KR102469931B1 - Composition for cleaning a mask, pre-composition for cleaning a mask, and method for manufacturing the same - Google Patents
Composition for cleaning a mask, pre-composition for cleaning a mask, and method for manufacturing the same Download PDFInfo
- Publication number
- KR102469931B1 KR102469931B1 KR1020170170539A KR20170170539A KR102469931B1 KR 102469931 B1 KR102469931 B1 KR 102469931B1 KR 1020170170539 A KR1020170170539 A KR 1020170170539A KR 20170170539 A KR20170170539 A KR 20170170539A KR 102469931 B1 KR102469931 B1 KR 102469931B1
- Authority
- KR
- South Korea
- Prior art keywords
- acid
- ammonium
- cleaning liquid
- mask
- composition
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 119
- 238000004140 cleaning Methods 0.000 title claims abstract description 107
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000007788 liquid Substances 0.000 claims abstract description 82
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 71
- -1 ammonium salt compounds Chemical class 0.000 claims abstract description 49
- 150000001875 compounds Chemical class 0.000 claims abstract description 45
- 229910052751 metal Inorganic materials 0.000 claims abstract description 42
- 239000002184 metal Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000003513 alkali Substances 0.000 claims abstract description 40
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 39
- 150000007524 organic acids Chemical class 0.000 claims abstract description 35
- 235000005985 organic acids Nutrition 0.000 claims abstract description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 35
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 30
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical group [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 26
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 20
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 16
- 229910052709 silver Inorganic materials 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 229910045601 alloy Inorganic materials 0.000 claims description 15
- 239000000956 alloy Substances 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 14
- 150000002739 metals Chemical class 0.000 claims description 14
- 239000005695 Ammonium acetate Substances 0.000 claims description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 13
- 229910052782 aluminium Inorganic materials 0.000 claims description 13
- 235000019257 ammonium acetate Nutrition 0.000 claims description 13
- 229940043376 ammonium acetate Drugs 0.000 claims description 13
- 229910052749 magnesium Inorganic materials 0.000 claims description 13
- 239000011777 magnesium Substances 0.000 claims description 13
- 239000004332 silver Substances 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 12
- 239000010935 stainless steel Substances 0.000 claims description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 11
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 10
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 10
- 229910052791 calcium Inorganic materials 0.000 claims description 10
- 239000011575 calcium Substances 0.000 claims description 10
- 229910052744 lithium Inorganic materials 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 235000006408 oxalic acid Nutrition 0.000 claims description 10
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 9
- 239000010949 copper Substances 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 9
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 8
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 8
- KVFVBPYVNUCWJX-UHFFFAOYSA-M ethyl(trimethyl)azanium;hydroxide Chemical compound [OH-].CC[N+](C)(C)C KVFVBPYVNUCWJX-UHFFFAOYSA-M 0.000 claims description 8
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims description 8
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 8
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 claims description 8
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 8
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 8
- 239000004254 Ammonium phosphate Substances 0.000 claims description 7
- 229940010556 ammonium phosphate Drugs 0.000 claims description 7
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 7
- 229940070336 ammonium phosphate,monobasic Drugs 0.000 claims description 7
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 7
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 7
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 7
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 7
- 229940116349 dibasic ammonium phosphate Drugs 0.000 claims description 7
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 7
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims 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 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 5
- 239000011651 chromium Substances 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 239000011975 tartaric acid Substances 0.000 claims description 5
- 235000002906 tartaric acid Nutrition 0.000 claims description 5
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 4
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims description 4
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 4
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 4
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 4
- 235000011054 acetic acid Nutrition 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000001361 adipic acid Substances 0.000 claims description 4
- 235000011037 adipic acid Nutrition 0.000 claims description 4
- 150000008044 alkali metal hydroxides Chemical group 0.000 claims description 4
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 4
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 4
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 4
- HNEGQIOMVPPMNR-IHWYPQMZSA-N citraconic acid Chemical compound OC(=O)C(/C)=C\C(O)=O HNEGQIOMVPPMNR-IHWYPQMZSA-N 0.000 claims description 4
- 229940018557 citraconic acid Drugs 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- 239000001530 fumaric acid Substances 0.000 claims description 4
- 239000004310 lactic acid Substances 0.000 claims description 4
- 235000014655 lactic acid Nutrition 0.000 claims description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 4
- 239000011976 maleic acid Substances 0.000 claims description 4
- 239000001630 malic acid Substances 0.000 claims description 4
- 235000011090 malic acid Nutrition 0.000 claims description 4
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 4
- 150000005622 tetraalkylammonium hydroxides Chemical class 0.000 claims description 4
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims description 4
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 claims description 3
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 2
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 2
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- 239000000174 gluconic acid Substances 0.000 claims description 2
- 235000012208 gluconic acid Nutrition 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 6
- 229910021529 ammonia Inorganic materials 0.000 claims 6
- 239000000908 ammonium hydroxide Substances 0.000 claims 6
- 230000000694 effects Effects 0.000 abstract description 5
- 238000004090 dissolution Methods 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 22
- 230000008859 change Effects 0.000 description 11
- 238000011156 evaluation Methods 0.000 description 7
- 239000004615 ingredient Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 229910001374 Invar Inorganic materials 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000005137 deposition process Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000001771 vacuum deposition Methods 0.000 description 4
- 239000010408 film Substances 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- QOSATHPSBFQAML-UHFFFAOYSA-N hydrogen peroxide;hydrate Chemical compound O.OO QOSATHPSBFQAML-UHFFFAOYSA-N 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 239000002798 polar solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 239000013585 weight reducing agent Substances 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 150000003868 ammonium compounds Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
Classifications
-
- 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
- C11D7/26—Organic compounds containing oxygen
- C11D7/266—Esters or carbonates
-
- C11D11/0047—
-
- 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
-
- 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
- C11D7/06—Hydroxides
-
- 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
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/10—Salts
- C11D7/105—Nitrates; Nitrites
-
- 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
- C11D7/16—Phosphates including polyphosphates
-
- 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
- C11D7/26—Organic compounds containing oxygen
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
본 발명은 하이드록실기를 포함하는 알칼리 화합물; 암모늄염 화합물; 유기산; 과산화수소; 및 물을 포함하는 마스크 세정액 조성물, 마스크 세정액 예비-조성물, 및 마스크 세정액 조성물의 제조방법을 제공한다. 상기 조성물은 마스크를 손상시키지 않으면서, 마스크 상에 증착된 금속을 산화 및 용해과정에 의해 신속하게 제거하는 효과를 제공한다.The present invention relates to an alkali compound containing a hydroxyl group; ammonium salt compounds; organic acids; hydrogen peroxide; and a mask cleaning liquid composition containing water, a mask cleaning liquid pre-composition, and a method for preparing the mask cleaning liquid composition. The composition provides an effect of quickly removing the metal deposited on the mask by oxidation and dissolution without damaging the mask.
