WO2004042811A1 - 洗浄液及びそれを用いた洗浄方法 - Google Patents
洗浄液及びそれを用いた洗浄方法 Download PDFInfo
- Publication number
- WO2004042811A1 WO2004042811A1 PCT/JP2003/014183 JP0314183W WO2004042811A1 WO 2004042811 A1 WO2004042811 A1 WO 2004042811A1 JP 0314183 W JP0314183 W JP 0314183W WO 2004042811 A1 WO2004042811 A1 WO 2004042811A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- cleaning
- acid
- salt
- present
- sodium
- Prior art date
Links
- 238000004140 cleaning Methods 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000000203 mixture Substances 0.000 title description 16
- 239000000758 substrate Substances 0.000 claims abstract description 55
- 229910052751 metal Inorganic materials 0.000 claims abstract description 40
- 239000002184 metal Substances 0.000 claims abstract description 40
- 239000004065 semiconductor Substances 0.000 claims abstract description 36
- 239000002738 chelating agent Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 150000003839 salts Chemical class 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 150000001875 compounds Chemical class 0.000 claims abstract description 23
- 239000003513 alkali Substances 0.000 claims abstract description 14
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 14
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical group OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 125000002947 alkylene group Chemical group 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 58
- 239000002253 acid Substances 0.000 claims description 18
- 239000000872 buffer Substances 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 10
- 229910052744 lithium Inorganic materials 0.000 claims description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound 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 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229940120146 EDTMP Drugs 0.000 claims description 7
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 claims description 7
- BPSYZMLXRKCSJY-UHFFFAOYSA-N 1,3,2-dioxaphosphepan-2-ium 2-oxide Chemical compound O=[P+]1OCCCCO1 BPSYZMLXRKCSJY-UHFFFAOYSA-N 0.000 claims description 6
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 4
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 claims description 3
- 229940090960 diethylenetriamine pentamethylene phosphonic acid Drugs 0.000 claims description 3
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 claims description 3
- DUYCTCQXNHFCSJ-UHFFFAOYSA-N dtpmp Chemical compound OP(=O)(O)CN(CP(O)(O)=O)CCN(CP(O)(=O)O)CCN(CP(O)(O)=O)CP(O)(O)=O DUYCTCQXNHFCSJ-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 239000006173 Good's buffer Substances 0.000 claims description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- ADLJEHFHJBJGOX-UHFFFAOYSA-N n'-[2-(2-aminoethylamino)ethyl]ethane-1,2-diamine;azane Chemical compound N.NCCNCCNCCN ADLJEHFHJBJGOX-UHFFFAOYSA-N 0.000 claims description 2
- UXVMRCQQPJIQGC-UHFFFAOYSA-N n,n,n',n'-tetrakis(ethenyl)ethane-1,2-diamine Chemical group C=CN(C=C)CCN(C=C)C=C UXVMRCQQPJIQGC-UHFFFAOYSA-N 0.000 claims description 2
- GGHDAUPFEBTORZ-UHFFFAOYSA-N propane-1,1-diamine Chemical compound CCC(N)N GGHDAUPFEBTORZ-UHFFFAOYSA-N 0.000 claims 4
- OXMASCYDRYZZKC-UHFFFAOYSA-N O=P1OCCCCCCO1 Chemical compound O=P1OCCCCCCO1 OXMASCYDRYZZKC-UHFFFAOYSA-N 0.000 claims 2
- JKTORXLUQLQJCM-UHFFFAOYSA-N 4-phosphonobutylphosphonic acid Chemical compound OP(O)(=O)CCCCP(O)(O)=O JKTORXLUQLQJCM-UHFFFAOYSA-N 0.000 claims 1
- KQDHKMRXNDZKGT-UHFFFAOYSA-N P(O)(O)=O.C=C.C=C.C=C.C=C Chemical compound P(O)(O)=O.C=C.C=C.C=C.C=C KQDHKMRXNDZKGT-UHFFFAOYSA-N 0.000 claims 1
- WDWQXVJKSPAKMT-UHFFFAOYSA-N P1(OCO1)=O.N Chemical compound P1(OCO1)=O.N WDWQXVJKSPAKMT-UHFFFAOYSA-N 0.000 claims 1
- VEDPSYHRYWKAAE-UHFFFAOYSA-N [K].NCCNCCNCCN Chemical compound [K].NCCNCCNCCN VEDPSYHRYWKAAE-UHFFFAOYSA-N 0.000 claims 1
- ZDRPGXANPTXAAP-UHFFFAOYSA-N [Na].C=C.C=C.C=C Chemical compound [Na].C=C.C=C.C=C ZDRPGXANPTXAAP-UHFFFAOYSA-N 0.000 claims 1
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims 1
- 150000008041 alkali metal carbonates Chemical class 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- PWRMVXOVJDQTON-UHFFFAOYSA-N azane;propane Chemical compound N.CCC PWRMVXOVJDQTON-UHFFFAOYSA-N 0.000 claims 1
