WO2015111684A1 - 窒化チタン除去用液体組成物およびそれを用いた半導体素子の洗浄方法、並びに半導体素子の製造方法 - Google Patents
窒化チタン除去用液体組成物およびそれを用いた半導体素子の洗浄方法、並びに半導体素子の製造方法 Download PDFInfo
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- WO2015111684A1 WO2015111684A1 PCT/JP2015/051784 JP2015051784W WO2015111684A1 WO 2015111684 A1 WO2015111684 A1 WO 2015111684A1 JP 2015051784 W JP2015051784 W JP 2015051784W WO 2015111684 A1 WO2015111684 A1 WO 2015111684A1
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- group
- carbon atoms
- alkyl group
- substituted
- alkyl
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- 239000000203 mixture Substances 0.000 title claims abstract description 103
- 239000007788 liquid Substances 0.000 title claims abstract description 99
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims description 22
- 238000004140 cleaning Methods 0.000 title claims description 18
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 80
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 80
- 239000010937 tungsten Substances 0.000 claims abstract description 80
- 150000001875 compounds Chemical class 0.000 claims abstract description 52
- 239000011229 interlayer Substances 0.000 claims abstract description 47
- 150000003839 salts Chemical class 0.000 claims abstract description 47
- 239000000758 substrate Substances 0.000 claims abstract description 26
- 150000003973 alkyl amines Chemical class 0.000 claims abstract description 25
- 150000002222 fluorine compounds Chemical class 0.000 claims abstract description 21
- 239000007800 oxidant agent Substances 0.000 claims abstract description 17
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 12
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012935 ammoniumperoxodisulfate Substances 0.000 claims abstract description 8
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 193
- 125000004432 carbon atom Chemical group C* 0.000 claims description 153
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 119
- 125000003342 alkenyl group Chemical group 0.000 claims description 102
- 125000001153 fluoro group Chemical group F* 0.000 claims description 87
- -1 fluoroalkyl ether Chemical compound 0.000 claims description 65
- 229910052731 fluorine Inorganic materials 0.000 claims description 41
- 125000003709 fluoroalkyl group Chemical group 0.000 claims description 31
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 23
- 239000004065 semiconductor Substances 0.000 claims description 20
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- 229910019142 PO4 Inorganic materials 0.000 claims description 18
- 235000021317 phosphate Nutrition 0.000 claims description 18
- 239000010452 phosphate Substances 0.000 claims description 16
- 229910052794 bromium Inorganic materials 0.000 claims description 15
- 229910052801 chlorine Inorganic materials 0.000 claims description 15
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Natural products C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 15
- 125000005843 halogen group Chemical group 0.000 claims description 15
- 150000004693 imidazolium salts Chemical group 0.000 claims description 15
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 14
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 14
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims description 12
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 12
- 239000011734 sodium Substances 0.000 claims description 12
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 11
- 150000005215 alkyl ethers Chemical class 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 8
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 8
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 6
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- 239000011591 potassium Substances 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- MOVBJUGHBJJKOW-UHFFFAOYSA-N methyl 2-amino-5-methoxybenzoate Chemical compound COC(=O)C1=CC(OC)=CC=C1N MOVBJUGHBJJKOW-UHFFFAOYSA-N 0.000 claims description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 4
- 239000011698 potassium fluoride Substances 0.000 claims description 4
- 235000003270 potassium fluoride Nutrition 0.000 claims description 4
- NAWXUBYGYWOOIX-SFHVURJKSA-N (2s)-2-[[4-[2-(2,4-diaminoquinazolin-6-yl)ethyl]benzoyl]amino]-4-methylidenepentanedioic acid Chemical compound C1=CC2=NC(N)=NC(N)=C2C=C1CCC1=CC=C(C(=O)N[C@@H](CC(=C)C(O)=O)C(O)=O)C=C1 NAWXUBYGYWOOIX-SFHVURJKSA-N 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 claims description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 claims description 3
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-M dihydrogenphosphate Chemical compound OP(O)([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-M 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 16
- 230000007797 corrosion Effects 0.000 description 14
- 238000011282 treatment Methods 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical class OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 238000005530 etching Methods 0.000 description 6
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003002 pH adjusting agent Substances 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 101100269850 Caenorhabditis elegans mask-1 gene Proteins 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229960003237 betaine Drugs 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229920002120 photoresistant polymer Polymers 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- GJYWPRKIEORZLX-UHFFFAOYSA-M 1,3-didecyl-2-methylimidazol-1-ium;chloride Chemical compound [Cl-].CCCCCCCCCCN1C=C[N+](CCCCCCCCCC)=C1C GJYWPRKIEORZLX-UHFFFAOYSA-M 0.000 description 2
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 2
- OPXNHKQUEXEWAM-UHFFFAOYSA-M 1-dodecyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCCN1C=C[N+](C)=C1 OPXNHKQUEXEWAM-UHFFFAOYSA-M 0.000 description 2
- GKQHIYSTBXDYNQ-UHFFFAOYSA-M 1-dodecylpyridin-1-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+]1=CC=CC=C1 GKQHIYSTBXDYNQ-UHFFFAOYSA-M 0.000 description 2
- ZCPPLZJPPBIWRU-UHFFFAOYSA-M 1-hexadecyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCN1C=C[N+](C)=C1 ZCPPLZJPPBIWRU-UHFFFAOYSA-M 0.000 description 2
- YCMFMSOTJOUSLI-UHFFFAOYSA-M 1-hexadecyl-4-methylpyridin-1-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+]1=CC=C(C)C=C1 YCMFMSOTJOUSLI-UHFFFAOYSA-M 0.000 description 2
- LCXGSWXECDJESI-UHFFFAOYSA-M 1-methyl-3-octadecylimidazol-1-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCCN1C=C[N+](C)=C1 LCXGSWXECDJESI-UHFFFAOYSA-M 0.000 description 2
- SDXDXENAFAXVMX-UHFFFAOYSA-M 1-methyl-3-tetradecylimidazol-1-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCN1C=C[N+](C)=C1 SDXDXENAFAXVMX-UHFFFAOYSA-M 0.000 description 2
- GVUBEJANEHZYPA-UHFFFAOYSA-L 1-octyl-4-(1-octylpyridin-1-ium-4-yl)pyridin-1-ium;dibromide Chemical compound [Br-].[Br-].C1=C[N+](CCCCCCCC)=CC=C1C1=CC=[N+](CCCCCCCC)C=C1 GVUBEJANEHZYPA-UHFFFAOYSA-L 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 2
- JVQOASIPRRGMOS-UHFFFAOYSA-M dodecyl(trimethyl)azanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCC[N+](C)(C)C JVQOASIPRRGMOS-UHFFFAOYSA-M 0.000 description 2
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- WJLUBOLDZCQZEV-UHFFFAOYSA-M hexadecyl(trimethyl)azanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCCCCCC[N+](C)(C)C WJLUBOLDZCQZEV-UHFFFAOYSA-M 0.000 description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 2
- PPNHCZHNVOCMHS-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCCCC[N+](C)(C)C PPNHCZHNVOCMHS-UHFFFAOYSA-M 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- HTZVLLVRJHAJJF-UHFFFAOYSA-M 1-decyl-3-methylimidazolium chloride Chemical compound [Cl-].CCCCCCCCCCN1C=C[N+](C)=C1 HTZVLLVRJHAJJF-UHFFFAOYSA-M 0.000 description 1
- HJUPHPDWOUZDKH-UHFFFAOYSA-M 1-decylpyridin-1-ium;chloride Chemical compound [Cl-].CCCCCCCCCC[N+]1=CC=CC=C1 HJUPHPDWOUZDKH-UHFFFAOYSA-M 0.000 description 1
- XQIHTJQRSIYLSU-UHFFFAOYSA-L 1-methyl-4-(1-tetradecylpyridin-1-ium-4-yl)pyridin-1-ium;dibromide Chemical compound [Br-].[Br-].C1=C[N+](CCCCCCCCCCCCCC)=CC=C1C1=CC=[N+](C)C=C1 XQIHTJQRSIYLSU-UHFFFAOYSA-L 0.000 description 1
- YFVBASFBIJFBAI-UHFFFAOYSA-M 1-tetradecylpyridin-1-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+]1=CC=CC=C1 YFVBASFBIJFBAI-UHFFFAOYSA-M 0.000 description 1
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 1
- FGLHFQPDMSLJBI-UHFFFAOYSA-N 2-[2-(2-octadecoxyethoxy)ethoxy]ethyl dihydrogen phosphate Chemical compound [H]OP(=O)(O[H])OC([H])([H])C([H])([H])OC([H])([H])C([H])([H])OC([H])([H])C([H])([H])OC([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])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])[H] FGLHFQPDMSLJBI-UHFFFAOYSA-N 0.000 description 1
- IZBZQUREHISXFJ-UHFFFAOYSA-N 2-[4-chloro-5-methyl-3-(trifluoromethyl)pyrazol-1-yl]acetic acid Chemical compound CC1=C(Cl)C(C(F)(F)F)=NN1CC(O)=O IZBZQUREHISXFJ-UHFFFAOYSA-N 0.000 description 1
