WO2018154775A1 - Liquide de gravure et son utilisation - Google Patents
Liquide de gravure et son utilisation Download PDFInfo
- Publication number
- WO2018154775A1 WO2018154775A1 PCT/JP2017/007466 JP2017007466W WO2018154775A1 WO 2018154775 A1 WO2018154775 A1 WO 2018154775A1 JP 2017007466 W JP2017007466 W JP 2017007466W WO 2018154775 A1 WO2018154775 A1 WO 2018154775A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- copper
- etching
- hydrogen
- transparent conductive
- conductive film
- Prior art date
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- 238000005530 etching Methods 0.000 title claims abstract description 145
- 239000007788 liquid Substances 0.000 title abstract description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 115
- 229910052802 copper Inorganic materials 0.000 claims abstract description 115
- 239000010949 copper Substances 0.000 claims abstract description 115
- 238000004090 dissolution Methods 0.000 claims abstract description 33
- 239000003085 diluting agent Substances 0.000 claims abstract description 29
- 239000003112 inhibitor Substances 0.000 claims abstract description 29
- 239000007800 oxidant agent Substances 0.000 claims abstract description 25
- 229910001507 metal halide Inorganic materials 0.000 claims abstract description 23
- 150000005309 metal halides Chemical class 0.000 claims abstract description 23
- 229910000039 hydrogen halide Inorganic materials 0.000 claims abstract description 22
- 239000012433 hydrogen halide Substances 0.000 claims abstract description 22
- 150000003839 salts Chemical class 0.000 claims abstract description 10
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000001590 oxidative effect Effects 0.000 claims abstract description 7
- 239000004020 conductor Substances 0.000 claims description 66
- 238000000034 method Methods 0.000 claims description 35
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- 239000003960 organic solvent Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 claims description 14
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 14
- 235000011007 phosphoric acid Nutrition 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 11
- -1 alkaline earth metal chlorates Chemical class 0.000 claims description 11
- 150000003016 phosphoric acids Chemical class 0.000 claims description 11
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 9
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 8
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 8
- 150000001451 organic peroxides Chemical class 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 229910052783 alkali metal Inorganic materials 0.000 claims description 7
- 150000001340 alkali metals Chemical class 0.000 claims description 7
- 150000004820 halides Chemical class 0.000 claims description 7
- 229910000042 hydrogen bromide Inorganic materials 0.000 claims description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 7
- 229910000043 hydrogen iodide Inorganic materials 0.000 claims description 7
- 150000002823 nitrates Chemical class 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 150000002826 nitrites Chemical class 0.000 claims description 7
- 230000000737 periodic effect Effects 0.000 claims description 7
- 239000000243 solution Substances 0.000 description 70
- 230000000052 comparative effect Effects 0.000 description 17
- 239000007864 aqueous solution Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 15
- WTDHULULXKLSOZ-UHFFFAOYSA-N hydroxylamine hydrochloride Substances Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 description 14
- 239000012452 mother liquor Substances 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 238000007654 immersion Methods 0.000 description 7
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000001110 calcium chloride Substances 0.000 description 6
- 229910001628 calcium chloride Inorganic materials 0.000 description 6
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 229910052736 halogen Inorganic materials 0.000 description 5
- 239000005020 polyethylene terephthalate Substances 0.000 description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 150000002367 halogens Chemical class 0.000 description 4
- WCYJQVALWQMJGE-UHFFFAOYSA-M hydroxylammonium chloride Chemical compound [Cl-].O[NH3+] WCYJQVALWQMJGE-UHFFFAOYSA-M 0.000 description 4
- 239000004973 liquid crystal related substance Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- JFDZBHWFFUWGJE-UHFFFAOYSA-N benzonitrile Chemical compound N#CC1=CC=CC=C1 JFDZBHWFFUWGJE-UHFFFAOYSA-N 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 description 2
- YVBCULSIZWMTFY-UHFFFAOYSA-N 4-Heptanol Natural products CCCC(O)CCC YVBCULSIZWMTFY-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 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 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 150000004683 dihydrates Chemical class 0.000 description 2
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910003437 indium oxide Inorganic materials 0.000 description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 235000013772 propylene glycol Nutrition 0.000 description 2