Description
본 발명은 마스크 세정액 조성물, 구체적으로 증착 공정에서 사용되는 마스크 상의 각종 금속을 제거하는 마스크 세정액 조성물, 마스크 세정액 예비-조성물, 및 마스크 세정액 조성물의 제조방법에 관한 것이다.The present invention relates to a mask cleaning liquid composition, specifically a mask cleaning liquid composition for removing various metals on a mask used in a deposition process, a mask cleaning liquid pre-composition, and a method for preparing the mask cleaning liquid composition.
평판 디스플레이(flat panel display, FPD)는 표시장치로서 주목 받고 있으며, 그 중에서도 액정 표시장치와 OLED(Organic Light Emitting Diode)가 관심의 대상이 되고 있다.A flat panel display (FPD) is attracting attention as a display device, and among them, a liquid crystal display device and an organic light emitting diode (OLED) are attracting attention.
현재 디스플레이로서 가장 많이 사용되고 있는 액정표시장치는, 기존의 CRT (Cathod ray tube; 음극선관)에 비해 가볍고 부피가 작으며 저전력 등의 장점을 가지고 있다. 그러나 자체발광이 아니기 때문에 후면광(Backlight)을 사용하여야 하며, 액정을 사용하여 시야각이 제한을 받는 단점이 있다.A liquid crystal display device, which is currently most widely used as a display, has advantages such as light weight, small volume, and low power consumption compared to conventional cathode ray tubes (CRTs). However, since it is not self-luminous, a backlight must be used, and the viewing angle is limited due to the use of liquid crystal.
이에 비해 OLED 소자는 저전압구동, 높은 발광 효율, 넓은 시야각, 빠른 응답속도 등의 장점이 있으며, 무엇보다도 자체발광형이기 때문에 후면광 등이 필요하지 않은 장점이 있다. 이러한 OLED 소자는 자체발광을 하는 발광 유기물을 사용하여 음극과 양극으로부터 공급된 전자와 정공이 재결합되면서 발광이 일어나게 된다.On the other hand, OLED devices have advantages such as low voltage driving, high luminous efficiency, wide viewing angle, and fast response speed, and above all, because they are self-emitting, they do not require a back light. Such an OLED device uses a light-emitting organic material that emits light by itself, and electrons and holes supplied from a cathode and an anode recombine to emit light.
이런 OLED와 같은 반도체 디바이스 또는 평판 디스플레이는 제조 공정 중 전기전도성 패턴 등을 형성하기 위하여 마스크를 이용하여 금속 증착을 수행하게 된다. 이때, 마스크의 표면에도 금속이 부착되게 되며, 이렇게 부착된 금속으로 인하여 마스크로 형성된 패턴의 형상이 변형될 수 있다. 이는, 증착공정의 효율 저하를 야기하며, 제조되는 반도체 디바이스 또는 평판 디스플레이의 성능에도 영향을 미칠 수 있으므로, 마스크에 증착된 금속을 제거해야 할 필요가 있다.A semiconductor device such as an OLED or a flat panel display performs metal deposition using a mask to form an electrically conductive pattern or the like during a manufacturing process. At this time, metal is also attached to the surface of the mask, and the shape of the pattern formed by the mask may be deformed due to the metal attached in this way. This causes a decrease in the efficiency of the deposition process and may affect the performance of a semiconductor device or flat panel display to be manufactured, so it is necessary to remove the metal deposited on the mask.
대한민국 공개특허 제2005-0054452호는 저분자 유기형 EL 소자 제조의 진공 증착 공정에서 이용하는 마스크의 세정액 및 세정방법에 관한 것으로서, 저분자형 유기 EL 소자 제조의 진공증착 공정에 있어서, 이용하는 마스크의 세정액으로 비프로톤성 극성용제(aprotic polar solvent)를 1종류 또는 2종류 이상 포함하는 세정액에 관한 내용을 개시하고 있다.Korean Patent Laid-open Publication No. 2005-0054452 relates to a cleaning liquid and cleaning method for a mask used in a vacuum deposition process for manufacturing a low molecular weight organic EL device. Disclosed is a cleaning liquid containing one or two or more aprotic polar solvents.
그러나, 상기 세정액의 경우 OLED 소자의 유기재료의 증착 시 사용된 금속 마스크의 유기박막재료를 제거하기 위한 것이며, 그 조성 또한 비프로톤성 극성용제로 이루어져 있는 것으로서, 마스크 상에 부착되는 각종 금속을 제거하지 못하는 문제점이 있다.However, in the case of the cleaning liquid, it is for removing the organic thin film material of the metal mask used in the deposition of the organic material of the OLED device, and its composition is also made of an aprotic polar solvent, which removes various metals attached to the mask. There are problems with not being able to do it.
대한민국 공개특허 제2009-0081566호는 은 박막의 식각액 조성물 및 이를 이용한 금속 패턴형성방법에 관한 것으로서, 은 또는 은 합금의 단일막 및 상기 단일막과 산화인듐막으로 구성되는 다중막의 식각액 조성물에 관한 것이다.Korean Patent Publication No. 2009-0081566 relates to an etchant composition of a silver thin film and a method of forming a metal pattern using the same, and relates to a single film of silver or silver alloy and a multilayer etchant composition composed of the single film and an indium oxide film. .
그러나, 상기 식각액 조성물을 사용하여 마스크를 세척할 경우, 마스크 자체에 부식이 일어날 여지가 있어 바람직하지 않다.However, when the mask is washed using the etchant composition, corrosion may occur in the mask itself, which is undesirable.