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims 1
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims 1
- 125000000547 substituted alkyl group Chemical group 0.000 claims 1
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 27
- 238000005498 polishing Methods 0.000 abstract description 16
- 239000003795 chemical substances by application Substances 0.000 abstract description 14
- 238000005530 etching Methods 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 11
- 150000002739 metals Chemical class 0.000 abstract description 9
- 238000007788 roughening Methods 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 19
- 239000010949 copper Substances 0.000 description 19
- 229910052710 silicon Inorganic materials 0.000 description 19
- 239000010703 silicon Substances 0.000 description 19
- 235000012431 wafers Nutrition 0.000 description 19
- -1 methylmethylene group Chemical group 0.000 description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000011575 calcium Substances 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 229910021642 ultra pure water Inorganic materials 0.000 description 6
- 239000012498 ultrapure water Substances 0.000 description 6
- 239000010419 fine particle Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 2
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 2
- 239000006172 buffering agent Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000009499 grossing Methods 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- HQRPHMAXFVUBJX-UHFFFAOYSA-M lithium;hydrogen carbonate Chemical compound [Li+].OC([O-])=O HQRPHMAXFVUBJX-UHFFFAOYSA-M 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
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- 238000005507 spraying Methods 0.000 description 2
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- WNKKRLJRXMEVSB-UHFFFAOYSA-N 1-(cyclohexylamino)ethanesulfonic acid Chemical compound OS(=O)(=O)C(C)NC1CCCCC1 WNKKRLJRXMEVSB-UHFFFAOYSA-N 0.000 description 1
- PVOAHINGSUIXLS-UHFFFAOYSA-N 1-Methylpiperazine Chemical compound CN1CCNCC1 PVOAHINGSUIXLS-UHFFFAOYSA-N 0.000 description 1
- INEWUCPYEUEQTN-UHFFFAOYSA-N 3-(cyclohexylamino)-2-hydroxy-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(O)CNC1CCCCC1 INEWUCPYEUEQTN-UHFFFAOYSA-N 0.000 description 1
- ORUKAMXGCAIPEY-UHFFFAOYSA-N 3-amino-1-cyclohexylpropane-1-sulfonic acid Chemical compound NCCC(S(O)(=O)=O)C1CCCCC1 ORUKAMXGCAIPEY-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- WYLNFICFIJTWIH-UHFFFAOYSA-N C=C.[Li] Chemical group C=C.[Li] WYLNFICFIJTWIH-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- PJWWRFATQTVXHA-UHFFFAOYSA-N Cyclohexylaminopropanesulfonic acid Chemical compound OS(=O)(=O)CCCNC1CCCCC1 PJWWRFATQTVXHA-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- 101000806511 Homo sapiens Protein DEPP1 Proteins 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- FSVCELGFZIQNCK-UHFFFAOYSA-N N,N-bis(2-hydroxyethyl)glycine Chemical compound OCCN(CCO)CC(O)=O FSVCELGFZIQNCK-UHFFFAOYSA-N 0.000 description 1
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- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
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- NQOBKHLJLHTKGM-UHFFFAOYSA-N P(O)(O)=O.C=C.C=C.C=C.C=C.C=C Chemical compound P(O)(O)=O.C=C.C=C.C=C.C=C.C=C NQOBKHLJLHTKGM-UHFFFAOYSA-N 0.000 description 1
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- 102100037469 Protein DEPP1 Human genes 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
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- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
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- STIAPHVBRDNOAJ-UHFFFAOYSA-N carbamimidoylazanium;carbonate Chemical compound NC(N)=N.NC(N)=N.OC(O)=O STIAPHVBRDNOAJ-UHFFFAOYSA-N 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- 229960005141 piperazine Drugs 0.000 description 1
- 229960003506 piperazine hexahydrate Drugs 0.000 description 1
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- 238000012805 post-processing Methods 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- SVPHCAKUHIFNAV-UHFFFAOYSA-N potassium;propane-1,1-diamine Chemical compound [K].CCC(N)N SVPHCAKUHIFNAV-UHFFFAOYSA-N 0.000 description 1