- QCAHUFWKIQLBNB-UHFFFAOYSA-N 3-(3-methoxypropoxy)propan-1-ol Chemical compound COCCCOCCCO QCAHUFWKIQLBNB-UHFFFAOYSA-N 0.000 description 1
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 description 1
- OXFBEEDAZHXDHB-UHFFFAOYSA-M 3-methyl-1-octylimidazolium chloride Chemical compound [Cl-].CCCCCCCCN1C=C[N+](C)=C1 OXFBEEDAZHXDHB-UHFFFAOYSA-M 0.000 description 1
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- CXRFDZFCGOPDTD-UHFFFAOYSA-M Cetrimide Chemical compound [Br-].CCCCCCCCCCCCCC[N+](C)(C)C CXRFDZFCGOPDTD-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 description 1
- OKZROTDSNDMSHM-UHFFFAOYSA-N FC(C(=O)O)(N(C(F)(F)F)C(F)(F)F)C(C(C(C(C(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F Chemical compound FC(C(=O)O)(N(C(F)(F)F)C(F)(F)F)C(C(C(C(C(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F OKZROTDSNDMSHM-UHFFFAOYSA-N 0.000 description 1
- MAQOZCVPCRVOCW-UHFFFAOYSA-N N,N,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,12-heptacosafluorododecan-1-amine Chemical compound FN(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F MAQOZCVPCRVOCW-UHFFFAOYSA-N 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- 241000282320 Panthera leo Species 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229940107816 ammonium iodide Drugs 0.000 description 1
- ZRDJERPXCFOFCP-UHFFFAOYSA-N azane;iodic acid Chemical compound [NH4+].[O-]I(=O)=O ZRDJERPXCFOFCP-UHFFFAOYSA-N 0.000 description 1
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 description 1
- TTZLKXKJIMOHHG-UHFFFAOYSA-M benzyl-decyl-dimethylazanium;chloride Chemical compound [Cl-].CCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 TTZLKXKJIMOHHG-UHFFFAOYSA-M 0.000 description 1
- UHWHEIKTDHONME-UHFFFAOYSA-M benzyl-decyl-dimethylazanium;hydroxide Chemical compound [OH-].CCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 UHWHEIKTDHONME-UHFFFAOYSA-M 0.000 description 1
- OCBHHZMJRVXXQK-UHFFFAOYSA-M benzyl-dimethyl-tetradecylazanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 OCBHHZMJRVXXQK-UHFFFAOYSA-M 0.000 description 1
- XLJOZOQVNCBJMT-UHFFFAOYSA-M benzyl-dimethyl-tetradecylazanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 XLJOZOQVNCBJMT-UHFFFAOYSA-M 0.000 description 1
- VEYPOAHLDFFNPD-UHFFFAOYSA-M benzyl-dodecyl-dimethylazanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 VEYPOAHLDFFNPD-UHFFFAOYSA-M 0.000 description 1
- LAUPTJWHHKNSCT-UHFFFAOYSA-M benzyl-hexadecyl-dimethylazanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 LAUPTJWHHKNSCT-UHFFFAOYSA-M 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- SXPWTBGAZSPLHA-UHFFFAOYSA-M cetalkonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 SXPWTBGAZSPLHA-UHFFFAOYSA-M 0.000 description 1
- 229960000228 cetalkonium chloride Drugs 0.000 description 1
- YMKDRGPMQRFJGP-UHFFFAOYSA-M cetylpyridinium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+]1=CC=CC=C1 YMKDRGPMQRFJGP-UHFFFAOYSA-M 0.000 description 1
- ZRKZFNZPJKEWPC-UHFFFAOYSA-N decylamine-N,N-dimethyl-N-oxide Chemical compound CCCCCCCCCC[N+](C)(C)[O-] ZRKZFNZPJKEWPC-UHFFFAOYSA-N 0.000 description 1
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 description 1
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 1
- 229940075557 diethylene glycol monoethyl ether Drugs 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- BHCBQALBZYVPNR-UHFFFAOYSA-N dodecyl 2-amino-2-methylpropanoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)(C)N BHCBQALBZYVPNR-UHFFFAOYSA-N 0.000 description 1
- SYELZBGXAIXKHU-UHFFFAOYSA-N dodecyldimethylamine N-oxide Chemical compound CCCCCCCCCCCC[N+](C)(C)[O-] SYELZBGXAIXKHU-UHFFFAOYSA-N 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 150000003840 hydrochlorides Chemical group 0.000 description 1
- 229910000043 hydrogen iodide Inorganic materials 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- YWWNNLPSZSEZNZ-UHFFFAOYSA-N n,n-dimethyldecan-1-amine Chemical compound CCCCCCCCCCN(C)C YWWNNLPSZSEZNZ-UHFFFAOYSA-N 0.000 description 1
- YWFWDNVOPHGWMX-UHFFFAOYSA-N n,n-dimethyldodecan-1-amine Chemical compound CCCCCCCCCCCCN(C)C YWFWDNVOPHGWMX-UHFFFAOYSA-N 0.000 description 1
- IBOBFGGLRNWLIL-UHFFFAOYSA-N n,n-dimethylhexadecan-1-amine oxide Chemical compound CCCCCCCCCCCCCCCC[N+](C)(C)[O-] IBOBFGGLRNWLIL-UHFFFAOYSA-N 0.000 description 1
- UQKAOOAFEFCDGT-UHFFFAOYSA-N n,n-dimethyloctan-1-amine Chemical compound CCCCCCCCN(C)C UQKAOOAFEFCDGT-UHFFFAOYSA-N 0.000 description 1
- SFBHPFQSSDCYSL-UHFFFAOYSA-N n,n-dimethyltetradecan-1-amine Chemical compound CCCCCCCCCCCCCCN(C)C SFBHPFQSSDCYSL-UHFFFAOYSA-N 0.000 description 1
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 description 1
- GMTCPFCMAHMEMT-UHFFFAOYSA-N n-decyldecan-1-amine Chemical compound CCCCCCCCCCNCCCCCCCCCC GMTCPFCMAHMEMT-UHFFFAOYSA-N 0.000 description 1
- MJCJUDJQDGGKOX-UHFFFAOYSA-N n-dodecyldodecan-1-amine Chemical compound CCCCCCCCCCCCNCCCCCCCCCCCC MJCJUDJQDGGKOX-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- HVZWVEKIQMJYIK-UHFFFAOYSA-N nitryl chloride Chemical compound [O-][N+](Cl)=O HVZWVEKIQMJYIK-UHFFFAOYSA-N 0.000 description 1
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- LXPCOISGJFXEJE-UHFFFAOYSA-N oxifentorex Chemical compound C=1C=CC=CC=1C[N+](C)([O-])C(C)CC1=CC=CC=C1 LXPCOISGJFXEJE-UHFFFAOYSA-N 0.000 description 1
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-O pyridinium Chemical group C1=CC=[NH+]C=C1 JUJWROOIHBZHMG-UHFFFAOYSA-O 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- ABVVEAHYODGCLZ-UHFFFAOYSA-N tridecan-1-amine Chemical compound CCCCCCCCCCCCCN ABVVEAHYODGCLZ-UHFFFAOYSA-N 0.000 description 1
- SWZDQOUHBYYPJD-UHFFFAOYSA-N tridodecylamine Chemical compound CCCCCCCCCCCCN(CCCCCCCCCCCC)CCCCCCCCCCCC SWZDQOUHBYYPJD-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/004—Surface-active compounds containing F
- C11D1/006—Surface-active compounds containing fluorine and phosphorus
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/29—Sulfates of polyoxyalkylene ethers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/34—Derivatives of acids of phosphorus
- C11D1/345—Phosphates or phosphites
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0073—Anticorrosion compositions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/122—Sulfur-containing, e.g. sulfates, sulfites or gypsum
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/24—Organic compounds containing halogen
- C11D3/245—Organic compounds containing halogen containing fluorine
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/39—Organic or inorganic per-compounds
- C11D3/3947—Liquid compositions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/08—Acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/10—Salts
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3209—Amines or imines with one to four nitrogen atoms; Quaternized amines
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/36—Organic compounds containing phosphorus
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
- C23G1/06—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
- C23G1/061—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors nitrogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/106—Other heavy metals refractory metals
-
- 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
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/0206—Cleaning during device manufacture during, before or after processing of insulating layers
- H01L21/02063—Cleaning during device manufacture during, before or after processing of insulating layers the processing being the formation of vias or contact holes
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/3213—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer
- H01L21/32133—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only
- H01L21/32134—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only by liquid etching only
-
- 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
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76801—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing
- H01L21/76802—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing by forming openings in dielectrics
- H01L21/76814—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing by forming openings in dielectrics post-treatment or after-treatment, e.g. cleaning or removal of oxides on underlying conductors
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/311—Etching the insulating layers by chemical or physical means
- H01L21/31144—Etching the insulating layers by chemical or physical means using masks
Definitions
- the present invention relates to a liquid composition, and more particularly, a liquid composition for removing titanium nitride used for a hard mask without corroding tungsten and a low dielectric constant interlayer insulating film used for wiring in a manufacturing process of a semiconductor device. And a method for cleaning a semiconductor element using the same, and a method for manufacturing a semiconductor element.