그러므로, 증착 공정에서 사용되는 마스크 상에 증착되는 은, 마그네슘, 칼슘, 리튬, 알루미늄 등과 같은 각종 금속을 효율적으로 제거하면서, 마스크 자체에는 데미지를 주지 않는 마스크 세정액 조성물의 개발이 요구되는 상황이다.Therefore, there is a need to develop a mask cleaning liquid composition that does not damage the mask itself while efficiently removing various metals such as silver, magnesium, calcium, lithium, aluminum, etc. deposited on the mask used in the deposition process.
본 발명은 종래기술의 상기와 같은 문제를 해결하기 위하여 안출된 것으로서, 마스크에 손상을 주지 않으면서, 증착 공정에서 마스크 상에 부착된 각종 금속 및 유기 오염물을 효율적으로 제거할 수 있는 마스크 세정액 조성물, 마스크 세정액 예비-조성물, 및 마스크 세정액 조성물의 제조방법을 제공하는 것을 목적으로 한다.The present invention has been made to solve the above problems of the prior art, a mask cleaning liquid composition capable of efficiently removing various metal and organic contaminants attached to the mask in a deposition process without damaging the mask, It is an object to provide a mask cleaning liquid pre-composition and a method for producing the mask cleaning liquid composition.
상기 목적을 달성하기 위하여, 본 발명은 하이드록실기를 포함하는 알칼리 화합물; 암모늄염 화합물; 유기산; 과산화수소; 및 물을 포함하는 마스크 세정액 조성물을 제공한다.In order to achieve the above object, the present invention is an alkali compound containing a hydroxyl group; ammonium salt compounds; organic acids; hydrogen peroxide; And it provides a mask cleaning liquid composition containing water.
본 발명의 일 실시 형태에 있어서, 상기 마스크 세정액 조성물은 은, 마그네슘, 칼슘, 리튬, 알루미늄 및 이터븀으로 이루어진 군에서 선택되는 1종 이상의 금속 또는 이의 합금을 제거하기 위하여 사용될 수 있다. In one embodiment of the present invention, the mask cleaning liquid composition may be used to remove one or more metals or alloys thereof selected from the group consisting of silver, magnesium, calcium, lithium, aluminum, and ytterbium.
본 발명의 일 실시 형태에 있어서, 상기 마스크는 철, 크롬, 니켈, 구리, 규소 및 이들의 조합으로 이루어진 군에서 선택되는 1 이상의 재료 또는 이들의 합금을 포함하는 것일 수 있다. In one embodiment of the present invention, the mask may include one or more materials selected from the group consisting of iron, chromium, nickel, copper, silicon, and combinations thereof, or alloys thereof.
또한, 본 발명은 하이드록실기를 포함하는 알칼리 화합물, 유기산, 및 물을 포함하며, 암모늄염 화합물, 과산화수소 및 물과 혼합하여 사용하기 위한 용도를 갖는 마스크 세정액 예비-조성물을 제공한다. In addition, the present invention includes an alkali compound containing a hydroxyl group, an organic acid, and water, and an ammonium salt compound, hydrogen peroxide and A mask wash liquid pre-composition intended for use in admixture with water is provided.
또한, 본 발명은 암모늄염 화합물, 과산화수소 및 물을 포함하며, 하이드록실기를 포함하는 알칼리 화합물, 유기산, 및 물과 혼합하여 사용하기 위한 용도를 갖는 마스크 세정액 예비-조성물을 제공한다. In addition, the present invention is an ammonium salt compound, hydrogen peroxide and Provided is a mask cleaning liquid pre-composition containing water and intended for use in a mixture with an alkali compound containing a hydroxyl group, an organic acid, and water.
또한, 본 발명은 하이드록실기를 포함하는 알칼리 화합물, 암모늄염 화합물, 유기산 및 물을 포함하며, 과산화수소 또는 과산화수소수와 혼합하여 사용하기 위한 용도를 갖는 마스크 세정액 예비-조성물을 제공한다.In addition, the present invention provides a mask cleaning liquid pre-composition containing an alkali compound containing a hydroxyl group, an ammonium salt compound, an organic acid and water, and having a purpose for use in combination with hydrogen peroxide or hydrogen peroxide water.
또한, 본 발명은 (a) 하이드록실기를 포함하는 알칼리 화합물, 유기산, 및 물을 포함하는 마스크 세정액 예비-조성물을 제조하는 단계; (b) 암모늄염 화합물, 과산화수소 및 물을 포함하는 마스크 세정액 예비-조성물을 제조하는 단계; 및 (c) 상기 (a)단계에서 제조된 예비-조성물과 (b)단계에서 제조된 예비-조성물을 혼합하는 단계;를 포함하는 마스크 세정액 조성물의 제조방법을 제공한다.In addition, the present invention includes (a) preparing a mask cleaning liquid pre-composition comprising an alkali compound containing a hydroxyl group, an organic acid, and water; (b) preparing a mask cleaning liquid pre-composition comprising an ammonium salt compound, hydrogen peroxide and water; and (c) mixing the pre-composition prepared in step (a) with the pre-composition prepared in step (b).
또한, 본 발명은 (a) 하이드록실기를 포함하는 알칼리 화합물, 암모늄염 화합물, 유기산, 및 물을 포함하는 마스크 세정액 예비-조성물을 제조하는 단계; 및 (b) 상기 (a)단계에서 제조된 예비-조성물과 과산화수소 또는 과산화수소수를 혼합하는 단계;를 포함하는 마스크 세정액 조성물의 제조방법을 제공한다.In addition, the present invention provides a mask cleaning liquid pre-composition comprising (a) an alkali compound containing a hydroxyl group, an ammonium salt compound, an organic acid, and water; preparing a composition; and (b) mixing the pre-composition prepared in step (a) with hydrogen peroxide or hydrogen peroxide solution.
본 발명에 따른 마스크 세정액 조성물은 마스크를 손상시키지 않으면서, 마스크 상에 증착된 금속을 산화 및 용해과정에 의해 신속하게 제거하는 효과를 제공한다. The mask cleaning liquid composition according to the present invention provides an effect of rapidly removing metal deposited on a mask by oxidation and dissolution without damaging the mask.
또한, 본 발명은 상기 마스크 세정액 조성물을 제조하는 효율적인 방법을 제공한다.In addition, the present invention provides an efficient method for preparing the mask cleaning liquid composition.