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- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 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
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
- H01L21/02052—Wet cleaning only
-
- 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
-
- 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
- H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
-
- C11D2111/22—
Definitions
- the present invention relates to a cleaning liquid for a semiconductor substrate which may have metal wiring and has been subjected to a polishing treatment, an etching treatment, a CMP treatment and the like, and a method for cleaning the semiconductor substrate using the same.
- a silicon wafer surface serving as a substrate is repeatedly subjected to a smoothing process, an etching process for providing various layers on the substrate, a process for smoothing the surface after lamination, and the like. Be done.
- fine particles such as polishing particles, impurities derived from various metals, and foreign substances derived from slurry adhere to the surface of the semiconductor substrate. It is known that if the production of a semiconductor is continued while these impurities remain, the possibility that the finally obtained semiconductor becomes inappropriate becomes high.
- the liquid properties (pH) of the cleaning liquid used in this cleaning step are preferably the same as those of the various processing liquids used in the preceding step.
- an alkaline cleaning solution is preferably used after the step of using an alkaline polishing agent or an alkaline etching solution.
- conventional cleaning liquids for example, Japanese Patent Application Laid-Open No. 5-275405, International Publication No. 01Z0717989 pamphlet, Japanese Patent Application Laid-Open No. 10-072054, Japanese Patent Application Laid-Open No.
- the present invention has been made by focusing on the problems existing in the prior art as described above.
- the purpose is that even if used after a process using an alkaline polishing agent or an alkaline etching solution, particles on the substrate surface become gelled and difficult to remove, and the semiconductor substrate surface becomes rough.
- An object of the present invention is to provide an alkaline cleaning solution capable of efficiently removing fine particles (particles) and impurities derived from various metals on the surface of a semiconductor substrate without causing problems such as easy generation. Disclosure of the invention
- the present invention has the following configurations.
- a semiconductor which contains a chelating agent represented by the following general formula (1) or a salt thereof, an alkali compound and pure water, and has a pH of 8 to 13 and may be provided with metal wiring. Cleaning solution for substrates.
- a method for cleaning a semiconductor substrate which comprises cleaning the semiconductor substrate on which metal wiring may be provided, using the cleaning liquid of (1).
- the cleaning composition used in the cleaning step contains a chelating agent represented by the following general formula (1) or a salt thereof, an alkaline compound, and pure water.
- Y 1 and ⁇ 2 represent a lower alkylene group
- ⁇ represents an integer of 0 to 4
- at least 4 of R 1 to R 4 and n R 5 have an alkyl group having a phosphonic acid group. And the remainder represents an alkyl group.
- the lower alkylene group is preferably a linear or branched one having 1 to 4 carbon atoms, and specific examples include a methylene group, an ethylene group, a propylene group, a methylmethylene group, a methylethylene group, an ethylmethylene group, and a butylene. Group, methylpropylene group, ethylethylene group and the like.
- alkyl group of the alkyl group which may have a phosphonic acid group a linear or branched one having 1 to 4 carbon atoms is preferable. Specific examples include a methyl group, an ethyl group, and an n-propyl group. , Isopropyl, n-butyl, isobutyl, sec-butyl, tert-butyl and the like.