- 230000007261 regionalization Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- COWKRCCNQSQUGJ-UHFFFAOYSA-N 1,1,2,2,3-pentafluoropropan-1-ol Chemical compound OC(F)(F)C(F)(F)CF COWKRCCNQSQUGJ-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- 239000005968 1-Decanol Substances 0.000 description 1
- JOLQKTGDSGKSKJ-UHFFFAOYSA-N 1-ethoxypropan-2-ol Chemical compound CCOCC(C)O JOLQKTGDSGKSKJ-UHFFFAOYSA-N 0.000 description 1
- NBUKAOOFKZFCGD-UHFFFAOYSA-N 2,2,3,3-tetrafluoropropan-1-ol Chemical compound OCC(F)(F)C(F)F NBUKAOOFKZFCGD-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 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
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229920012266 Poly(ether sulfone) PES Polymers 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
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- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 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
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 1
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 1
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- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- YALMXYPQBUJUME-UHFFFAOYSA-L calcium chlorate Chemical compound [Ca+2].[O-]Cl(=O)=O.[O-]Cl(=O)=O YALMXYPQBUJUME-UHFFFAOYSA-L 0.000 description 1
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- 238000009713 electroplating Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
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- 238000000605 extraction Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- CRJZNQFRBUFHTE-UHFFFAOYSA-N hydroxylammonium nitrate Chemical compound O[NH3+].[O-][N+]([O-])=O CRJZNQFRBUFHTE-UHFFFAOYSA-N 0.000 description 1
- VGYYSIDKAKXZEE-UHFFFAOYSA-L hydroxylammonium sulfate Chemical compound O[NH3+].O[NH3+].[O-]S([O-])(=O)=O VGYYSIDKAKXZEE-UHFFFAOYSA-L 0.000 description 1
- 229910000378 hydroxylammonium sulfate Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
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- 150000002576 ketones Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- ZWRUINPWMLAQRD-UHFFFAOYSA-N n-Nonyl alcohol Natural products CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- FVSKHRXBFJPNKK-UHFFFAOYSA-N propionitrile Chemical compound CCC#N FVSKHRXBFJPNKK-UHFFFAOYSA-N 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 150000004072 triols Chemical class 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Images
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
- H01L21/04—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
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
Definitions
- the present invention relates to a technique for etching a transparent conductive film containing indium oxide used in a liquid crystal display or the like, and more particularly to an etching solution used for etching a transparent conductive film having a pattern made of a copper conductor on the surface and use thereof.
- Transparent conductive films including ITO (indium-tin oxide) films are widely used in the field of electronic devices such as antistatic films, heat reflective films, transparent electrodes of photoelectric conversion elements and various flat panel displays. Recently, with the spread of portable information terminals, notebook PCs, small TVs, etc., the demand for liquid crystal displays (LCDs) has increased.
- ITO indium-tin oxide
- the etching solution (Patent Document 2) already completed by the present applicant is composed of a halogen acid, a halogen metal salt, an oxidizing agent, and a remaining diluted solution, and the corrosion amount of the copper conductor in the currently used etching solution for the ITO film.
- a halogen acid a halogen acid
- a halogen metal salt a halogen metal salt
- an oxidizing agent a remaining diluted solution
- the corrosion amount of the copper conductor in the currently used etching solution for the ITO film There are few drugs. However, even when etching is performed using this etching solution, dissolution of the copper conductor cannot be ignored, and damage to the high-definition copper circuit pattern is inevitable.
- Patent Document 3 Patent Document 4
- the manufacturing process of the transparent electrode pattern is efficient.
- the resistance value of the feeder circuit increases because the etching of the copper conductor in the upper layer of the ITO film proceeds excessively.
- Patent Document 5 Although a method of using different etching solutions for the etching of the copper film and the etching of the transparent conductor layer has been proposed (Patent Document 5), no detailed examination has been made on the composition of each etching solution here. It cannot be said that it has reached the practical level.
- JP2015-60937A Japanese Patent No. 4897148 JP 2011-114194 A JP2013-89731A JP 2014-52737 A JP 2017-10996 A JP 2002-241968 A
- the present invention has been made in view of the above points, and the problem thereof is to selectively use an ITO circuit while maintaining a high etching rate for a crystalline transparent conductive film and without corroding a conductor containing copper as a main component. It is to realize the technique of etching.
- Another object of the present invention is to provide a transparent conductive film etching method capable of etching only an ITO conductor while suppressing dissolution of a copper conductor.