- tungsten and titanium nitride are used as a wiring material, and titanium nitride is recently used as a hard mask.
- titanium nitride In a semiconductor substrate in which tungsten and titanium nitride coexist on the surface, for example, when tungsten is used as a wiring and titanium nitride is used as a hard mask, it is required to remove titanium nitride without corroding tungsten. Titanium nitride can be removed relatively easily by using a composition containing hydrogen peroxide, but hydrogen peroxide is difficult to use because it is highly corrosive to tungsten. In addition, there is a need to increase the etch selectivity of titanium nitride to tungsten.
- Patent Document 1 discloses a quaternary ammonium and a salt thereof, a quaternary pyridinium and a salt thereof, a quaternary bipyridinium and a salt thereof, and a corrosion inhibitor using a quaternary imidazolium and a salt thereof.
- the anticorrosive agent disclosed in Cited Document 1 does not have sufficient anticorrosive effect on tungsten.
- Patent Document 2 concentrated sulfuric acid is used as a composition that does not use hydrogen peroxide, and titanium nitride can be etched without corroding tungsten.
- the etching rate of titanium nitride is as slow as 3 to 15 mm / min, and it is not practical when used for removing a titanium nitride hard mask having a thickness of usually several hundred to several thousand mm.
- Patent Document 3 titanium nitride can be etched without corroding tungsten using a composition containing an oxidizing agent, a fluorine compound, and an anticorrosive.
- the cited document 3 has problems such as low removal of titanium nitride and insufficient corrosion protection effect of tungsten.
- the object of the present invention is to solve at least one of the above conventional problems. Furthermore, the present invention provides a liquid composition capable of removing titanium nitride from a substrate including titanium nitride, tungsten and a low dielectric constant interlayer insulating film without corroding tungsten and the low dielectric constant interlayer insulating film, and a semiconductor using the same It is an object to provide a method for cleaning an element and a method for manufacturing a semiconductor element.
- the present inventors have found that the above problems can be solved by using a liquid composition containing a specific oxidizing agent, a fluorine compound, and a tungsten anticorrosive. That is, the present invention is as follows.
- Titanium nitride is removed from a substrate having titanium nitride, tungsten, and a low dielectric constant interlayer insulating film without corroding tungsten and the low dielectric constant interlayer insulating film, (A) an oxidizing agent that is at least one selected from the group consisting of potassium permanganate, ammonium peroxodisulfate, potassium peroxodisulfate, and sodium peroxodisulfate, (B) a fluorine compound, and (C) a tungsten anticorrosive, And a liquid composition having a pH value of 0 to 4, (C) the tungsten anticorrosive is an alkylamine and a salt thereof, a fluoroalkylamine and a salt thereof, an alkylamine oxide, a fluoroalkylamine oxide, an alkylbetaine, a fluoroalkylbetaine, an alkyl quaternary ammonium and a salt thereof, a fluorine compound
- the liquid composition according to ⁇ 1> which does not contain hydrogen peroxide.
- the fluorine compound (B) is at least one selected from the group consisting of hydrofluoric acid, ammonium fluoride, acidic ammonium fluoride, tetramethylammonium fluoride, potassium fluoride, hexafluorosilicic acid, and tetrafluoroboric acid. It is a liquid composition as described in ⁇ 1> above.
- the liquid composition according to ⁇ 1>, wherein the alkylamine or fluoroalkylamine in the C1 compound group is represented by the following general formula (1).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms.
- R 2 and R 3 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- the alkylamine salt or fluoroalkylamine salt in the C1 compound group is hydrochloride, nitrate, acetate, methanesulfonate, chlorate, perchlorate, hydrofluoride, hydrobromic acid ⁇ 1 which is at least one selected from the group consisting of a salt, hydroiodide, hydrogen sulfate, sulfate, hydrogen carbonate, carbonate, dihydrogen phosphate, hydrogen phosphate, and phosphate > Is a liquid composition described in the above.
- the liquid composition according to ⁇ 1>, wherein the alkylamine oxide or fluoroalkylamine oxide in the C1 compound group is represented by the following general formula (2).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms.
- R 2 and R 3 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- the liquid composition according to ⁇ 1>, wherein the alkylbetaine or fluoroalkylbetaine in the C1 compound group is represented by the following general formula (3) or (4).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms.
- R 2 and R 3 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms.
- R 2 and R 3 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- R 2 , R 3 and R 4 each represent a hydrogen atom, an alkyl group having 1 to 4 carbon atoms, a phenyl group or a benzyl group, and a part or all of the hydrogen atoms bonded to the alkyl group are substituted with fluorine atoms. Also good. ] [Wherein R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 , R 3 and R 4 each represent a hydrogen atom, an alkyl group having 1 to 4 carbon atoms, a phenyl group or a benzyl group, and a part or all of the hydrogen atoms bonded to the alkyl group are substituted with fluorine atoms. Also good.
- X represents a halogen atom: F, Cl, Br, or I. ] [Wherein R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 , R 3 and R 4 each represent a hydrogen atom, an alkyl group having 1 to 4 carbon atoms, a phenyl group or a benzyl group, and a part or all of the hydrogen atoms bonded to the alkyl group are substituted with fluorine atoms. Also good. ] ⁇ 9>
- the liquid quaternary pyridinium salt or fluoroalkyl quaternary pyridinium salt in the C1 compound group is the liquid composition according to the above ⁇ 1>, which is represented by the following general formula (8).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms.
- R 2 , R 3 , R 4 , R 5 and R 6 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group are substituted with fluorine atoms.
- X represents a halogen atom: F, Cl, Br, or I.
- R 3 to R 10 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- X represents a halogen atom: F, Cl, Br, or I.
- the alkyl quaternary imidazolium salt or fluoroalkyl quaternary imidazolium salt in the C1 compound group is the liquid composition according to the above ⁇ 1>, which is represented by the following general formula (10) or (11). .
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms.
- R 2 represents an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- R 3 to R 5 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- X represents a halogen atom: F, Cl, Br, or I.
- R 1 and R 2 represent an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of hydrogen atoms bonded to the alkyl group or alkenyl group are fluorine atoms. May be substituted.
- R 3 to R 5 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- X represents a halogen atom: F, Cl, Br, or I.
- the liquid composition according to ⁇ 1>, wherein the polyoxyalkylene alkyl ether or polyoxyalkylene fluoroalkyl ether in the C2 compound group is represented by the following general formula (13).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 represents an alkanediyl group having 2 to 6 carbon atoms, and n represents an integer of 2 to 20.
- R 1 and R 2 represent an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of hydrogen atoms bonded to the alkyl group or alkenyl group are fluorine atoms. May be substituted.
- R 3 and R 4 represent an alkanediyl group having 2 to 6 carbon atoms, m and n represent an integer of 2 to 20, and m and n may be the same or different.
- R 2 represents an alkanediyl group having 2 to 6 carbon atoms, and n represents a number of 2 to 20.
- M represents sodium (Na), potassium (K), or ammonium (NH 4 ).
- the liquid composition according to ⁇ 1>, wherein the alkyl diphenyl ether sulfonate or the fluoroalkyl diphenyl ether sulfonate in the C2 compound group is represented by the following general formula (17).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. It may be.
- M represents sodium (Na), potassium (K), or ammonium (NH 4 ).
- ⁇ 17> The liquid composition according to ⁇ 1>, wherein the concentration of ammonium peroxodisulfate, potassium peroxodisulfate, or sodium peroxodisulfate in the (A) oxidizing agent is 0.1 to 20% by mass.
- a method for manufacturing a semiconductor element in which titanium nitride is removed from a substrate having titanium nitride, tungsten, and a low dielectric constant interlayer insulating film without corroding tungsten and the low dielectric constant interlayer insulating film,
- a method for producing a semiconductor device comprising bringing a liquid composition according to any one of ⁇ 1> to ⁇ 19> above into contact with a substrate having tungsten and a low dielectric constant interlayer insulating film.
- the liquid composition of the present invention can remove titanium nitride in a substrate having titanium nitride, tungsten, and a low dielectric constant interlayer insulating film without corroding tungsten and the low dielectric constant interlayer insulating film.