- the number of phosphonic acid groups which may be possessed by these alkyl groups is usually 1 to 2, and preferably 1.
- the chelating agent represented by the above general formula (1) or a salt thereof adheres to and remains on the semiconductor substrate which has been subjected to polishing treatment, etching treatment, CMP treatment, and may have metal wiring. Included to capture and remove metal impurities.
- the metal impurities include transition metals such as iron (Fe), nickel (Ni), and copper; and aluminum salts such as calcium (Ca) and magnesium (Mg). Examples thereof include those derived from lithium earth metals, such as these metals themselves, their hydroxides, and their oxides.
- the chelating agent represented by the general formula (1) or a salt thereof removes metal impurities by forming stable complex ions with these metals.
- Examples of the salt of the chelating agent include lithium metal salts, sodium salts, alkali metal salts such as potassium salts, and ammonium salts.
- Specific examples of the chelating agent or its salt include ethylenediaminetetraethylenephosphonic acid, ethylenediaminetetraethylenephosphonate ammonium, ethylenediaminetetraethylenephosphonate potassium, ethylenediaminetetraethylenephosphonate sodium, ethylenediaminetetraethylenephosphonate, ethylenediaminetetraethylene.
- chelating agents or salts thereof those in which all of R 1 to R 4 and n R 5 in the formula of the above general formula (1) are alkyl groups having a phosphonic acid group are considered as metal impurities. It is preferable because of its high ability to form a complex.
- n in the formula (1) is preferably an integer of 0 to 2 because it can be easily manufactured.
- EDT P0 ethylenediaminetetramethylenephosphonic acid
- EDT P0 ethylenediaminetetramethylenephosphonic acid
- Ethylenediaminetetramethylenephosphonic acid ammonium ethylenediaminetetramethylenephosphonic acid potassium
- Sodium ethylenediaminetetramethylenephosphonate Lithium ethylenediaminetetramethylenephosphonate
- DEPP 0 Diethylenetriaminepentaethylenephosphonic acid
- TETHP Triethylenetetramine hexaethylenephosphonic acid
- PDTMP Propanediaminetetraethylenephosphonic acid
- the lower limit of the content of the chelating agent or a salt thereof in the cleaning composition is preferably at least 0.001% by weight, more preferably at least 0.05% by weight, and most preferably at most 0.01% by weight.
- the upper limit is preferably 20% by weight or less, more preferably 15% by weight or less, and most preferably 10% by weight or less.
- Alkali compounds are used to reduce fluctuations in liquid properties during cleaning when performing post-processing such as polishing, etching, and CMP, which are performed using various alkaline chemicals.
- the liquid property has a lower limit of preferably pH 8 or more, more preferably, in order to facilitate the handling of the composition.
- the upper limit is preferably pH 3 or less, more preferably 12 or less, and most preferably 11 or less.
- the polishing composition or the like remaining on the surface gels, making it difficult to clean or adjusting the particle potential to a negative value. It is used to effectively suppress the phenomenon that particles such as particles are re-adsorbed to the surface of the silicon layer. It is also used to promote the dissociation of chelating agents and to promote complex formation reactions with impurity metals.
- alkali metal compound used for such a purpose examples include an alkali metal hydroxide (eg, potassium hydroxide, sodium hydroxide, lithium hydroxide, etc.), and a carbonate of an alkali metal (eg, hydrogen carbonate).
- an alkali metal hydroxide eg, potassium hydroxide, sodium hydroxide, lithium hydroxide, etc.
- a carbonate of an alkali metal eg, hydrogen carbonate.
- alkaline metal hydroxides which are relatively commonly used as alkaline polishing agents, etching agents, CMP agents and the like, are particularly preferred.
- the use of abrasives, etching agents, CMP agents, etc., which are used in the pre-cleaning process, are widely used as polishing agents, generate insoluble fine particles, etc. due to fluctuations in alkali components. It is possible to suppress the damage, avoid the damage to the substrate surface, and increase the cleaning effect.
- the content of the alkaline compound in the cleaning solution varies depending on the type, but the lower limit is usually 0.1% by weight or more, more preferably 0.5% by weight or more, and most preferably 1% by weight or more.