이하, 본 발명에 대하여 더욱 상세히 설명한다.Hereinafter, the present invention will be described in more detail.
본 발명은 하이드록실기를 포함하는 알칼리 화합물; 암모늄염 화합물; 유기산; 과산화수소; 및 물을 포함하는 마스크 세정액 조성물에 관한 것이다.The present invention relates to an alkali compound containing a hydroxyl group; ammonium salt compounds; organic acids; hydrogen peroxide; And it relates to a mask cleaning liquid composition comprising water.
상기 마스크 세정액 조성물은 조성물 총 중량에 대하여,The mask cleaning liquid composition, based on the total weight of the composition,
하이드록실기를 포함하는 알칼리 화합물 0.1 내지 10 중량%; 암모늄염 화합물 0.1 내지 10 중량%; 유기산 0.5 내지 10 중량%; 과산화수소 1 내지 60 중량%; 및 잔부의 물을 포함할 수 있다. 0.1 to 10% by weight of an alkali compound containing a hydroxyl group; 0.1 to 10% by weight of an ammonium salt compound; 0.5 to 10% by weight of an organic acid; 1 to 60% by weight of hydrogen peroxide; and balance water.
일반적으로 OLED와 같은 반도체 소자를 제조하기 위해서, 기판의 소정 영역에 은, 마그네슘, 칼슘, 리튬, 알루미늄 또는 이터븀과 같은 전기전도성 재료를 진공증착(vaccum vapor deposition)하여 캐소드 전극 등을 형성하게 된다.In general, in order to manufacture a semiconductor device such as an OLED, an electrically conductive material such as silver, magnesium, calcium, lithium, aluminum or ytterbium is vacuum vapor deposited on a predetermined region of a substrate to form a cathode electrode or the like. .
이 과정에서 증착을 위하여 사용된 마스크 위에도 증착하고자 했던 금속이 증착되게 되므로, 마스크 상의 증착된 금속을 제거해야 할 필요가 있다.In this process, since the metal to be deposited is also deposited on the mask used for deposition, it is necessary to remove the deposited metal on the mask.
본 발명에 따른 마스크 세정액 조성물은 마스크 상에 증착 또는 부착된 금속, 특히 OLED 제조 공정에서 진공증착 공정에 의하여 마스크 상에 증착 또는 부착되는 은, 마그네슘, 칼슘, 리튬, 알루미늄, 이터븀과 같은 금속을 효율적으로 제거할 수 있다.The mask cleaning liquid composition according to the present invention is a metal deposited or attached on a mask, in particular, a metal such as silver, magnesium, calcium, lithium, aluminum, or ytterbium deposited or attached on a mask by a vacuum deposition process in an OLED manufacturing process. can be effectively removed.
이하에서, 본 발명의 마스크 세정액 조성물을 구성하는 구성성분들에 대하여 설명한다. Hereinafter, components constituting the mask cleaning liquid composition of the present invention will be described.
하이드록실기를 포함하는 알칼리 화합물Alkali compounds containing hydroxyl groups
상기 하이드록실기를 포함하는 알칼리 화합물은 pH 조절제 이며, 수용액 상태에서 마스크표면과 마스크 상부에 부착된 금속의 계면에 침투하여 빠른 시간에 마스크 표면으로부터 금속을 탈착시키는 기능을 수행한다. 상기 하이드록실기를 포함하는 알칼리 화합물은 용제에 포함되어 하이드록사이드 이온을 배출하며, 산화된 금속의 용해를 촉진하는 역할을 하며 또한, 파티클(particle)의 재흡착을 방지 하며 세정효과를 향상시킨다.The alkali compound containing the hydroxyl group is a pH adjusting agent and penetrates into the interface between the mask surface and the metal attached to the top of the mask in an aqueous solution to quickly detach the metal from the mask surface. The alkali compound containing the hydroxyl group is included in the solvent to release hydroxide ions, serves to promote the dissolution of oxidized metal, and also prevents re-adsorption of particles and improves the cleaning effect .
본 발명의 하이드록실기를 포함하는 알칼리 화합물로는 알칼리금속 하이드록사이드 또는 테트라알킬암모늄 하이드록사이드를 사용할 수 있다. Alkali metal hydroxide or tetraalkylammonium hydroxide may be used as the alkali compound containing a hydroxyl group of the present invention.
상기 알칼리금속 하이드록사이드로는 리튬하이드록사이드, 나트륨하이드록사이드, 칼륨하이드록사이드, 칼슘하이드록사이드, 바륨하이드록사이드 등을 들 수 있으며, 테트라 알킬암모늄 하이드록사이드로는 테트라메틸암모늄 하이드록사이드(TMAH), 에틸트리메틸암모늄 하이드록사이드(ETMAH), 테트라에틸암모늄 하이드 록사이드(TEAH), 테트라프로필암모늄 하이드록사이드(TPAH) 및 테트라부틸암모늄 하이드록사이드(TBAH) 등을 들수 있으며, 이들은 1종 단독으로 또는 2종 이상의 조합으로 사용될 수 있다.Examples of the alkali metal hydroxide include lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium hydroxide, barium hydroxide, and the like, and tetramethylammonium hydroxide as tetraalkylammonium hydroxide oxide (TMAH), ethyltrimethylammonium hydroxide (ETMAH), tetraethylammonium hydroxide (TEAH), tetrapropylammonium hydroxide (TPAH), and tetrabutylammonium hydroxide (TBAH). These may be used individually by 1 type or in combination of 2 or more types.
상기 하이드록실기를 포함하는 알칼리 화합물은 조성물 총 중량에 대하여 0.1 내지 10 중량%, 바람직하게는 0.1 내지 5 중량%로 포함될 수 있다. The alkali compound containing the hydroxyl group may be included in an amount of 0.1 to 10% by weight, preferably 0.1 to 5% by weight, based on the total weight of the composition.