- a further object of the present invention is to obtain an etching solution with little change with time.
- the present inventors were able to selectively dissolve the transparent conductive film without corroding the conductor mainly composed of copper, and the change with time was suppressed.
- a new high performance etchant has been completed. That is, the present invention is as follows.
- the (a) hydrogen halide comprises at least one selected from hydrogen chloride, hydrogen bromide, and hydrogen iodide
- the metal halide (b) is composed of one or more selected from halides of Group 1, 2, and 13 elements of the periodic table
- the (c) copper dissolution inhibitor comprises one or more selected from hydroxylamine and a salt thereof
- the (d) diluent is composed of water and / or an organic solvent, and may optionally contain phosphoric acids
- the (e) oxidizing agent comprises one or more selected from alkali metal and / or alkaline earth metal chlorates, nitrates or nitrites, perchloric acid, nitric acid, hydrogen peroxide, organic peroxides, Used for etching a transparent conductive film having a conductor pattern
- a transparent conductive film having a conductor pattern mainly composed of copper on its surface containing (a) hydrogen halide, (b) metal halide, (c) copper dissolution inhibitor, (d) diluent, and optionally ( e) A method for etching a transparent conductive film having a conductive pattern mainly composed of copper on the surface, the method comprising a step of contacting an etchant that may contain an oxidizing agent,
- the (a) hydrogen halide comprises at least one selected from hydrogen chloride, hydrogen bromide, and hydrogen iodide
- the metal halide (b) is composed of one or more selected from halides of Group 1, 2, and 13 elements of the periodic table
- the (c) copper dissolution inhibitor comprises one or more selected from hydroxylamine and a salt thereof
- the (d) diluent is composed of water and / or an organic solvent, and may optionally contain phosphoric acids
- the (e) oxidizing agent comprises one or more selected from alkali metal and
- Step 1 A step of forming a transparent conductive film on the substrate,
- Step 2 A step of forming a conductor film containing copper as a main component on the transparent conductive film,
- Step 3 A step of etching the conductor film containing copper as a main component to form a conductor pattern containing copper as a main component on the transparent conductive film,
- Step 4 A transparent conductive film having a conductor pattern mainly composed of copper obtained in Step 3 on its surface is obtained by (a) hydrogen halide, (b) metal halide, (c) copper dissolution inhibitor, ( d) a step of forming a transparent electrode pattern by etching a transparent conductive film by contacting with an etchant containing a diluent and optionally (e) an oxidizing agent;
- a method for forming a transparent electrode pattern having a copper-based conductor pattern on the surface In step 4 above,
- the (a) hydrogen halide comprises at least one selected from hydrogen chloride,
- a copper dissolution inhibitor is newly added to an etching solution in which the main component comprising the components (a) and (b) and the optional component (d) are dissolved in the diluent (d).
- the transparent conductive film can be etched precisely corresponding to the resist pattern without corroding the copper conductor pattern adjacent thereto. Using such an etching method, the copper conductor and the transparent electrode can be patterned with higher definition.
- the transparent conductive film which has the conductor pattern which has copper as a main component on the surface just before an etching is represented typically.
- the transparent electrode which uses the etching liquid of this invention and which has the conductor pattern which has copper as a main component on the surface is represented typically.
- the resist pattern has already been removed.
- the transparent electrode which uses the etching liquid for a comparison which does not contain a copper dissolution inhibitor and which has the conductor pattern which has copper as a main component on the surface is represented typically.
- the resist pattern has already been removed.
- the etching solution of the present invention contains (a) hydrogen halide, (b) metal halide, (c) copper dissolution inhibitor, (d) diluent, and may optionally contain (e) an oxidizing agent.
- the hydrogen halide is composed of one or more selected from hydrogen chloride, hydrogen bromide, and hydrogen iodide. Of these, hydrogen chloride (hydrochloric acid) is preferred.
- hydrogen chloride hydrogen chloride (hydrochloric acid) is preferred.
- Such (a) hydrogen halide is used in the form dissolved in (d) diluent, preferably in the form of an aqueous solution.
- concentration of (a) hydrogen halide in the etching solution of the present invention is appropriately adjusted according to the desired etching rate, but is generally 0.1 mol% to 7 mol%, preferably 1.0 mol%. It is in the range of ⁇ 5.0 mol%.
- the metal halide is composed of one or more selected from halides of Group 1, 2 and 13 elements of the periodic table.