- an appropriate buffer may be added to the washing solution of the present invention in order to keep the pH within the above range.
- a buffer include boric acid and a biochemical buffer.
- the good buffer examples include N, N-bis (2-hydroxysethyl) glycine (Bicine), and N-cyclohexyl-3-aminopropanesulfonic acid (CAP S), N-cyclohexyl-2-hydroxy-3-amino-propanesulfonic acid (CAPS ⁇ ), N-cyclohexyl-1-aminoaminosulfonic acid (CHES), and more preferably N-cyclohexyl-1-aminoaminosulfonic acid (CHES) Preferred are cyclohexyl-3-aminopropanesulfonic acid (CAPS), N-cyclohexyl-1-aminoethanesulfonic acid (CHES) and the like.
- CAP S N, N-bis (2-hydroxysethyl) glycine
- CAP S N-cyclohexyl-3-aminopropanesulfonic acid
- CAS ⁇ N-cyclohexyl-2-hydroxy-3-a
- the concentration of the buffer in the washing solution of the present invention has a lower limit of usually 0.01% by weight or more, preferably 0.05% by weight or more, and more preferably 0.1% by weight or more.
- the upper limit is usually 10% by weight or less, preferably 5% by weight or less, more preferably 2.0% by weight or less. Pure water is contained for dissolving each component of the chelating agent or a salt thereof and an alkali compound, and if necessary, a buffer.
- the water contains as little impurities as possible to prevent the action of other components from being hindered.
- pure water, ultrapure water, distilled water, or the like in which foreign matter is removed through a filter after removing impurity ions with an ion exchange resin is preferable.
- the cleaning liquid of the present invention is supplied as a solution containing each component at the above-described concentrations. Although this solution may be used for washing as it is, it is usually desirable to dilute it appropriately in consideration of the washing cost and washing effect.
- the washing liquid of the present invention is prepared by dissolving the above-described chelating agent according to the present invention or a salt thereof and an alkali compound, and if necessary, components of a buffer in water.
- any method capable of finally preparing a solution containing these components can be used. There is no particular limitation.
- a method in which a chelating agent or a salt thereof and an alkaline compound according to the present invention and, if necessary, a buffer are directly added to water, followed by stirring and dissolving;
- the chelating agent or its salt and the alkali compound according to the present invention in which the chelating agent or its salt and an alkaline compound according to the present invention and, if necessary, a buffer are separately dissolved in water.
- a method of mixing with a salt-containing solution, (5) the present invention A chelating agent or a salt thereof and an alkaline compound are directly added to water, and the mixture is stirred and dissolved, and the solution containing a chelating agent or a salt thereof and an alkali compound according to the present invention is separately dissolved in water. And a method of mixing the obtained solution with the buffer-containing solution according to the present invention.
- the thus-prepared washing solution of the present invention is preferably subjected to a filtration treatment or the like before use.
- the cleaning method using the cleaning liquid of the present invention may be any method as long as the cleaning liquid of the present invention can come into contact with the surface of the semiconductor substrate. Spraying method (single wafer processing) and the like.
- the cleaning with the cleaning solution of the present invention may be used in combination with a physical cleaning method such as brush scrub or megasonic.
- a physical cleaning method such as brush scrub or megasonic.
- a method of applying the cleaning solution of the present invention to the substrate surface to make the cleaning solution present on the substrate surface and then performing physical cleaning, Immersed in the cleaning solution of the present invention After that, a method of performing physical cleaning after removing the substrate from the cleaning solution to make the cleaning solution exist on the substrate surface, a method of performing physical cleaning while the substrate is immersed in the cleaning solution of the present invention, A method of performing physical cleaning after sprinkling the cleaning solution of the present invention on the surface of the substrate by sprinkling the cleaning solution of the present invention on the surface of the substrate, or a method of performing physical cleaning while spraying the cleaning solution of the present invention on the substrate surface is used.
- Examples of the semiconductor substrate that can be cleaned with the cleaning liquid of the present invention and that may have metal wiring on its surface include so-called silicon wafers, glass substrates for LCDs and PDPs, and compound semiconductors such as GaAs and GaAs. Substrates, printed wiring boards, and the like.