상술한 범위로 포함되는 경우, 마스크 상부에 부착된 금속의 탈착 속도 저하로 인한 세정력 저하를 방지할 수 있으며, 장기 사용시 상기 알칼리 화합물의 석출에 의한 재오염을 방지할 수 있으며, 마스크 표면에 변색도 방지할 수 있어서 바람직하다. When included within the above-mentioned range, it is possible to prevent deterioration in detergency due to a decrease in the desorption rate of metal attached to the upper part of the mask, and to prevent re-contamination due to precipitation of the alkali compound during long-term use, and also to prevent discoloration on the mask surface. It is preferable to avoid it.
암모늄 화합물ammonium compounds
상기 암모늄염 화합물은 마스크 상에 부착된 금속에 대한 용해도를 증가시키는 기능을 수행한다. 특히, 상기 암모늄염 화합물은 세정액 혼합 조성물에 포함되어 세정액이 Ag에 대하여 우수한 용해도를 갖게 한다. The ammonium salt compound serves to increase the solubility of the metal attached to the mask. In particular, the ammonium salt compound is included in the cleaning liquid mixture composition to make the cleaning liquid have excellent solubility in Ag.
상기 암모늄염 화합물로는, 예를 들어, 아세트산암모늄, 질산암모늄, 인산암모늄, 제1인산암모늄, 제2인산암모늄, 황산암모늄, 과황산암모늄, 탄산암모늄, 중탄산암모늄 등을 들 수 있으며, 이들은 1종 단독으로 또는 2종 이상의 조합으로 사용될 수 있다.Examples of the ammonium salt compound include ammonium acetate, ammonium nitrate, ammonium phosphate, monobasic ammonium phosphate, dibasic ammonium phosphate, ammonium sulfate, ammonium persulfate, ammonium carbonate, and ammonium bicarbonate. They may be used alone or in combination of two or more.
상기 암모늄염 화합물은 조성물 총 중량에 대하여 0.1 내지 10 중량%, 바람직하게는 1 내지 5 중량%로 포함될 수 있다. 암모늄염 화합물이 상술한 범위로 포함되면, 금속, 구체적으로 은과 같은 금속에 대한 충분한 용해성을 제공하며, 장기 사용시 암모늄염 화합물이 석출됨에 따라 재오염의 원인으로 작용하는 것이 방지되어 바람직하다.The ammonium salt compound may be included in an amount of 0.1 to 10% by weight, preferably 1 to 5% by weight, based on the total weight of the composition. When the ammonium salt compound is included in the above-described range, it provides sufficient solubility for metals, specifically metals such as silver, and is preferably prevented from acting as a cause of recontamination as the ammonium salt compound is precipitated during long-term use.
유기산organic acid
상기 유기산은 후술할 과산화수소에 의해 산화된 금속과 킬레이트 결합을 통해 금속을 용해시키는 역할을 수행한다. The organic acid serves to dissolve the metal through a chelate bond with a metal oxidized by hydrogen peroxide, which will be described later.
상기 유기산으로는, 예를 들어, 설포살리실산, 글루코닉산, 구연산, 에틸렌디아민테트라아세트산, 초산, 개미산, 및 옥살산, 타타르산, 말산, 말론산, 말레산, 프탈산, 락트산, 숙신산, 글루타르산, 아디프산, 피메르산, 세바스산, 푸마르산, 이타콘산, 수베르산, 아젤라인산, 시트라콘산 등을 들 수 있으며, 이들은 1종 단독으로 또는 2종 이상의 조합으로 사용될 수 있다.Examples of the organic acids include sulfosalicylic acid, gluconic acid, citric acid, ethylenediaminetetraacetic acid, acetic acid, formic acid, and oxalic acid, tartaric acid, malic acid, malonic acid, maleic acid, phthalic acid, lactic acid, succinic acid, and glutaric acid. , adipic acid, pimeric acid, sebacic acid, fumaric acid, itaconic acid, suberic acid, azelaic acid, citraconic acid, and the like, which may be used alone or in combination of two or more.
특히, 상기 유기산은 카르복실기를 2개 이상 포함하는 화합물인 것일 수 있으며, 상기 카르복실기를 2개 이상 포함하는 화합물은 구연산, 에틸렌디아민테트라아세트산, 옥살산, 타타르산, 말산, 말론산, 말레산, 프탈산, 락트산, 숙신산, 글루타르산, 아디프산, 피메르산, 세바스산, 푸마르산, 이타콘산, 수베르산, 아젤라인산, 시트라콘산으로 이루어진 군으로부터 선택되는 1종 이상일 수 있다. In particular, the organic acid may be a compound containing two or more carboxyl groups, and the compound containing two or more carboxyl groups may include citric acid, ethylenediaminetetraacetic acid, oxalic acid, tartaric acid, malic acid, malonic acid, maleic acid, phthalic acid, It may be at least one selected from the group consisting of lactic acid, succinic acid, glutaric acid, adipic acid, pimeric acid, sebacic acid, fumaric acid, itaconic acid, suberic acid, azelaic acid, and citraconic acid.
상기 유기산은 조성물 총 중량에 대하여 0.5 내지 10 중량%, 바람직하게는 1 내지 5 중량%로 포함될 수 있다. 유기산이 상술한 범위로 포함되면 금속에 대한 용해성이 좋아지며, STS(Stainless steel), Ni, Fe와 Ni의 합금, Cu 또는 실리콘을 포함하는 마스크의 부식 염려가 방지되므로 바람직하다. The organic acid may be included in an amount of 0.5 to 10% by weight, preferably 1 to 5% by weight, based on the total weight of the composition. When the organic acid is included in the above-described range, solubility in metal is improved, and corrosion concerns of a mask including STS (Stainless steel), Ni, an alloy of Fe and Ni, Cu, or silicon are prevented, so it is preferable.
과산화 수소hydrogen peroxide
상기 과산화수소는 강한 산화제 역할을 수행할 수 있다. The hydrogen peroxide can act as a strong oxidizing agent.
과산화수소는 조성물 총 중량에 대하여 1 내지 60 중량%, 바람직하게는 5 내지 40 중량%로 포함될 수 있다. 과산화수소가 상술한 범위로 포함될 경우 금속에 대한 산화를 촉진하여 금속 제거력을 향상 시킬 수 있다. 상기 범위를 초과하는 경우 제거력 향상 효과가 더 이상 증대되지 않아 경제적 측면에서 바람직하지 않다. Hydrogen peroxide may be included in an amount of 1 to 60% by weight, preferably 5 to 40% by weight, based on the total weight of the composition. When hydrogen peroxide is included in the above-described range, metal removal may be improved by promoting oxidation of metal. When the above range is exceeded, the effect of improving the removal power is not further increased, which is not preferable from an economic point of view.