- FIG. 1 is a schematic view showing a cross section of a semiconductor element including a titanium nitride hard mask 1, a tungsten wiring 2, and a low dielectric constant interlayer insulating film 3.
- FIG. 1 is a schematic view showing a cross section of a semiconductor element including a titanium nitride hard mask 1, a tungsten wiring 2, and a low dielectric constant interlayer insulating film 3.
- the liquid composition of the present invention is used for removing titanium nitride in a substrate having titanium nitride and tungsten and a low dielectric constant interlayer insulating film without corroding tungsten and the low dielectric constant interlayer insulating film.
- the oxidizing agent contained in the liquid composition of the present invention functions as an oxidizing agent for titanium nitride.
- component (A) functions as an oxidizing agent for titanium nitride.
- One feature of the liquid composition of the present invention is that it does not contain hydrogen peroxide. Since the liquid composition of the present invention does not contain hydrogen peroxide, there is no problem of corroding tungsten.
- the oxidizing agent include potassium permanganate, ammonium peroxodisulfate, potassium peroxodisulfate, and sodium peroxodisulfate. These oxidizing agents may be used alone or in combination of two or more.
- the content of potassium permanganate as component (A) in the liquid composition of the present invention is preferably 0.001% by mass to 0.1% by mass, and 0.005% by mass to 0.1% by mass. %, More preferably 0.005% by mass to 0.05% by mass.
- the content of potassium permanganate (component (A)) in the liquid composition of the present invention is within the above range, the titanium nitride is highly removable and does not corrode tungsten and the low dielectric constant interlayer insulating film.
- the higher the potassium permanganate concentration the higher the titanium nitride removability.
- the corrosiveness of tungsten increases, so it is not preferable if the potassium permanganate concentration is too high.
- the content of component (A) ammonium peroxodisulfate, potassium peroxodisulfate, and sodium peroxodisulfate in the liquid composition of the present invention is preferably 0.1% by mass to 20% by mass.
- the content is more preferably 1% by mass to 10% by mass, and particularly preferably 0.5% by mass to 10% by mass. If the content of ammonium peroxodisulfate, potassium peroxodisulfate, and sodium peroxodisulfate in the liquid composition of the present invention is within the above range, the titanium nitride is highly removable, and tungsten and a low dielectric constant interlayer insulating film are formed. Does not corrode.
- the fluorine compound contained in the liquid composition of the present invention has a titanium nitride etching function.
- the fluorine compound is selected from compounds having a fluorine atom.
- the fluorine compound include fluorine compounds such as hydrofluoric acid, ammonium fluoride, acidic ammonium fluoride, tetramethylammonium fluoride, potassium fluoride, hexafluorosilicic acid, ammonium hexafluorosilicate, tetrafluoroboric acid, and ammonium tetrafluoroborate.
- fluorine compounds may be used alone or in combination of two or more.
- hydrofluoric acid, ammonium fluoride, acidic ammonium fluoride, tetramethylammonium fluoride, and potassium fluoride are more preferable.
- hydrofluoric acid, ammonium fluoride, and acidic ammonium fluoride are preferable.
- the content of the fluorine compound as the component (B) in the liquid composition of the present invention is preferably in the range of 0.01 to 1% by mass, more preferably 0.05 to 1% by mass, It is particularly preferably 0.05 to 0.5% by mass. If the content of the fluorine compound in the liquid composition of the present invention is within the above range, the removal of titanium nitride is high and tungsten and the low dielectric constant interlayer insulating film are not corroded. The higher the concentration of the fluorine compound, the higher the removal of titanium nitride. On the other hand, the corrosivity of tungsten and the low dielectric constant interlayer insulating film increases, so it is not preferable that the concentration of the fluorine compound is too high.
- component (C) Tungsten anticorrosive
- the tungsten anticorrosive contained in the liquid composition of the present invention contains two or more different compounds selected from the C1 compound group. Alternatively, it includes one or more selected from the C1 compound group and one or more selected from the C2 compound group, and thereby has an anticorrosive function for tungsten.
- the C1 compound group (hereinafter sometimes referred to as “component (C1)”) includes alkylamines and salts thereof, fluoroalkylamines and salts thereof, alkylamine oxides, fluoroalkylamine oxides, alkylbetaines, fluoroalkyls.
- alkyl quaternary ammonium and its salt fluoroalkyl quaternary ammonium and its salt
- alkyl quaternary pyridinium salt fluoroalkyl quaternary pyridinium salt
- alkyl quaternary bipyridinium salt fluoroalkyl quaternary bipyridinium salt
- alkyl quaternary imidazolium Salts and fluoroalkyl quaternary imidazolium salts.
- the alkylamine or fluoroalkylamine is preferably represented by the following general formula (1).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 and R 3 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- Alkylamine salt or fluoroalkylamine salt is hydrochloride, nitrate, acetate, methanesulfonate, chlorate, perchlorate, hydrofluoride, hydrobromide, hydrogen iodide. It is at least one selected from the group consisting of acid salts, hydrogen sulfates, sulfates, hydrogen carbonates, carbonates, dihydrogen phosphates, hydrogen phosphates, and phosphates.
- alkylamine and its salt or fluoroalkylamine and its salt include, for example, octylamine, decylamine, dodecylamine, tetradecylamine, hexadecylamine, octadecylamine, dodecylamine hydrochloride, perfluorododecylamine, dioctyl Examples include amine, didecylamine, didodecylamine, trioctylamine, tridecylamine, tridodecylamine, octyldimethylamine, decyldimethylamine, and dodecyldimethylamine. Of these, dodecylamine, tetradecylamine, and hexadecylamine are preferable.
- the alkylamine oxide or fluoroalkylamine oxide is preferably represented by the following general formula (2).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 and R 3 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- alkylamine oxide or fluoroalkylamine oxide include, for example, N-decyl-N, N-dimethylamine oxide, N-dodecyl-N, N-dimethylamine oxide, N-tetradecyl-N, N-dimethylamine.
- Surflon® S-241 is preferred.
- the alkylbetaine or fluoroalkylbetaine is preferably represented by the following general formula (3) or (4).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 and R 3 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 and R 3 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- alkylbetaine or fluoroalkylbetaine include, for example, dodecyldimethylaminoacetic acid betaine, perfluorododecyldimethylaminoacetic acid betaine, dodecyldimethylaminosulfobetaine, perfluorododecyldimethylaminosulfobetaine, amphital (trade name, Daiichi Kogyo). And alkylbetaine manufactured by Pharmaceutical Co., Ltd.). Of these, Amphithr 20YB and Amphithr 24B are preferable.
- Alkyl quaternary ammonium and its salt or fluoroalkyl quaternary ammonium and its salt are preferably represented by the following general formula (5), (6) or (7).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 , R 3 and R 4 each represent a hydrogen atom, an alkyl group having 1 to 4 carbon atoms, a phenyl group or a benzyl group, and a part or all of the hydrogen atoms bonded to the alkyl group are substituted with fluorine atoms. Also good. ] [Wherein R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 , R 3 and R 4 each represent a hydrogen atom, an alkyl group having 1 to 4 carbon atoms, a phenyl group or a benzyl group, and a part or all of the hydrogen atoms bonded to the alkyl group are substituted with fluorine atoms. Also good.
- X represents a halogen atom: F, Cl, Br, or I. ] [Wherein R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 , R 3 and R 4 each represent a hydrogen atom, an alkyl group having 1 to 4 carbon atoms, a phenyl group or a benzyl group, and a part or all of the hydrogen atoms bonded to the alkyl group are substituted with fluorine atoms. Also good. ]
- alkyl quaternary ammonium and salts thereof or fluoroalkyl quaternary ammonium and salts thereof include, for example, dodecyltrimethylammonium hydroxide, tetradecyltrimethylammonium hydroxide, hexadecyltrimethylammonium hydroxide, and benzyldimethyldecylammonium hydroxide.
- the (C1) alkyl quaternary pyridinium salt or fluoroalkyl quaternary pyridinium salt is preferably represented by the following general formula (8).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 , R 3 , R 4 , R 5 and R 6 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group are substituted with fluorine atoms.
- X represents a halogen atom: F, Cl, Br, or I.
- (C1) alkyl quaternary pyridinium salts or fluoroalkyl quaternary pyridinium salts include, for example, 1-decylpyridinium chloride, 1-dodecylpyridinium chloride, 1-tetradecylpyridinium chloride, 1-hexadecylpyridinium chloride, and 1-hexadecyl-4-methylpyridinium chloride. Of these, 1-dodecylpyridinium chloride and 1-hexadecyl-4-methylpyridinium chloride are preferable.
- the (C1) alkyl quaternary bipyridinium salt or fluoroalkyl quaternary bipyridinium salt is preferably represented by the following general formula (9).
