=1.68
酸產生劑(PAG1):九氟丁烷磺酸三苯基鋶
鹼(Quencher):三乙醇胺
【表3】
如表3,於含矽膜中之矽含量為1~30質量%之實驗例1~22(Film1~22)、與含矽膜中之矽含量超過30質量%之比較實驗例1~3(Film23~25)中之任一者,均獲得有垂直剖面形狀之圖案,且未發生圖案崩塌。
[實施例‧比較例]
(圖案蝕刻‧離子注入‧濕式剝離試驗)
對於在上述圖案化試驗形成了光阻圖案之矽晶圓,將形成之光阻圖案作為遮罩,以條件(1)進行乾蝕刻,對於含矽膜轉印圖案。然後將已轉印圖案之含矽膜作為遮罩,以條件(2)進行乾蝕刻,對於旋塗式碳膜轉印圖案。又,此時旋塗式碳膜上殘留了一部分含矽膜。
(1)以CHF3/CF4系氣體之蝕刻條件
裝置:東京威力科創(股)製乾蝕刻裝置TeliusSP
蝕刻條件(1):
(2)以O2/N2系氣體之蝕刻條件
裝置:東京威力科創(股)製乾蝕刻裝置Telius SP
蝕刻條件(2):
腔室壓力2Pa
然後利用上述乾蝕刻形成圖案,將殘留一部分含矽膜之旋塗式碳膜作為遮罩,使用日新離子設備(股)製離子注入裝置EXCEED3000AH,以80keV、7X1015/cm2之條件對於矽晶圓注入硼離子。
然後對於以如上述方式進行了離子注入之矽晶圓,使用硫酸過水(H2SO4:H2O2:H2O=96:1:3)實施濕式剝離,將作為遮罩使用之殘留了一部分含矽膜之旋塗式碳膜除去後,使用光學顯微鏡計算遮罩之殘渣之數目。結果示於表4。
如表4可知:使用矽含量為1~30質量%之含矽膜(Film1~22)之實施例1~22中,剝離後幾乎無殘渣,離子注入後可以將離子注入使用之遮罩以剝離液進行濕式剝離。
另一方面,使用矽含量超過30質量%之含矽膜Film23~25之比較例1~3中,剝離後觀察到殘渣,可知:離子注入後無法以剝離液將離子注入使用之遮罩予以濕式剝離。
由以上可知:若為本發明之半導體裝置基板之製造方法,於使用含矽膜之半導體裝置基板之製造方法,可以將離子注入使用之遮罩以剝離液輕易且對於半導體裝置基板不造成損害地進行濕式剝離。
又,本發明不限於上述實施形態。上述實施形態為例示,和本發明之申請專利範圍記載之技術思想有實質上相同構成且發揮同樣作用效果者,均包括在本發明之技術範圍內。
1‧‧‧半導體裝置製造用被加工體基板
2‧‧‧有機下層膜
3‧‧‧含矽膜
4‧‧‧光阻膜
4’‧‧‧光阻圖案
Claims (18)
- 一種半導體裝置基板之製造方法,其特徵為包含以下步驟:(1)於半導體裝置製造用被加工體基板上形成有機下層膜,於該有機下層膜上塗佈含矽膜形成用組成物並加熱,以形成矽含量為1質量%以上30質量%以下之含矽膜;(2)在該含矽膜上塗佈含有因酸作用而改變極性並且改變對於顯影液之溶解度之聚合物之光阻組成物並形成光阻膜;(3)將該光阻膜曝光、顯影而形成光阻圖案;(4)將該光阻圖案作為乾蝕刻遮罩,利用乾蝕刻對於該含矽膜轉印圖案;(5)將該已轉印圖案之含矽膜作為乾蝕刻遮罩,利用乾蝕刻對於該有機下層膜轉印圖案,圖案轉印後使該含矽膜之一部分或全部殘留於已轉印該圖案之有機下層膜上;(6)將該已轉印圖案之有機下層膜作為遮罩,對於該半導體裝置製造用被加工體基板注入離子;及(7)將作為該離子注入之遮罩使用之殘留有該含矽膜之一部分或全部之有機下層膜以剝離液剝離。
- 如申請專利範圍第1項之半導體裝置基板之製造方法,其中,於該(6)步驟,將以該含矽膜之一部分或全部與該有機下層膜形成之圖案作為遮罩,對於該半導體裝置製造用被加工體基板注入離子。
- 如申請專利範圍第1或2項之半導體裝置基板之製造方法,其中,於該(7)步驟,將作為該離子注入之遮罩使用之殘留有該含矽膜之一部分或全部之有機下層膜同時以剝離液剝離。
- 如申請專利範圍第1或2項之半導體裝置基板之製造方法,其中,該剝離液含有過氧化氫。
- 如申請專利範圍第1或2項之半導體裝置基板之製造方法,其中,該剝離液含有硫酸。
- 如申請專利範圍第1或2項之半導體裝置基板之製造方法,其中,於該(7)步驟,以該剝離液處理後,進一步以含氟離子之剝離液進行剝離。
- 如申請專利範圍第1或2項之半導體裝置基板之製造方法,其中,於該(7)步驟,以該剝離液處理後,進一步以含氨之洗滌液進行洗滌。
- 如申請專利範圍第1或2項之半導體裝置基板之製造方法,其中,該半導體裝置製造用被加工體基板係使用已形成半導體電路之一部分或全部的半導體裝置基板,或已於該半導體裝置基板成膜了金屬膜、非晶金屬膜、金屬碳化膜、金屬氧化膜、金屬氮化膜、金屬氧化碳化膜、及金屬氧化氮化膜中之任一者的基板。
- 如申請專利範圍第8項之半導體裝置基板之製造方法,其中,該金屬包括矽、鈦、鎢、鉿、鋯、鉻、鍺、銅、銀、金、鋁、銦、鎵、砷、鈀、鐵、鉭、銥、鉬、或該等之合金。
- 如申請專利範圍第1或2項之半導體裝置基板之製造方法,其中,該離子注入之離子物種為硼、磷、砷、碳、氮、氧、氟、氬、矽、鎵、鍺、銦、及銻中之任一者。
- 如申請專利範圍第1或2項之半導體裝置基板之製造方法,其中,該含矽膜形成用組成物至少含有聚矽氧烷及溶劑。
- 如申請專利範圍第11項之半導體裝置基板之製造方法,其中,該聚矽氧烷含有交聯性有機基。
- 如申請專利範圍第12項之半導體裝置基板之製造方法,其中,該交聯性有機基為環氧基、苯酚基、及萘酚基中之任一者。
- 如申請專利範圍第11項之半導體裝置基板之製造方法,其中,該聚矽氧烷含有鹵化有機基。
- 如申請專利範圍第14項之半導體裝置基板之製造方法,其中,該鹵化有機基之鹵素為氟或氯。
- 如申請專利範圍第11項之半導體裝置基板之製造方法,其中,該含矽膜形成用組成物更含有因熱、光、或此兩者之作用而產生酸之酸產生劑。
- 如申請專利範圍第11項之半導體裝置基板之製造方法,其中,該含矽膜形成用組成物更含有含氟之有機化合物。
- 如申請專利範圍第11項之半導體裝置基板之製造方法,其中,該含矽膜形成用組成物更含有交聯劑。
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