물water
본 발명의 마스크 세정액 조성물은 잔부의 물을 포함한다. 상기 물은 불순물을 최대한 저감시킨 탈이온수(deionized water) 또는 초순수(ultrapure water)일 수 있으나, 이에 한정되지 않는다.The mask cleaning liquid composition of the present invention contains the balance of water. The water may be deionized water or ultrapure water in which impurities are reduced as much as possible, but is not limited thereto.
본 발명의 마스크 세정액 조성물은 은, 마그네슘, 칼슘, 리튬, 알루미늄, 이터븀 등으로 이루어진 군에서 선택되는 1 이상의 금속 또는 이의 합금을 제거하기 위여 사용될 수 있다. 구체적으로, 본 발명에 따른 마스크 세정액 조성물은 반도체 소자 제조 공정 중, 전기전도성 패턴을 형성하기 위하여 수행하는 금속 증착 공정에서 이용되는 마스크 상에 함께 증착되는 각종 금속, 더욱 구체적으로 은, 마그네슘, 칼슘, 리튬, 알루미늄, 이터븀 등으로 이루어진 군에서 선택되는 1 이상의 금속 또는 이의 합금을 제거하기 위하여 사용될 수 있다. The mask cleaning liquid composition of the present invention may be used to remove one or more metals or alloys thereof selected from the group consisting of silver, magnesium, calcium, lithium, aluminum, ytterbium, and the like. Specifically, the mask cleaning liquid composition according to the present invention includes various metals, more specifically, silver, magnesium, calcium, It may be used to remove one or more metals or alloys thereof selected from the group consisting of lithium, aluminum, ytterbium, and the like.
또한, 본 발명의 바람직한 실시형태에서, 상기 마스크 세정액 조성물은 은, 마그네슘, 칼슘, 리튬, 알루미늄, 이터븀 등으로 이루어진 군에서 선택되는 1 이상의 금속 또는 이의 합금을 선택적 제거에 바람직하게 사용될 수 있다. In addition, in a preferred embodiment of the present invention, the mask cleaning liquid composition may be preferably used for selectively removing one or more metals or alloys thereof selected from the group consisting of silver, magnesium, calcium, lithium, aluminum, ytterbium, and the like.
상기 "선택적 제거"란, 상기 마스크 세정액 조성물이 상기 은, 마그네슘, 칼슘, 리튬, 알루미늄, 이터븀 등으로 이루어진 군에서 선택되는 1 이상의 금속 또는 이의 합금만을 선택적으로 제거하고, 마스크를 이루고 있는 철, 크롬, 니켈, 구리, 규소 및 이들의 조합으로 이루어진 군에서 선택되는 1 이상의 재료 또는 이의 합금에는 손상을 주지 않는 것을 의미한다. The "selective removal" means that the mask cleaning liquid composition selectively removes only one or more metals or alloys thereof selected from the group consisting of silver, magnesium, calcium, lithium, aluminum, ytterbium, etc., and iron constituting the mask, It means that one or more materials selected from the group consisting of chromium, nickel, copper, silicon, and combinations thereof or alloys thereof are not damaged.
본 발명의 또 다른 실시형태에 있어서, 상기 마스크는 철, 크롬, 니켈, 구리, 규소 및 이들의 조합으로 이루어진 군에서 선택되는 1 이상의 재료 또는 이의 합금을 포함하여 제조된 것일 수 있다. 본 발명의 또 다른 실시형태에 있어서, 상기 마스크는 STS(Stainless steel), Ni단체, Fe와 Ni의 합금, Cu 또는 실리콘을 포함하여 제조된 것일 수 있다. 상기에서 "Ni단체"는 Ni로만 이루어진 것을 의미한다. In another embodiment of the present invention, the mask may be made of one or more materials selected from the group consisting of iron, chromium, nickel, copper, silicon, and combinations thereof, or an alloy thereof. In another embodiment of the present invention, the mask may be made of STS (Stainless steel), a single Ni, an alloy of Fe and Ni, Cu or silicon. In the above, "Ni simple substance" means made only of Ni.
본 발명에 따른 마스크 세정액 조성물은 당업계에서 통상적으로 사용되고 있는 철, 크롬, 니켈, 구리, 규소 및 이들의 합금으로 이루어진 군에서 선택되는 1 이상을 포함하여 제조된 마스크, 더욱 구체적으로 STS(Stainless steel), Ni단체, Fe와 Ni의 합금, Cu 또는 실리콘을 포함하여 제조된 마스크에는 데미지를 주지 않으면서, 상기 마스크 상의 부착된 은, 마그네슘, 칼슘, 리튬, 알루미늄 및 이터븀과 같은 금속을 선택적으로 제거할 수 있다. The mask cleaning liquid composition according to the present invention is a mask manufactured by including at least one selected from the group consisting of iron, chromium, nickel, copper, silicon, and alloys thereof commonly used in the art, more specifically, STS (Stainless Steel ), Ni alone, an alloy of Fe and Ni, Cu or silicon, without causing damage to the mask, selectively attaching metals such as silver, magnesium, calcium, lithium, aluminum and ytterbium on the mask can be removed
본 발명의 또 다른 실시형태에 있어서, 상기 마스크 세정액 조성물은 진공 증착 공정에 사용되는 마스크를 세정하는 것일 수 있다. 구체적으로, 상기 마스크 세정액 조성물은 OLED와 같은 반도체 소자 제조 공정 중 전기전도성 패턴을 형성하기 위한 진공 증착 공정에 사용되는 마스크를 세정하는 것일 수 있다.In another embodiment of the present invention, the mask cleaning liquid composition may clean a mask used in a vacuum deposition process. Specifically, the mask cleaning liquid composition may be used to clean a mask used in a vacuum deposition process for forming an electrically conductive pattern during a manufacturing process of a semiconductor device such as an OLED.