- R 1 and R 2 represent an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of hydrogen atoms bonded to the alkyl group or alkenyl group are fluorine atoms. May be substituted.
- R 3 to R 10 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- X represents a halogen atom: F, Cl, Br, or I.
- alkyl quaternary bipyridinium salt or the fluoroalkyl quaternary bipyridinium salt include, for example, 1,1′-di-n-octyl-4,4′-bipyridinium dibromide, 1-methyl-1′-tetradecyl-4 , 4′-bipyridinium dibromide, and 1,1′-di-n-perfluorooctyl-4,4′-bipyridinium dibromide. Of these, 1,1'-di-n-octyl-4,4'-bipyridinium dibromide is preferred.
- the (C1) alkyl quaternary imidazolium salt or fluoroalkyl quaternary imidazolium salt is preferably represented by the following general formula (10) or (11). [Wherein R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 represents an alkyl group having 1 to 4 carbon atoms
- R 3 to R 5 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group are fluorine atoms. May be substituted.
- X represents a halogen atom: F, Cl, Br, or I. ] [Wherein R 1 and R 2 represent an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of hydrogen atoms bonded to the alkyl group or alkenyl group are fluorine atoms. May be substituted.
- R 3 to R 5 represent a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group may be substituted with a fluorine atom.
- X represents a halogen atom: F, Cl, Br, or I. ]
- alkyl quaternary imidazolium salt or the fluoroalkyl quaternary imidazolium salt include, for example, 1-octyl-3-methylimidazolium chloride, 1-decyl-3-methylimidazolium chloride, 1-dodecyl-3- Methylimidazolium chloride, 1-tetradecyl-3-methylimidazolium chloride, 1-hexadecyl-3-methylimidazolium chloride, 1-octadecyl-3-methylimidazolium chloride, 1,3-didecyl-2-methylimidazolium chloride And 1-perfluorooctylimidazolium chloride.
- 1-dodecyl-3-methylimidazolium chloride 1-tetradecyl-3-methylimidazolium chloride, 1-hexadecyl-3-methylimidazolium chloride, 1-octadecyl-3-methylimidazolium chloride, and 1,3- Didecyl-2-methylimidazolium chloride is preferred.
- the C2 compound group (hereinafter sometimes referred to as “component (C2)”) includes polyoxyalkylene alkylamine, polyoxyalkylene fluoroalkylamine, polyoxyalkylene alkyl ether, polyoxyalkylene fluoroalkyl ether, polyoxyalkylene fluoroalkyl ether, Examples include oxyalkylene alkyl phosphate ester, polyoxyalkylene fluoroalkyl phosphate ester, polyoxyalkylene alkyl ether sulfate, polyoxyalkylene fluoroalkyl ether sulfate, alkyl diphenyl ether sulfonate, and fluoroalkyl diphenyl ether sulfonate.
- the polyoxyalkylene alkylamine or polyoxyalkylene fluoroalkylamine is preferably represented by the following general formula (12).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 and R 3 represent an alkanediyl group having 2 to 6 carbon atoms, m and n represent an integer of 2 to 20, and m and n may be the same or different.
- polyoxyalkylene alkylamine or polyoxyalkylene fluoroalkylamine include, for example, Neimine (trade name, polyoxyethylene alkylamine manufactured by NOF Corporation), Neugen (trade name, manufactured by Daiichi Kogyo Seiyaku Co., Ltd. Oxyethylene alkylamine), and the like.
- Neimine® F-215, Neugen® ET-189, and Neugen® XL-140 are preferable.
- the polyoxyalkylene alkyl ether or polyoxyalkylene fluoroalkyl ether is preferably represented by the following general formula (13).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 represents an alkanediyl group having 2 to 6 carbon atoms, and n represents an integer of 2 to 20.
- polyoxyalkylene alkyl ether or the polyoxyalkylene fluoroalkyl ether include, for example, New Coal (trade name, alkyl ether type nonionic surfactant manufactured by Nippon Emulsifier Co., Ltd.), Footage (trade name, Neos Co., Ltd.) Polyoxyethylene perfluoroalkyl ether), anti-floss (trade name, special nonionic surfactant manufactured by Daiichi Kogyo Seiyaku Co., Ltd.), and the like.
- New Coal® 2308-LY, Anti-Floss® M-9, Aftergent® 222F, Aftergent® 250, and Aftergent® 251 are preferable.
- the polyoxyalkylene alkyl phosphate ester or the polyoxyalkylene fluoroalkyl phosphate ester is preferably represented by the following general formula (14) or (15).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. May be.
- R 2 represents an alkanediyl group having 2 to 6 carbon atoms, and n represents an integer of 2 to 20.
- R 1 and R 2 represent an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of hydrogen atoms bonded to the alkyl group or alkenyl group are fluorine atoms. May be substituted.
- R 3 and R 4 represent an alkanediyl group having 2 to 6 carbon atoms, m and n represent an integer of 2 to 20, and m and n may be the same or different.
- polyoxyalkylene alkyl phosphate ester or the polyoxyalkylene fluoroalkyl phosphate ester include phosphanol (trade name, polyoxyethylene phosphate ester manufactured by Toho Chemical Industry Co., Ltd.).
- Phosphanol RA-600, Phosphanol RS-710, Phosphanol RL-310, Phosphanol ED-230, Phosphanol or iD10-P, Phosphanol ML-240, Phosphanol OF- 100 is preferred.
- the polyoxyalkylene alkyl ether sulfate or polyoxyalkylene fluoroalkyl ether sulfate is preferably represented by the following general formula (16).
- R 1 represents an alkyl group having 8 to 18 carbon atoms, an alkenyl group having 8 to 18 carbon atoms, a phenyl group or a benzyl group, and a part or all of the hydrogen atoms bonded to the alkyl group or alkenyl group are It may be substituted with a fluorine atom.
- R 2 represents an alkanediyl group having 2 to 6 carbon atoms, and n represents an integer of 2 to 20.
- M represents sodium (Na), potassium (K), or ammonium (NH 4 ).
- polyoxyalkylene alkyl ether sulfate or polyoxyalkylene fluoroalkyl ether sulfate include, for example, hightenol (trade name, polyoxyethylene alkyl ether sulfonic acid manufactured by Daiichi Kogyo Seiyaku Co., Ltd.). Of these, high tenol NF-08, high tenol NF-13, and high tenol NF-17 are preferred.
- the alkyl diphenyl ether sulfonate or the fluoroalkyl diphenyl ether sulfonate is preferably represented by the following general formula (17).
- R 1 represents an alkyl group having 8 to 18 carbon atoms or an alkenyl group having 8 to 18 carbon atoms, and a part or all of hydrogen atoms bonded to the alkyl group or alkenyl group are substituted with fluorine atoms. It may be.
- M represents sodium (Na), potassium (K), or ammonium (NH 4 ).
- alkyl diphenyl ether sulfonates or fluoroalkyl diphenyl ether sulfonates include, for example, PELEX (trade name, alkyl diphenyl ether disulfonate manufactured by Kao Corporation). Of these, PELEX® SS-H and PELEX® SS-L are preferable.
- the content of the tungsten anticorrosive agent (component (C)) in the liquid composition of the present invention is preferably in the range of 0.002 to 2% by mass, and preferably 0.004 to 1.0% by mass. More preferred is 0.01 to 0.4% by mass.
- the content of the component (C) in the liquid composition of the present invention is within the above range, sufficient tungsten anticorrosion performance can be obtained. If the concentration of the tungsten anticorrosive is less than 0.002% by weight, sufficient anticorrosion performance may not be obtained, and if it exceeds 2% by mass, it is not economical and is not suitable for practical use.
- the content of the component (C1) that is the tungsten anticorrosive agent in the liquid composition of the present invention is preferably in the range of 0.001 to 1% by mass, and preferably 0.002 to 0.5% by mass. More preferred is 0.005 to 0.2% by mass. If the content of the component (C1) in the liquid composition of the present invention is within the above range, sufficient tungsten anticorrosion performance can be obtained. If the concentration of the tungsten anticorrosive is less than 0.001% by weight, sufficient anticorrosion performance may not be obtained, and if it exceeds 1% by mass, it is not economical and is not suitable for practical use.
- the content of the component (C2) that is the tungsten anticorrosive in the liquid composition of the present invention is preferably in the range of 0.001 to 1% by mass, and preferably 0.001 to 0.5% by mass. More preferred is 0.005 to 0.2% by mass. If the content of the component (C2) in the liquid composition of the present invention is within the above range, sufficient tungsten anticorrosion performance can be obtained. If the concentration of the tungsten anticorrosive is less than 0.001% by weight, sufficient anticorrosion performance may not be obtained, and if it exceeds 1% by mass, it is not economical and is not suitable for practical use.
- the pH value of the liquid composition of the present invention is preferably 0 to 4, more preferably 0.5 to 3.5, and particularly preferably 1 to 3.