- the cleaning liquid of the present invention is used for silicon wafers, for 100 and? It is useful for glass substrates for P, compound semiconductor substrates such as GaAs and GaAs, and particularly useful for compound semiconductors such as silicon wafers, GaAs, and GaAs.
- the cleaning liquid of the present invention includes a substrate having a metal wiring such as copper, silver, aluminum, tungsten plug, chromium, or gold provided on the surface thereof, among which copper or silver wiring is provided. This is useful for substrates with copper wiring, especially those with copper wiring on the surface, and most useful for semiconductor substrates with copper wiring.
- the cleaning liquid of the present invention exhibits an effective cleaning effect even at room temperature, but since the cleaning efficiency is higher at higher temperatures, it may be used after being heated appropriately. When heating, it is used usually at 30 to 80 ° C, preferably at 35 to 70 ° C, more preferably at 40 to 6 ° C.
- the cleaning solution of the present invention contains various auxiliary components (for example, a surfactant, a preservative, and an organic solvent) as long as the effects of the present invention are not impaired, in addition to the above components. Even if it is included, it does not matter at all. It is not desirable to add hydrogen peroxide to the cleaning solution of the present invention. In other words, when a semiconductor substrate provided with metal wiring is cleaned using a substance containing hydrogen peroxide, the surface of the metal wiring is oxidized, and the possibility of causing a disconnection due to an increase in resistance or corrosion increases. The versatility of the cleaning solution of the present invention is impaired. Therefore, it is desirable not to add hydrogen peroxide to the cleaning solution of the present invention.
- auxiliary components for example, a surfactant, a preservative, and an organic solvent
- the lower limit of the concentration used is usually 0.01% by weight or more, preferably 0.05% by weight or more, more preferably 0.
- the upper limit is usually 5.0% by weight or less, preferably 2.0% by weight or less, more preferably 1.0% by weight or less. According to the embodiment described in detail above, the following effects are exhibited.
- the chelating agent or its salt contained in the cleaning composition is more likely to form stable complex ions with metal impurities derived from transition metals and the like than conventional chelating agents such as EDTA. High ability to wash and remove. Therefore, when cleaning the surface of a semiconductor substrate which may have metal wiring on the surface, the amount of metal impurities adhering to the surface can be reduced.
- the surface of the semiconductor substrate exhibits a negative potential at a short time. Is repelled electrostatically, and the re-adhesion of metal impurities and abrasive grains to the substrate surface can be suppressed. For this reason, contamination of the semiconductor substrate due to impurities derived from transition metals such as Cu, Fe and Ni and alkaline earth metals such as Ca and Mg can be suppressed.
- the cleaning liquid of the present invention is adjusted to be alkaline, it can be adjusted to the same liquid properties as the alkaline polishing composition, the etching composition, and the CMP composition. Problems such as gelling of abrasive components and substrate surface roughness can be minimized, and a high cleaning effect can be obtained.
- the present invention will be described in more detail with reference to Examples and Comparative Examples, but the present invention is not limited thereto.
- the concentration of the impurity metal adsorbed and remaining on the silicon wafer surface was determined by recovering the impurity metal on the silicon wafer surface with a dilute HF solution and using a lead furnace atomic absorption spectrometry. (Hereinafter, it is abbreviated as dilute HF recovery one atomic absorption method)
- dilute HF recovery one atomic absorption method ultrapure water was used as the water used for liquid preparation and analysis, and ultrahigh purity reagent was used for HF.
- EDTPO Ethylenediaminetetramethylenephosphonic acid
- TETHP Triethylenetetramine hexaethylenephosphonic acid
- PDTMP Propandiamine tetraethylene phosphonic acid
- DT PA diethylenetriaminepentaacetic acid
- TMAH hydroxyl
- Colloidal silica having a particle size of 100 nm or less and Fe, Cu, and A of 100 p ⁇ b as metal impurities so as to be 15% by weight in an aqueous potassium hydroxide solution.