본 발명에 따른 마스크 세정액 조성물은 상기 마스크에 심각한 손상을 입히지 않고, 반복적으로 세정이 가능하기 때문에 사용 기간이 크게 연장될 수 있는 이점이 있으며, 세정을 고온에서 수행하지 않고 실온에서 실시하는 것이 가능하기 때문에 마스크가 세정 시 변형되는 것을 방지할 수 있다.The mask cleaning liquid composition according to the present invention has the advantage of greatly extending the use period because it can be repeatedly cleaned without causing serious damage to the mask, and it is possible to perform cleaning at room temperature instead of high temperature. Therefore, it is possible to prevent the mask from being deformed during cleaning.
구체적으로, 본 발명에 따른 마스크 세정액 조성물은 10 내지 40℃, 바람직하게는 20 내지 30℃, 보다 바람직하게는 약 25℃에서 사용이 가능하며, 고온 하에서 세정할 필요가 없기 때문에 마스크가 세정 시 변형되는 것을 방지할 수 있는 이점이 있다.Specifically, the mask cleaning liquid composition according to the present invention can be used at 10 to 40 ° C, preferably 20 to 30 ° C, more preferably about 25 ° C, and since there is no need to clean at a high temperature, the mask is deformed during washing. There are advantages to preventing this from happening.
본 발명에 있어서, 상기 마스크 세정액 조성물을 이용하여 마스크를 세정하는 방법은 특별히 한정하지는 않는다. 예컨대, 세정하고자 하는 마스크를 침지 세정법, 요동 세정법, 초음파 세정법, 샤워·스프레이 세정법, 퍼들 세정법, 브러쉬 세정법, 교반 세정법 등의 방법을 통하여 세정할 수 있으며, 바람직하게는 침지 세정법 또는 초음파 세정법을 통하여 세정할 수 있다.In the present invention, the method of cleaning the mask using the mask cleaning liquid composition is not particularly limited. For example, the mask to be cleaned can be cleaned through methods such as immersion cleaning method, shaking cleaning method, ultrasonic cleaning method, shower/spray cleaning method, puddle cleaning method, brush cleaning method, agitation cleaning method, etc., preferably through immersion cleaning method or ultrasonic cleaning method. can do.
본 발명의 마스크 세정액 조성물은 하이드록실기를 포함하는 알칼리 화합물; 암모늄염 화합물; 유기산; 과산화수소; 및 물을 포함하는 1액형의 형태로 제조될 수 있다. The mask cleaning liquid composition of the present invention includes an alkali compound containing a hydroxyl group; ammonium salt compounds; organic acids; hydrogen peroxide; And it can be prepared in a one-component form containing water.
또한, 본 발명의 마스크 세정액 조성물은 혼합하여 사용할 수 있는 다양한 형태의 2액형의 형태로 제조될 수도 있다. In addition, the mask cleaning liquid composition of the present invention may be prepared in a two-component form that can be mixed and used.
본 발명은 2액형의 마스크 세정액 조성물의 예비-조성물로서 예를 들어, 하이드록실기를 포함하는 알칼리 화합물, 유기산, 및 물을 포함하며, 암모늄염 화합물, 과산화수소 및 물과 혼합하여 사용하기 위한 용도를 갖는 마스크 세정액 예비-조성물을 제공한다.The present invention is a pre-composition of a two-component mask cleaning liquid composition, which includes, for example, an alkali compound containing a hydroxyl group, an organic acid, and water, and has a use for use in combination with an ammonium salt compound, hydrogen peroxide, and water. A mask wash pre-composition is provided.
상기 마스크 세정액 예비-조성물은, 예를 들어, 하이드록실기를 포함하는 알칼리 화합물 0.1 내지 10 중량부; 유기산 0.5 내지 10 중량부; 및 물 10 내지 90 중량부를 포함할 수 있다. 상기 각 성분들의 조성비의 의의는 상기에서 기술한 것과 동일하다.The pre-composition of the mask cleaning solution may include, for example, 0.1 to 10 parts by weight of an alkali compound containing a hydroxyl group; 0.5 to 10 parts by weight of an organic acid; and 10 to 90 parts by weight of water. The significance of the composition ratio of each component is the same as that described above.
또한, 암모늄염 화합물, 과산화수소 및 물을 포함하며, 하이드록실기를 포함하는 알칼리 화합물, 유기산, 및 물과 혼합하여 사용하기 위한 용도를 갖는 마스크 세정액 예비-조성물을 제공한다.Also provided is a mask cleaning liquid pre-composition containing an ammonium salt compound, hydrogen peroxide and water and having a purpose for use in a mixture with an alkali compound containing a hydroxyl group, an organic acid, and water.
상기 마스크 세정액 예비-조성물은, 예를 들어, 암모늄염 화합물 0.1 내지 10 중량부; 과산화수소 1 내지 60 중량부; 및 물 10 내지 80 중량부를 포함할 수 있다. 상기 조성비의 의의는 상기에서 기술한 것과 동일하다.The mask cleaning solution pre-composition may include, for example, 0.1 to 10 parts by weight of an ammonium salt compound; 1 to 60 parts by weight of hydrogen peroxide; and 10 to 80 parts by weight of water. The significance of the composition ratio is the same as that described above.
본 발명은 2액형의 마스크 세정액 조성물의 예비-조성물로서 예를 들어, 하이드록실기를 포함하는 알칼리 화합물, 암모늄염 화합물, 유기산, 및 물을 포함하며, 과산화수소 또는 과산화수소수와 혼합하여 사용하기 위한 용도를 갖는 마스크 세정액 예비-조성물을 제공한다.The present invention is a pre-composition of a two-component mask cleaning liquid composition, for example, containing an alkali compound containing a hydroxyl group, an ammonium salt compound, an organic acid, and water, for use in combination with hydrogen peroxide or hydrogen peroxide water . A mask wash pre-composition having
상기 마스크 세정액 예비-조성물은, 예를 들어, 하이드록실기를 포함하는 알칼리 화합물 0.1 내지 10 중량부; 암모늄염 화합물 0.1 내지 10 중량부; 유기산 0.5 내지 10 중량부; 및 물 70 내지 95 중량부를 포함할 수 있다. 상기 조성비의 의의는 상기에서 기술한 것과 동일하다.The pre-composition of the mask cleaning solution may include, for example, 0.1 to 10 parts by weight of an alkali compound containing a hydroxyl group; 0.1 to 10 parts by weight of an ammonium salt compound; 0.5 to 10 parts by weight of an organic acid; and 70 to 95 parts by weight of water. The significance of the composition ratio is the same as that described above.