- the pH adjuster for adjusting the pH value (sometimes referred to as the component (D)) is not particularly limited as long as the pH can be adjusted.
- hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, perchloric acid Mineral and organic acids such as acetic acid, and inorganic and organic base compounds such as ammonia, potassium hydroxide, sodium hydroxide, tetramethylammonium hydroxide. These acid or base compounds may be used alone or in combination.
- nitric acid, sulfuric acid, phosphoric acid, acetic acid, ammonia, potassium hydroxide and tetramethylammonium hydroxide are particularly preferred.
- the content of the pH adjusting agent in the liquid composition of the present invention is appropriately determined depending on the contents of other components so that the pH of the liquid composition becomes a target value.
- the liquid composition of the present invention is usually used in the above-described (A) component, (B) component, (C) component, and a pH adjusting agent contained as required, as well as water and other cleaning liquid compositions.
- Various water-soluble organic solvents and additives to be used can be included as long as the effects of the liquid composition described above are not impaired.
- water from which metal ions, organic impurities, particle particles, and the like have been removed by distillation, ion exchange treatment, filter treatment, various adsorption treatments, and the like is preferable, pure water is more preferable, and ultrapure water is particularly preferable.
- the water-soluble organic solvent is not particularly limited as long as it does not inhibit the effect of the liquid composition described above.
- ethylene glycol such as diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, dipropylene glycol monomethyl ether, etc.
- Alcohols such as methanol, ethanol, 1-propanol, 2-propanol, 1-butanol and t-butanol; ethylene glycol, propylene glycol, glycerin and the like can be preferably used.
- a method of manufacturing a semiconductor device includes removing titanium nitride from a substrate including titanium nitride, tungsten, and a low dielectric constant interlayer insulating film without corroding tungsten and the low dielectric constant interlayer insulating film.
- the method includes a step of bringing the liquid composition into contact with a substrate including titanium nitride, tungsten, and a low dielectric constant interlayer insulating film.
- titanium nitride can be removed from a substrate including titanium nitride, tungsten, and a low dielectric constant interlayer insulating film without corroding tungsten and the low dielectric constant interlayer insulating film.
- the method for manufacturing a semiconductor device targets a substrate including titanium nitride, tungsten, and a low dielectric constant interlayer insulating film.
- the object to be cleaned is formed by laminating a tungsten wiring, a low dielectric constant interlayer insulating film, a titanium nitride hard mask, a photoresist on a substrate such as a silicon wafer, and then subjecting the photoresist to a selective exposure / development process.
- a pattern can be formed, and then, using this resist pattern as a mask, a titanium nitride hard mask and a low dielectric constant interlayer insulating film are subjected to a dry etching process, and the photoresist is removed.
- the method of bringing the liquid composition into contact with the object to be cleaned there is no particular limitation on the method of bringing the liquid composition into contact with the object to be cleaned.
- the method of bringing the liquid composition into contact with the object by dropping the liquid composition (single-leaf spin processing) or spraying, etc.
- a method of immersing in an object can be employed.
- any method can be used for cleaning.
- the use temperature of the liquid composition of the present invention is preferably from 10 to 70 ° C, particularly preferably from 20 to 60 ° C. If the temperature of a liquid composition is 10 degreeC or more, since the etching rate will become favorable, the outstanding production efficiency will be obtained. On the other hand, if it is 70 degrees C or less, a liquid composition change can be suppressed and etching conditions can be kept constant. Although the etching rate is increased by increasing the temperature of the liquid composition, an optimal processing temperature may be determined as appropriate in consideration of minimizing the composition change of the liquid composition.
- Titanium nitride removability, tungsten anticorrosive and low dielectric constant interlayer insulating film were evaluated by SEM observation.
- the cross sections of the substrates after the contact treatment of the liquid compositions obtained in the examples and comparative examples were measured using a scanning electron microscope (“SU9000 (model number)”; manufactured by Hitachi High-Tech Fielding Co., Ltd.) with an acceleration voltage of 2 kV and an emission current. Observed at 7 ⁇ A.
- Corrosion resistance E of the low dielectric constant interlayer insulating film 3 The low dielectric constant interlayer insulating film showed no change compared to before cleaning. G: The surface of the low dielectric constant interlayer insulating film was slightly recessed. P: Corrosion was observed in the low dielectric constant interlayer insulating film.
- Example 1 In a 10 L polypropylene container, 8.53 kg of pure water and 1.0 kg of 0.02 mol / L potassium permanganate solution (made by Wako Pure Chemical Industries, Ltd., special grade, molecular weight 158.03) as component (A) , 0.0375 kg of 40% by mass ammonium fluoride solution (Morita Chemical Co., Ltd., grade for semiconductor, molecular weight 37.04) as component (B), and Surflon S-241 (30% by mass product) as component (C1) (Trade name, perfluoroalkylamine oxide manufactured by AGC Seimi Chemical Co., Ltd.) 0.0033 kg, and phosphanol RS-710 (trade name, polyoxyethylene phosphate ester manufactured by Toho Chemical Co., Ltd.) as component (C2) 0.001 kg and as component (D) 47% by mass sulfuric acid (manufactured by Wako Pure Chemical Industries, Ltd., special grade, molecular weight 9) .08) 0.426kg was charged.
- a semiconductor element having a wiring structure having a cross section as shown in FIG. 1 is immersed at 50 ° C. for 5 minutes, and then rinsed with ultrapure water and dried nitrogen Drying was performed by injecting gas.
- the substrate including the titanium nitride and tungsten and the low dielectric constant interlayer insulating film after the cleaning treatment is broken, and the cross section of the substrate is observed with an SEM, thereby removing the titanium nitride hard mask 1, the tungsten wiring 2, and the low dielectric constant.
- the corrosion resistance of the interlayer insulating film 3 was evaluated, titanium nitride was completely removed, and corrosion of tungsten and corrosion of the low dielectric constant interlayer insulating film were not observed (Table 1).
- Examples 2 to 41 Cleaning treatment was performed in the same manner as in Example 1 except that liquid compositions having the blending amounts shown in Tables 1 to 7 were prepared. The evaluation results are shown in Tables 1-7. As a result of observing the cross section of the substrate after the cleaning process with SEM, the titanium nitride was completely removed from the substrate after the cleaning process with any liquid composition, and the corrosion of tungsten and the low dielectric constant interlayer insulating film was observed. Was not.
- Comparative Examples 1-10 Cleaning treatment was performed in the same manner as in Example 1 except that liquid compositions having the blending amounts shown in Tables 8 to 9 were prepared. The evaluation results are shown in Tables 8-9. As a result of observing the cross section of the substrate after the cleaning treatment with an SEM, there was no liquid composition satisfying all of the titanium nitride removability and the corrosion resistance of tungsten and the low dielectric constant interlayer insulating film.
- Comparative Example 11 According to the blending amounts shown in Table 10, ammonium iodate as the oxidizing agent, hexafluorosilicic acid as the etching agent, and 5-phenyl-1H-tetrazole and myristyltrimethylammonium bromide as the anticorrosive agent are blended. Washing treatment was performed in the same manner as described above. Table 10 shows the evaluation results. As a result of observing the cross section of the substrate after the cleaning treatment with an SEM, the removal of titanium nitride was insufficient.
- the liquid composition of the present invention can be suitably used for cleaning a substrate including titanium nitride, tungsten, and a low dielectric constant interlayer insulating film, and is excellent in titanium nitride without corroding tungsten and the low dielectric constant interlayer insulating film. Can be removed at a high speed, and high productivity can be achieved.