- metal halide is generally one or more selected from chloride, bromide and iodide of sodium, potassium, magnesium, calcium and aluminum, and the element period in that the etching rate can be increased.
- Chlorides of Group 2 elements (alkaline earth metals) in the table are preferred, and calcium chloride is particularly preferred.
- Calcium chloride and other metal halides can be used in combination.
- a readily available hydrate can be used as calcium chloride.
- metal halide is used in the form dissolved in (d) diluent, preferably in the form of an aqueous solution.
- the concentration of the (b) metal halide in the etching solution of the present invention is appropriately adjusted according to the desired etching rate, but is generally 0.01 mol% to 6 mol%, preferably 0.1 mol%. It is in the range of ⁇ 5.0 mol%.
- the copper dissolution inhibitor is composed of one or more selected from hydroxylamine and a salt thereof.
- Such (c) copper dissolution inhibitor is used in the form dissolved in (d) diluent, preferably in the form of an aqueous solution. If the density
- hydroxylammonium chloride When using hydroxylammonium chloride as a copper dissolution inhibitor, generally a 20% by weight aqueous solution of hydroxylammonium chloride is prepared on a weight basis, and (a) hydrogen halide, (b) halogenated. 1 ml or more of the above aqueous solution is added per liter of the mother liquor of the etching solution which may contain metal, (d) diluent, and (e) oxidant, and preferably 1 ml to 20 ml in consideration of cost.
- the (d) diluent is composed of water and / or an organic solvent, and may optionally contain phosphoric acids.
- This (d) diluent functions as a solvent for the (a) hydrogen halide, (b) metal halide, and (c) copper dissolution inhibitor contained in the etching solution of the present invention. It also functions as a solvent for the optional component (e) oxidizing agent.
- ion-exchanged water or distilled water is usually used.
- the organic solvent used as a diluent is not limited as long as it is an organic solvent that can dissolve the constituents of the etching solution of the present invention, exhibits a relatively low electrical conductivity, and does not affect the etching process. Can be used.
- organic solvents examples include methanol, ethanol, isopropanol, 1-propanol, 1-butanol, 2-butanol, t-butanol, 2-methyl-1-propanol, 1-pentanol, 1-hexanol, 1 Alcohols such as heptanol, 4-heptanol, 1-octanol, 1-nonyl alcohol, 1-decanol, 1-dodecanol; diols such as ethylene glycol, 1,2-propanediol, propylene glycol, butanediol, glycerin or the like Triols; Ketones such as acetone, acetylacetone, and methyl ethyl ketone; Nitriles such as acetonitrile, propionitrile, butyronitrile, isobutyronitrile, and benzonitrile; Acetaldehyde, propionaldehyde Which aldehydes; lower alkylene
- the diluent (d) of the present invention may be the above-mentioned water or the above-mentioned organic solvent, or may be a mixture of the above-mentioned water and the organic solvent in any quantitative ratio. .
- Phosphoric acids can also be dissolved in the diluent.
- the phosphoric acids used here include any of phosphoric acid, phosphorous acid, and hypophosphorous acid.
- the ionization equilibrium of the aqueous solution constituting the etching solution of the present invention can be adjusted by adding one or more of these phosphoric acids to the diluent.
- These phosphoric acids are supplementary at appropriate concentrations depending on the characteristics of the material to be etched, such as the transparent electrode film to which the etching solution of the present invention is applied, the substrate in contact with the film, and the metal species including copper in the conductor. Can be blended.
- a diluent (d) of the present invention typically, water and / or alcohol is used.
- the (e) oxidizing agent increases the etching rate of the etching solution of the present invention and reduces corrosion of the device material by (a) hydrogen halide and (b) metal halide contained in the etching solution of the present invention. Therefore, it is a component used as necessary.
- Such (e) oxidizing agent is at least one selected from alkali metal and / or alkaline earth metal chlorates, nitrates or nitrites, perchloric acid, nitric acid, hydrogen peroxide, and organic peroxides.
- an oxidizing agent When an oxidizing agent is used, its addition amount is not limited as long as it does not exceed the saturation amount, but is preferably 0.01 mol% or more, more preferably 0.01 mol% to 2.0 mol%.