- a nitrate of Ca was added to prepare an alkaline polishing composition. After polishing the surface of a 6-inch, P-type (100) silicon wafer with the contaminated polishing composition, the surface was rinsed with ultrapure water. After drying with a spin drier, the residual amount of the impurity metal adsorbed on the silicon wafer surface was measured by dilute HF recovery atomic absorption spectrometry.
- Example 1 A silicon wafer contaminated with Fe, Cu, A1, and Ca, prepared in the same manner as that used in Example 1, was treated with the compositions shown in Nos. 10 to 14 in Table 1. The solution was washed by immersing it in a solution diluted to 10 to 100 times by adding pure water and in pure water of No. 15 at 25 for 5 minutes. Then Example 1 The processing was performed in the same manner as described above. The results are shown in Table 1 (
- Example 2 When the silicon wafer contaminated with FeCuA1 and Ca prepared in the same manner as that used in Example 1 was subjected to brush scrubbing using a polyvinyl alcohol brush, No. 23 to No. 25 were added to the cleaning solution of pure water and diluted with 10 to 100 times diluted solution and ultrapure water (No. 26) and sprayed. After treating in the same manner as in Example 2, the amount of impurity metal remaining on the surface of the silicon wafer was measured in the same manner as in Example 1. The results are shown in Table 2.
- No. 33 No. 35 in Table 3 was prepared by replacing the chelating agent of the present invention with EDTA and DTPA, and this was diluted with pure water to a dilution of 10 to 100 times.
- the Cu plating film was immersed in the solution prepared as described above at 25 ° C. for 30 minutes, and the amount of corrosion-dissolved Cu ions was measured by the I-8 method. The results are shown in Table 3.
- the treating agent of the present invention has a smaller amount of dissolved Cu than the treating agent using EDTA or DTPA which is a conventional chelating agent, and the Cu wiring It was found that there was little damage to.
- Industrial potential EDTA or DTPA which is a conventional chelating agent
- the particles on the substrate surface are gelled and removed even after being used after the step using an alkaline polishing agent or an alkaline etching solution. It is possible to efficiently remove impurities derived from fine particles (fine particles) and various metals on the surface of the semiconductor substrate without causing problems such as difficulty in making the surface of the semiconductor substrate rough and the like. This has the effect.
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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US10/534,351 US7700532B2 (en) | 2002-11-08 | 2003-11-07 | Cleaning composition and method of cleaning therewith |
AU2003277597A AU2003277597A1 (en) | 2002-11-08 | 2003-11-07 | Cleaning composition and method of cleaning therewith |
JP2004549630A JP4752270B2 (ja) | 2002-11-08 | 2003-11-07 | 洗浄液及びそれを用いた洗浄方法 |
EP03810641A EP1562225A4 (en) | 2002-11-08 | 2003-11-07 | CLEANING COMPOSITION AND METHOD FOR CLEANING WITH THE COMPOSITION |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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JP2002324853 | 2002-11-08 | ||
JP2002-324853 | 2002-11-08 |
Publications (1)
Publication Number | Publication Date |
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WO2004042811A1 true WO2004042811A1 (ja) | 2004-05-21 |