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Abstract
Description
即ち、本発明は以下のとおりである。
<1> 窒化チタン、タングステンおよび低誘電率層間絶縁膜を有する基板より、タングステンおよび低誘電率層間絶縁膜を腐食することなく、窒化チタンを除去し、
(A)過マンガン酸カリウム、ペルオキソ二硫酸アンモニウム、ペルオキソ二硫酸カリウム、およびペルオキソ二硫酸ナトリウムからなる群より選ばれる少なくとも一種である酸化剤、
(B)フッ素化合物、および
(C)タングステン防食剤を含み、
かつpH値が0~4である液体組成物であって、
前記(C)タングステン防食剤が、アルキルアミンおよびその塩、フルオロアルキルアミンおよびその塩、アルキルアミンオキシド、フルオロアルキルアミンオキシド、アルキルベタイン、フルオロアルキルベタイン、アルキル4級アンモニウムおよびその塩、フルオロアルキル4級アンモニウムおよびその塩、アルキル4級ピリジニウム塩、フルオロアルキル4級ピリジニウム塩、アルキル4級ビピリジニウム塩、フルオロアルキル4級ビピリジニウム塩、アルキル4級イミダゾリウム塩、およびフルオロアルキル4級イミダゾリウム塩からなるC1化合物群より選択される2種以上の異なる化合物を含むか、あるいは、
前記C1化合物群より選択される1種以上と、ポリオキシアルキレンアルキルアミン、ポリオキシアルキレンフルオロアルキルアミン、ポリオキシアルキレンアルキルエーテル、ポリオキシアルキレンフルオロアルキルエーテル、ポリオキシアルキレンアルキルリン酸エステル、ポリオキシアルキレンフルオロアルキルリン酸エステル、ポリオキシアルキレンアルキルエーテル硫酸塩、ポリオキシアルキレンフルオロアルキルエーテル硫酸塩、アルキルジフェニルエーテルスルホン酸塩、およびフルオロアルキルジフェニルエーテルスルホン酸塩からなるC2化合物群より選択される1種以上とを含み、
前記(A)酸化剤における過マンガン酸カリウムの濃度が0.001~0.1質量%であり、
前記(B)フッ素化合物の濃度が0.01~1質量%である、前記液体組成物である。
<2> 過酸化水素を含まない、上記<1>に記載の液体組成物である。
<3> 前記(B)フッ素化合物が、フッ酸、フッ化アンモニウム、酸性フッ化アンモニウム、フッ化テトラメチルアンモニウム、フッ化カリウム、ヘキサフルオロ珪酸、およびテトラフルオロ硼酸からなる群より選ばれる少なくとも一種である上記<1>に記載の液体組成物である。
<4> 前記C1化合物群におけるアルキルアミンまたはフルオロアルキルアミンが下記一般式(1)で表される上記<1>に記載の液体組成物である。
<5> 前記C1化合物群におけるアルキルアミン塩またはフルオロアルキルアミン塩が、塩酸塩、硝酸塩、酢酸塩、メタンスルホン酸塩、塩素酸塩、過塩素酸塩、フッ化水素酸塩、臭化水素酸塩、よう化水素酸塩、硫酸水素塩、硫酸塩、炭酸水素塩、炭酸塩、リン酸二水素塩、リン酸水素塩、およびリン酸塩からなる群より選ばれる少なくとも一種である上記<1>に記載の液体組成物である。
<6> 前記C1化合物群におけるアルキルアミンオキシドまたはフルオロアルキルアミンオキシドが、下記一般式(2)で表される上記<1>に記載の液体組成物である。
<7> 前記C1化合物群におけるアルキルベタインまたはフルオロアルキルベタインが、下記一般式(3)または(4)で表される上記<1>に記載の液体組成物である。
<8> 前記C1化合物群におけるアルキル4級アンモニウムおよびその塩またはフルオロアルキル4級アンモニウムおよびその塩が、下記一般式(5)、(6)または(7)で表される上記<1>に記載の液体組成物である。
<9> 前記C1化合物群におけるアルキル4級ピリジニウム塩またはフルオロアルキル4級ピリジニウム塩が、下記一般式(8)で表される上記<1>に記載の液体組成物である。
<10> 前記C1化合物群におけるアルキル4級ビピリジニウム塩またはフルオロアルキル4級ビピリジニウム塩が、下記一般式(9)で表される上記<1>に記載の液体組成物である。
<11> 前記C1化合物群におけるアルキル4級イミダゾリウム塩またはフルオロアルキル4級イミダゾリウム塩が、下記一般式(10)または(11)で表される上記<1>に記載の液体組成物である。
<12> 前記C2化合物群におけるポリオキシアルキレンアルキルアミンまたはポリオキシアルキレンフルオロアルキルアミンが、下記一般式(12)で表される上記<1>に記載の液体組成物である。
<13> 前記C2化合物群におけるポリオキシアルキレンアルキルエーテルまたはポリオキシアルキレンフルオロアルキルエーテルが、下記一般式(13)で表される上記<1>に記載の液体組成物。
<14> 前記C2化合物群におけるポリオキシアルキレンアルキルリン酸エステルまたはポリオキシアルキレンフルオロアルキルリン酸エステルが、下記一般式(14)または(15)で表される上記<1>に記載の液体組成物である。
<15> 前記C2化合物群におけるポリオキシアルキレンアルキルエーテル硫酸塩またはポリオキシアルキレンフルオロアルキルエーテル硫酸塩が、下記一般式(16)で表される上記<1>に記載の液体組成物である。
<16> 前記C2化合物群におけるアルキルジフェニルエーテルスルホン酸塩またはフルオロアルキルジフェニルエーテルスルホン酸塩が、下記一般式(17)で表される上記<1>に記載の液体組成物である。
<17> 前記(A)酸化剤におけるペルオキソ二硫酸アンモニウム、ペルオキソ二硫酸カリウム、またはペルオキソ二硫酸ナトリウムの濃度が0.1~20質量%である上記<1>に記載の液体組成物である。
<18> 前記(C)タングステン防食剤の濃度が0.002~2質量%である上記<1>に記載の液体組成物である。
<19> 前記C1化合物の濃度が0.001~1質量%で、前記C2化合物の濃度が0.001~1質量%である上記<1>に記載の液体組成物である。
<20> 上記<1>~<19>のいずれかに記載の液体組成物を用いる半導体素子の洗浄方法である。
<21> 窒化チタン、タングステンおよび低誘電率層間絶縁膜を有する基板より、タングステンおよび低誘電率層間絶縁膜を腐食することなく、窒化チタンを除去する半導体素子の製造方法であって、窒化チタン、タングステンおよび低誘電率層間絶縁膜を有する基板に、上記<1>~<19>のいずれかに記載の液体組成物を接触させることを含む、前記半導体素子の製造方法である。
<液体組成物>
本発明の液体組成物は、窒化チタンとタングステンおよび低誘電率層間絶縁膜を有する基板において、タングステンおよび低誘電率層間絶縁膜を腐食することなく窒化チタンを除去するために使用されるものであり、(A)酸化剤、(B)フッ素化合物、および(C)タングステン防食剤を含み、pH値が0~4の液体組成物である。
本発明の液体組成物に含まれる酸化剤(以下、単に(A)成分ということがある)は、窒化チタンの酸化剤として機能するものである。本発明の液体組成物は、過酸化水素を含まないことが特徴の一つである。本発明の液体組成物は過酸化水素を含まないため、タングステンを腐食するという問題がない。酸化剤としては、過マンガン酸カリウム、ペルオキソ二硫酸アンモニウム、ペルオキソ二硫酸カリウム、及びペルオキソ二硫酸ナトリウムが好ましく挙げられる。これらの酸化剤は、単独で使用してもよく、また複数を組み合わせて使用してもよい。
本発明の液体組成物に含まれるフッ素化合物(以下、単に(B)成分ということがある)は、窒化チタンのエッチング機能を有する。フッ素化合物としては、フッ素原子を有する化合物より選択されるものである。フッ素化合物としては、例えば、フッ酸、フッ化アンモニウム、酸性フッ化アンモニウム、フッ化テトラメチルアンモニウム、フッ化カリウム、ヘキサフルオロ珪酸、ヘキサフルオロ珪酸アンモニウム、テトラフルオロ硼酸、テトラフルオロ硼酸アンモニウムといったフッ素化合物が好ましく挙げられる。これらのフッ素化合物は単独で使用してもよく、また複数を組み合わせて使用してもよい。これらのなかでもフッ酸、フッ化アンモニウム、酸性フッ化アンモニウム、フッ化テトラメチルアンモニウム、およびフッ化カリウムがより好ましい。特にフッ酸、フッ化アンモニウムおよび酸性フッ化アンモニウムが好ましい。
本発明の液体組成物に含まれるタングステン防食剤(以下、単に(C)成分ということがある。)は、C1化合物群より選択される2種以上の異なる化合物を含むか、あるいは、C1化合物群より選択される1種以上と、C2化合物群より選択される1種以上とを含み、それらによりタングステンの防食機能を有する。
本発明の液体組成物のpH値は0~4が好ましく、0.5~3.5がより好ましく、特に1~3が好ましい。