- the halogen concentration per liter of the etching solution of the present invention is 1 mol to the saturation amount, and 10 wt% to 90 wt% of the total halogen amount contained in the etching solution is the above (b) halogenated It is preferably supplied from metal.
- the transparent conductive film having the copper-based conductor pattern on the surface is used to dissolve the copper conductor. It can be etched without causing it.
- the “conductor mainly composed of copper” in the present invention is not limited to the case where the conductor is composed of a single copper, but the conductor is composed of a single copper layer and a composite oxide or alloy layer containing copper. This includes cases where
- a transparent conductive film having a conductor pattern mainly composed of copper on the surface is typically a film in which a circuit pattern composed of a conductor mainly composed of copper is formed on an ITO (indium-tin oxide) film. is there. Such a circuit pattern is formed in an electrode area connected to the display area. Therefore, a typical example of the transparent conductive film having a conductor pattern mainly composed of copper on the surface thereof in the present invention is a portion having a so-called extraction electrode.
- a resist pattern corresponding to the pattern of the transparent electrode is formed on this film when the transparent conductive film having a conductor pattern mainly composed of copper on the surface and the etching solution of the present invention are brought into contact with each other.
- the etching method of the present invention a portion of the transparent conductive film not covered with the resist pattern is etched to form a transparent electrode pattern. Since the etching solution of the present invention does not dissolve copper, in this etching method, only the transparent conductive film is etched while the copper pattern already formed on the transparent conductive film is well preserved. As a result, a high-definition copper pattern and transparent electrode pattern are formed.
- the method of contact between the etching solution of the present invention and the transparent conductive film having a conductor pattern mainly composed of copper on the surface is in accordance with a conventional method of etching treatment.
- the etching solution of the present invention heated to 30 ° C. to 70 ° C. is brought into contact with a transparent conductive film having a conductor pattern mainly composed of copper on the surface by dipping or spraying at this temperature.
- the immersion time in the immersion method, the amount of spray liquid in the spray method, and the like are appropriately set in consideration of the etching rate. At this time, by etching while blowing a gaseous oxidant such as oxygen, chlorine, nitrogen oxide, ozone, etc., corrosion of the device material can be reduced and the life of the device can be extended.
- a gaseous oxidant such as oxygen, chlorine, nitrogen oxide, ozone, etc.
- a transparent electrode pattern can be formed by a method including the following steps using the etching method of the present invention.
- Step 1 This is a step of forming a transparent conductive film on the substrate according to a conventional method.
- a substrate made of glass, quartz, polyethylene terephthalate (PET), polyethersulfone (PES) or the like used for an LCD (liquid crystal display) or a touch panel is used.
- a glass substrate or a PET substrate is used.
- the transparent conductive film include films made of ITO (indium tin oxide), indium oxide, tin oxide, and zinc oxide.
- an ITO film is preferable, and a crystalline ITO film is particularly preferable.
- a method for forming a transparent conductive film on a substrate sputtering, film deposition, vacuum deposition using ion assist, CVD (chemical vapor deposition), coating, spin coating, or spraying may be used. it can.
- the thickness of the transparent conductive film is selected according to the thickness according to the target device, but is generally in the range of 100 to 5000 mm.
- Step 2 A step of forming a conductor film containing copper as a main component on the transparent conductive film according to a conventional method.
- a method for forming a conductor film containing copper as a main component there are methods such as sputtering, CVD, and electroplating. Generally, sputtering is used.
- Step 3 the conductor film mainly composed of copper is etched to form a conductor pattern mainly composed of copper on the transparent conductive film.
- a resist material is applied on a conductor film containing copper as a main component, and a photomask having a pattern drawn on the surface of the resist material is formed.
- the resist material is irradiated with energy rays such as electromagnetic waves and electron beams through a photomask. The resist material is developed to form a resist pattern.
- the etching solution used in step 3 is an etching solution that does not corrode the transparent conductive film.
- an acidic etchant such as a persulfuric acid-based or hydrogen peroxide-based etchant can be used. After selectively etching the copper, the film is washed.
- Step 4 the transparent conductive film having a conductor pattern mainly composed of copper obtained in step 3 on the surface is etched using the etching solution of the present invention.
- step 4 a resist material is applied on the transparent conductive film having a conductor pattern mainly composed of copper obtained in step 3 on its surface, and a photomask having a pattern drawn on the surface of the resist material is formed.