Family
ID=32310455
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2003/014183 WO2004042811A1 (ja) | 2002-11-08 | 2003-11-07 | 洗浄液及びそれを用いた洗浄方法 |
Country Status (8)
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---|---|
US (1) | US7700532B2 (ja) |
EP (1) | EP1562225A4 (ja) |
JP (1) | JP4752270B2 (ja) |
KR (1) | KR100974034B1 (ja) |
CN (1) | CN100437922C (ja) |
AU (1) | AU2003277597A1 (ja) |
TW (1) | TW200418977A (ja) |
WO (1) | WO2004042811A1 (ja) |
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- 2003-11-07 WO PCT/JP2003/014183 patent/WO2004042811A1/ja active Application Filing
- 2003-11-07 JP JP2004549630A patent/JP4752270B2/ja not_active Expired - Fee Related
- 2003-11-07 EP EP03810641A patent/EP1562225A4/en not_active Withdrawn
- 2003-11-07 KR KR1020057008168A patent/KR100974034B1/ko not_active IP Right Cessation
- 2003-11-07 US US10/534,351 patent/US7700532B2/en not_active Expired - Fee Related
- 2003-11-07 AU AU2003277597A patent/AU2003277597A1/en not_active Abandoned
- 2003-11-10 TW TW092131362A patent/TW200418977A/zh not_active IP Right Cessation
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Cited By (16)
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JP2006179593A (ja) * | 2004-12-21 | 2006-07-06 | Sumco Corp | 半導体ウェーハの洗浄乾燥方法 |
JP2007016110A (ja) * | 2005-07-06 | 2007-01-25 | Adeka Corp | 化学機械的研磨用洗浄剤組成物および該洗浄剤組成物を用いる洗浄方法 |
JP2009543896A (ja) * | 2006-07-14 | 2009-12-10 | イーコラブ インコーポレイティド | アルカリ性床洗浄組成物及び床洗浄方法 |
CN102575201B (zh) * | 2009-09-11 | 2014-07-09 | 东友Fine-Chem股份有限公司 | 用于制造平面显示器的基板的清洗液组合物 |
WO2011031092A3 (ko) * | 2009-09-11 | 2011-08-04 | 동우 화인켐 주식회사 | 평판표시장치 제조용 기판의 세정액 조성물 |
CN102575201A (zh) * | 2009-09-11 | 2012-07-11 | 东友Fine-Chem股份有限公司 | 用于制造平面显示器的基板的清洗液组合物 |
US9334470B2 (en) | 2011-12-06 | 2016-05-10 | Kanto Kagaku Kabushiki Kaisha | Cleaning liquid composition for electronic device |
EP2602309A1 (en) | 2011-12-06 | 2013-06-12 | Kanto Kagaku Kabushiki Kaisha | Cleaning alkaline liquid composition for electronic device comprising a phosphonic acid derivative chelating agent |
WO2013162020A1 (ja) | 2012-04-27 | 2013-10-31 | 和光純薬工業株式会社 | 半導体基板用洗浄剤および半導体基板表面の処理方法 |
KR20150003217A (ko) | 2012-04-27 | 2015-01-08 | 와코 쥰야꾸 고교 가부시키가이샤 | 반도체 기판용 세정제 및 반도체 기판 표면의 처리방법 |
US9803161B2 (en) | 2012-04-27 | 2017-10-31 | Wako Pure Chemical Industries, Ltd. | Cleaning agent for semiconductor substrates and method for processing semiconductor substrate surface |
WO2014171355A1 (ja) | 2013-04-19 | 2014-10-23 | 関東化学株式会社 | 洗浄液組成物 |
JP2015189829A (ja) * | 2014-03-27 | 2015-11-02 | 株式会社フジミインコーポレーテッド | 研磨用組成物 |
JP2015189828A (ja) * | 2014-03-27 | 2015-11-02 | 株式会社フジミインコーポレーテッド | 研磨用組成物 |
CN112143573A (zh) * | 2020-09-29 | 2020-12-29 | 常州时创能源股份有限公司 | 硅片碱抛后清洗用添加剂及其应用 |
CN112143573B (zh) * | 2020-09-29 | 2021-07-06 | 常州时创能源股份有限公司 | 硅片碱抛后清洗用添加剂及其应用 |
Also Published As
Publication number | Publication date |
---|---|
CN100437922C (zh) | 2008-11-26 |
JP4752270B2 (ja) | 2011-08-17 |
KR100974034B1 (ko) | 2010-08-04 |
KR20050074556A (ko) | 2005-07-18 |
TWI330662B (ja) | 2010-09-21 |
CN1711627A (zh) | 2005-12-21 |
EP1562225A1 (en) | 2005-08-10 |
US20060154838A1 (en) | 2006-07-13 |
JPWO2004042811A1 (ja) | 2006-03-09 |
US7700532B2 (en) | 2010-04-20 |
TW200418977A (en) | 2004-10-01 |
AU2003277597A1 (en) | 2004-06-07 |
EP1562225A4 (en) | 2007-04-18 |
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