pH値を調整するためのpH調整剤((D)成分と呼ぶことがある)は、pHを調整出来るものであれば特に制限はなく、例えば、塩酸、硝酸、硫酸、リン酸、過塩素酸、酢酸などの鉱酸および有機酸類、アンモニア、水酸化カリウム、水酸化ナトリウム、水酸化テトラメチルアンモニウムなどの無機および有機塩基化合物が挙げられる。これらの酸または塩基化合物は単独で使用してもよく、また複数を組み合わせて使用してもよい。これらのなかでも、硝酸、硫酸、リン酸、酢酸、アンモニア、水酸化カリウムおよび水酸化テトラメチルアンモニウムが特に好ましい。
本発明の液体組成物中のpH調整剤の含有量は、液体組成物のpHが目的の値となるように、他の成分の含有量によって適宜決定されるものである。
本発明による半導体素子の製造方法は、窒化チタンとタングステンおよび低誘電率層間絶縁膜を含む基板より、タングステンおよび低誘電率層間絶縁膜を腐食することなく、窒化チタンを除去する半導体素子の製造方法であって、窒化チタンとタングステンおよび低誘電率層間絶縁膜を含む基板に上記の液体組成物を接触させる工程を含むものである。本発明の方法によれば、窒化チタンとタングステンおよび低誘電率層間絶縁膜を含む基板より、タングステンおよび低誘電率層間絶縁膜を腐食することなく、窒化チタンを除去することができる。
本発明の液体組成物の使用温度としては、10~70℃の温度が好ましく、特に20~60℃が好ましい。液体組成物の温度が10℃以上であれば、エッチング速度が良好となるため優れた生産効率が得られる。一方、70℃以下であれば、液組成変化を抑制し、エッチング条件を一定に保つことができる。液体組成物の温度を高くすることで、エッチング速度は上昇するが、液体組成物の組成変化を小さく抑えることなども考慮した上で、適宜最適な処理温度を決定すればよい。
合格はそれぞれEとGである。
判定;
I.窒化チタンハードマスク1の除去性
E:窒化チタンハードマスクが完全に除去された。
G:窒化チタンハードマスクがほとんど除去された。
P:窒化チタンハードマスクが除去されなかった。
II.タングステン配線2の防食性
E:タングステン配線が洗浄前と比較して変化が見られなかった。
G:タングステン配線の表面に少し荒れがみられた。
P:タングステン配線に腐食が観察された。
III.低誘電率層間絶縁膜3の防食性
E:低誘電率層間絶縁膜が洗浄前と比較して変化が見られなかった。
G:低誘電率層間絶縁膜の表面がわずかにくぼんでいた。
P:低誘電率層間絶縁膜に腐食が観察された。
容量10Lのポリプロピレン容器に、純水8.53kgと、(A)成分として0.02mol/L過マンガン酸カリウム溶液(和光純薬工業株式会社製、特級、分子量158.03)を1.0kgと、(B)成分として40質量%フッ化アンモニウム溶液(森田化学工業株式会社製、半導体用グレード、分子量37.04)を0.0375kgと、(C1)成分としてサーフロン S-241(30質量%品、商品名、AGCセイミケミカル株式会社製パーフルオロアルキルアミンオキシド)0.0033kgと、(C2)成分としてフォスファノール RS-710(商品名、東邦化学工業株式会社製のポリエキシエチレンリン酸エステル)0.001kgと、(D)成分として、47質量%硫酸(和光純薬工業株式会社製、特級、分子量98.08)0.426kgを投入した。攪拌して各成分の溶解を確認し、液体組成物を調製した。得られた液体組成物のpH値は1.4であった(表1)。
表1~7に示した配合量の液体組成物を調合した以外は、実施例1と同様にして洗浄処理を行った。評価結果を表1~7に示す。洗浄処理後の基板断面をSEMにて観察した結果、いずれの液体組成物による洗浄処理後の基板に関しても、窒化チタンは完全に除去されており、タングステンおよび低誘電率層間絶縁膜の腐食は観察されなかった。
表8~9に示した配合量の液体組成物を調合した以外は、実施例1と同様にして洗浄処理を行った。評価結果を表8~9に示す。洗浄処理後の基板断面をSEMにて観察した結果、窒化チタンの除去性、タングステンおよび低誘電率層間絶縁膜の防食性の全てを満たす液体組成物はなかった。
表10に示した配合量の通り、酸化剤としてよう素酸アンモニウム、エッチング剤としてヘキサフルオロ珪酸、防食剤として5-フェニル-1H-テトラゾールとミリスチルトリメチルアンモニウムブロミドを配合し、それ以外は実施例1と同様にして洗浄処理を行った。評価結果を表10に示す。洗浄処理後の基板断面をSEMにて観察した結果、窒化チタンの除去性が不十分であった。
2.低誘電率層間絶縁膜
3.タングステン
Claims (21)
- 窒化チタン、タングステンおよび低誘電率層間絶縁膜を有する基板より、タングステンおよび低誘電率層間絶縁膜を腐食することなく、窒化チタンを除去し、
(A)過マンガン酸カリウム、ペルオキソ二硫酸アンモニウム、ペルオキソ二硫酸カリウム、およびペルオキソ二硫酸ナトリウムからなる群より選ばれる少なくとも一種である酸化剤、
(B)フッ素化合物、および
(C)タングステン防食剤を含み、
かつpH値が0~4である液体組成物であって、
前記(C)タングステン防食剤が、アルキルアミンおよびその塩、フルオロアルキルアミンおよびその塩、アルキルアミンオキシド、フルオロアルキルアミンオキシド、アルキルベタイン、フルオロアルキルベタイン、アルキル4級アンモニウムおよびその塩、フルオロアルキル4級アンモニウムおよびその塩、アルキル4級ピリジニウム塩、フルオロアルキル4級ピリジニウム塩、アルキル4級ビピリジニウム塩、フルオロアルキル4級ビピリジニウム塩、アルキル4級イミダゾリウム塩、およびフルオロアルキル4級イミダゾリウム塩からなるC1化合物群より選択される2種以上の異なる化合物を含むか、あるいは、
前記C1化合物群より選択される1種以上と、ポリオキシアルキレンアルキルアミン、ポリオキシアルキレンフルオロアルキルアミン、ポリオキシアルキレンアルキルエーテル、ポリオキシアルキレンフルオロアルキルエーテル、ポリオキシアルキレンアルキルリン酸エステル、ポリオキシアルキレンフルオロアルキルリン酸エステル、ポリオキシアルキレンアルキルエーテル硫酸塩、ポリオキシアルキレンフルオロアルキルエーテル硫酸塩、アルキルジフェニルエーテルスルホン酸塩、およびフルオロアルキルジフェニルエーテルスルホン酸塩からなるC2化合物群より選択される1種以上とを含み、
前記(A)酸化剤における過マンガン酸カリウムの濃度が0.001~0.1質量%であり、
前記(B)フッ素化合物の濃度が0.01~1質量%である、前記液体組成物。 - 過酸化水素を含まない、請求項1に記載の液体組成物。
- 前記(B)フッ素化合物が、フッ酸、フッ化アンモニウム、酸性フッ化アンモニウム、フッ化テトラメチルアンモニウム、フッ化カリウム、ヘキサフルオロ珪酸、およびテトラフルオロ硼酸からなる群より選ばれる少なくとも一種である請求項1に記載の液体組成物。
- 前記C1化合物群におけるアルキルアミン塩またはフルオロアルキルアミン塩が、塩酸塩、硝酸塩、酢酸塩、メタンスルホン酸塩、塩素酸塩、過塩素酸塩、フッ化水素酸塩、臭化水素酸塩、よう化水素酸塩、硫酸水素塩、硫酸塩、炭酸水素塩、炭酸塩、リン酸二水素塩、リン酸水素塩、およびリン酸塩からなる群より選ばれる少なくとも一種である請求項1に記載の液体組成物。
- 前記C1化合物群におけるアルキルベタインまたはフルオロアルキルベタインが、下記一般式(3)または(4)で表される請求項1に記載の液体組成物。
- 前記C1化合物群におけるアルキル4級アンモニウムおよびその塩またはフルオロアルキル4級アンモニウムおよびその塩が、下記一般式(5)、(6)または(7)で表される請求項1に記載の液体組成物。
- 前記C1化合物群におけるアルキル4級イミダゾリウム塩またはフルオロアルキル4級イミダゾリウム塩が、下記一般式(10)または(11)で表される請求項1に記載の液体組成物。
- 前記C2化合物群におけるポリオキシアルキレンアルキルリン酸エステルまたはポリオキシアルキレンフルオロアルキルリン酸エステルが、下記一般式(14)または(15)で表される請求項1に記載の液体組成物。
- 前記(A)酸化剤におけるペルオキソ二硫酸アンモニウム、ペルオキソ二硫酸カリウム、またはペルオキソ二硫酸ナトリウムの濃度が0.1~20質量%である請求項1に記載の液体組成物。
- 前記(C)タングステン防食剤の濃度が0.002~2質量%である請求項1に記載の液体組成物。
- 前記C1化合物の濃度が0.001~1質量%で、前記C2化合物の濃度が0.001~1質量%である請求項1に記載の液体組成物。
- 請求項1~19のいずれかに記載の液体組成物を用いる半導体素子の洗浄方法。
- 窒化チタン、タングステンおよび低誘電率層間絶縁膜を有する基板より、タングステンおよび低誘電率層間絶縁膜を腐食することなく、窒化チタンを除去する半導体素子の製造方法であって、窒化チタン、タングステンおよび低誘電率層間絶縁膜を有する基板に、請求項1~19のいずれか一項に記載の液体組成物を接触させることを含む、前記半導体素子の製造方法。
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