- the resist material is irradiated with energy rays such as electromagnetic waves and electron beams through the photomask. The resist material is developed to form a resist pattern.
- the transparent conductive film thus obtained is brought into contact with the etching solution of the present invention as described above, and the conductor pattern already formed on the transparent conductive film is well preserved and is not protected with a resist.
- the transparent conductive film portion is selectively etched. After selectively etching the ITO film, the film is washed.
- an ITO film having a copper conductive pattern on the surface is etched in two ways: an etching solution of the present invention and (c) a comparative etching solution not containing a copper dissolution inhibitor. The pattern formation of each of the conductor made of copper and the ITO electrode was compared.
- dihydrate is used as the calcium chloride shown in Table 1, and the concentration indicates the calcium chloride concentration in the mother liquor.
- Dihydrate is used as the calcium nitrate shown in Table 1, and the concentration indicates the concentration of calcium nitrate in the mother liquor.
- Step 1 An ITO film having a thickness of 1500 mm was formed on a PET substrate having a thickness of 0.25 mm by sputtering.
- Step 2 A copper film having a thickness of 1 ⁇ m was formed on the obtained ITO film by sputtering.
- Step 3 A resist material was applied on the copper film, and the resist material was exposed and developed through a photomask. Thus, a resist pattern was formed on the copper film.
- the copper film was etched using a commercially available acid etching solution. Thus, a conductor pattern made of copper was formed on the ITO film.
- Step 4 A resist material was applied to the ITO film on which the conductor pattern made of copper was formed, and the resist material was exposed and developed through a photomask. Thus, a copper conductive pattern and a resist pattern on the ITO film were formed.
- the resist pattern was formed with a resist line width of approximately 40 ⁇ m and a resist line interval of approximately 20 ⁇ m.
- the ITO film having the conductor pattern made of copper thus obtained was immersed in the etching solution of the present invention prepared as follows and a comparative etching solution.
- an ITO film having a thickness of 1500 mm was provided on a PET substrate having a thickness of 0.25 mm by sputtering, and this film was used as a standard film for determining the immersion time.
- the standard film was previously immersed in each etching solution shown in Table 1, and the time from the start of immersion until the dissolution of the ITO film was completed was defined as the standard time (T).
- T standard time
- the completion of dissolution of the ITO film was confirmed by the fact that the surface resistance value of the standard film measured with a tester showed infinite. It shows that the etching rate of each etching liquid is so large that T is small.
- An ITO film having a conductor pattern made of copper was immersed in each of the etching solutions shown in Table 1 over a time corresponding to T ⁇ 1.5. During immersion, the temperature of each etching solution was maintained at 30 ° C.
- Etching was performed in such a sufficient time. After the immersion, the ITO film having a conductor pattern made of copper was washed and dried. Thus, an ITO electrode pattern was formed using an etching method using the etching solution of the present invention and the comparative etching solution.
- FIG. 1 schematically shows an ITO film having a conductor pattern made of copper on the surface immediately before etching in step 4.
- the resist line spacing (S1) immediately before etching was measured at four different points, and the average value (S1av) of the four values (S11, S12, S13, S14) was obtained.
- the resist line width (L1) immediately before etching was measured at four different points, and an average value (L1av) of four values (L11, L12, L13, L14) was obtained.
- FIG. 2 schematically shows an ITO electrode pattern having a conductor pattern made of copper on the surface, formed using the etching solution of the present invention (Examples 1 to 6).
- FIG. 3 schematically shows an ITO pattern having a conductive pattern made of copper on the surface, formed using a comparative etching solution (Comparative Example 1).
- the ITO pattern line width after etching (S2) was measured, and the average value (S2av) of the four values (S21, S22, S23, S24) was determined.
- the ITO pattern line width (L2) after etching was measured, and the average value (L2av) of the four values (L21, L22, L23, L24) was determined.
- Table 1 shows values of ⁇ S corresponding to Examples 1, 2, 3, 4, and Comparative Example 1.
- a smaller ⁇ S absolute value means that the resist pattern line spacing is more faithfully reproduced in the ITO electrode pattern line spacing because corrosion of the copper conductor pattern on the ITO film is suppressed.
- Table 1 shows values of ⁇ L corresponding to Examples 1, 2, 3, 4 and Comparative Example 1. It means that the smaller the absolute value of ⁇ L, the more faithfully the resist pattern line width is reproduced in the ITO electrode pattern line width by suppressing the corrosion of the copper conductor pattern on the ITO film.
- the resist pattern is accurately reproduced as an ITO electrode pattern.
- Such a selective etching effect of the etching solution of the present invention is stable until at least 5 hours have passed since the etching solution was prepared.
- the etching rate does not decrease compared to the case of Comparative Example 1 in which (c) the copper dissolution inhibitor is not used.
- Example 7 Example 8, Comparative Example 2
- An etching solution was manufactured under the conditions shown in Table 1. In Examples 8 and 9, etching was performed 24 hours after the addition of 20% by weight aqueous solution of (c) hydroxyammonium hydrochloride. In Comparative Example 2, the mother liquor 24 hours after preparation was used for etching.
- Etching was performed under the same conditions as in Example 1 using the etching solutions of Example 8 and Comparative Example 2, and evaluated.
- the contact method of the etching solution was changed from immersion to spraying, and other conditions were the same as in Example 1, and the ITO film was etched and evaluated. The results are shown in Table 2.
- the selective etching effect of the etching solution of the present invention is maintained even after 24 hours from the preparation of the etching solution or even when the contact method between the etching solution and the ITO film is changed.
- Example 9 is an example in which (c) a 20% by weight aqueous solution of hydroxyammonium hydrochloride was added in portions to the etching solution.
- 2 ml of (c) 20% by weight aqueous solution of hydroxyammonium hydrochloride was added to 1 L of the mother liquor shown in Table 1, and 24 hours later, the same amount of (c) A weight percent aqueous solution was added.
- the ITO film was etched and evaluated under the same conditions as in Example 1 using the etchant at the time when 72 hours had passed since the first addition of (c) hydroxyammonium hydrochloride. The results are shown in Table 3.
- Example 10 is also an example in which (c) a 20% by weight aqueous solution of hydroxyammonium hydrochloride was dividedly added to the etching solution.
- (c) a 20% by weight aqueous solution of hydroxyammonium hydrochloride was dividedly added to the etching solution.
- 2 ml of (c) 20% by weight aqueous solution of hydroxyammonium hydrochloride was added to 1 L of the mother liquor shown in Table 1, 24 hours and 48 hours later, again with the same amount of (c) as above.
- a 20 wt% aqueous solution of hydroxyammonium hydrochloride was added.
- the ITO film was etched and evaluated under the same conditions as in Example 1 using the etchant at the time when 72 hours had passed since the first addition of (c) hydroxyammonium hydrochloride. The results are shown in Table 3.
- Examples 11 and 12 are examples in which (e) the oxidizing agent was not added.
- the etching solution of the present invention was prepared by adding 2 ml of (c) 20% by weight aqueous solution of hydroxyammonium hydrochloride to 1 L of the mother liquor shown in Table 4, and the ITO film was etched and evaluated under the same conditions as in Example 1. The results are shown in Table 4.
- the etching solution of the present invention is epoch-making in that it has both an etching rate and selectivity for an ITO film and has little deterioration with time.
- a transparent electrode pattern having a copper wiring can be efficiently produced with high accuracy.
- the present invention can contribute to the manufacture of liquid crystal displays and touch panels that are thinner and require high-definition image display.
- Substrate 2 ITO film 3
- Copper conductive pattern 4 Resist pattern 5 ITO electrode pattern
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Abstract
Le problème décrit par la présente invention est de fournir un liquide de gravure qui dissout sélectivement un film conducteur transparent sans corroder le cuivre. La solution selon l'invention porte sur un liquide de gravure qui contient (a) un halogénure d'hydrogène, (b) un halogénure de métal, (c) un inhibiteur de dissolution du cuivre qui est choisi parmi l'hydroxylamine et ses sels et (d) un diluant, tout en contenant facultativement (e) un oxydant.
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JP2012508965A (ja) * | 2008-11-12 | 2012-04-12 | テクノ セミケム シーオー., エルティーディー. | 透明伝導膜エッチング溶液 |
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JP2010538167A (ja) * | 2007-09-06 | 2010-12-09 | イー.ケー.シー.テクノロジー.インコーポレーテッド | 銅表面を処理するための組成物およびその方法 |
JP2012508965A (ja) * | 2008-11-12 | 2012-04-12 | テクノ セミケム シーオー., エルティーディー. | 透明伝導膜エッチング溶液 |
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