상기 마스크 세정액 예비-조성물은, 하이드록실기를 포함하는 알칼리 화합물 0.1 내지 10 중량%; 암모늄염 화합물 0.1 내지 10 중량%; 유기산 0.5 내지 10 중량%; 과산화수소 1 내지 60 중량%; 및 잔부의 물을 포함하는 마스크 세정액 조성물을 제조하는데 이용될 수 있도록 각 구성성분의 함량을 포함할 수 있다. The mask cleaning liquid pre-composition includes 0.1 to 10% by weight of an alkali compound containing a hydroxyl group; 0.1 to 10% by weight of an ammonium salt compound; 0.5 to 10% by weight of an organic acid; 1 to 60% by weight of hydrogen peroxide; And it may include the content of each component so that it can be used to prepare a mask cleaning liquid composition containing the balance of water.
상기 2액형의 마스크 세정액 조성물의 제조방법은The method for producing the two-component mask cleaning liquid composition
(a) 하이드록실기를 포함하는 알칼리 화합물, 유기산, 및 물을 포함하는 마스크 세정액 예비-조성물을 제조하는 단계;(a) preparing a mask cleaning liquid pre-composition comprising an alkali compound containing a hydroxyl group, an organic acid, and water;
(b) 암모늄염 화합물, 과산화수소 및 물을 포함하는 마스크 세정액 예비-조성물을 제조하는 단계; 및(b) preparing a mask cleaning liquid pre-composition comprising an ammonium salt compound, hydrogen peroxide and water; and
(c) 상기 (a)단계에서 제조된 예비-조성물과 (b)단계에서 제조된 예비-조성물을 혼합하는 단계;를 포함할 수 있다. (c) mixing the pre-composition prepared in step (a) and the pre-composition prepared in step (b); may include.
또한, 상기 2액형의 마스크 세정액 조성물의 제조방법은 In addition, the method for preparing the two-component mask cleaning liquid composition
(a) 하이드록실기를 포함하는 알칼리 화합물, 암모늄염 화합물, 유기산, 및 물을 포함하는 마스크 세정액 예비-조성물을 제조하는 단계; 및(a) preparing a mask cleaning liquid pre-composition comprising an alkali compound containing a hydroxyl group, an ammonium salt compound, an organic acid, and water; and
(b) 상기 (a)단계에서 제조된 예비-조성물과 과산화수소 또는 과산화수소수를 혼합하는 단계;를 포함할 수 있다. (b) mixing the pre-composition prepared in step (a) with hydrogen peroxide or hydrogen peroxide solution; may include.
이하, 본 명세서를 구체적으로 설명하기 위해 실시예를 들어 상세히 설명한다. 그러나, 본 명세서에 따른 실시예들은 여러 가지 다른 형태로 변형될 수 있으며, 본 명세서의 범위가 아래에서 상술하는 실시예들에 한정되는 것으로 해석되지는 않는다. 본 명세서의 실시예들은 당 업계에서 평균적인 지식을 가진 자에게 본 명세서를 보다 완전하게 설명하기 위해 제공되는 것이다. 또한, 이하에서 함유량을 나타내는 "%" 및 "부"는 특별히 언급하지 않는 한 중량 기준이다.Hereinafter, examples will be described in detail in order to specifically describe the present specification. However, the embodiments according to the present specification may be modified in many different forms, and the scope of the present specification is not construed as being limited to the embodiments described below. The embodiments herein are provided to more completely explain the present specification to those skilled in the art. In addition, "%" and "parts" indicating content below are based on weight unless otherwise specified.
실시예 1 내지 15 및 비교예 1 내지 8: 마스크 세정액 조성물의 제조Examples 1 to 15 and Comparative Examples 1 to 8: Preparation of mask cleaning liquid composition
하기 표 1에 기재된 성분 및 함량으로 상온에서 1시간 동안 500rpm의 속도로 교반하여 실시예 및 비교예에 따른 마스크 세정액 조성물을 제조하였다.Mask cleaning liquid compositions according to Examples and Comparative Examples were prepared by stirring at a rate of 500 rpm for 1 hour at room temperature with the components and contents shown in Table 1 below.
(wt%)hydrogen peroxide
(wt%)
실시예 16 내지 19: 마스크 세정액 예비-조성물의 제조Examples 16 to 19: Preparation of Mask Wash Pre-Composition
하기 표 2에 기재된 성분 및 함량으로 상온에서 1시간 동안 500rpm의 속도로 교반하여 실시예 및 비교예에 따른 마스크 세정액 예비-조성물을 제조하였다.Mask cleaning liquid pre-compositions according to Examples and Comparative Examples were prepared by stirring at a rate of 500 rpm for 1 hour at room temperature with the ingredients and contents shown in Table 2 below.
(wt%)hydrogen peroxide
(wt%)
실시예 20 내지 21: 마스크 세정액 조성물의 제조Examples 20 to 21: Preparation of mask cleaning liquid composition
상기 실시예 16 및 17에서 제조된 각 예비-조성물을 5:5의 중량비로 혼합하여 실시예 20의 마스크 세정액 조성물을 제조하였다.Each of the pre-compositions prepared in Examples 16 and 17 was mixed in a weight ratio of 5:5 to prepare a mask cleaning liquid composition of Example 20.
또한, 상기 실시예 18 및 19에서 제조된 각 예비-조성물을 5:5의 중량비로 혼합하여 실시예 21의 마스크 세정액 조성물을 제조하였다.In addition, each of the pre-compositions prepared in Examples 18 and 19 was mixed in a weight ratio of 5:5 to prepare a mask cleaning liquid composition of Example 21.
시험예: 세정력 및 부식성 평가Test Example: Evaluation of Detergency and Corrosion
상기에서 제조된 실시예 및 비교예에 따른 마스크 세정액 조성물의 세정력 및 부식성을 평가하기 위하여 하기와 같은 실험을 수행하였다.In order to evaluate the cleaning power and corrosiveness of the mask cleaning liquid composition according to the examples and comparative examples prepared above, the following experiments were performed.
(1) 금속이 증착된 마스크 세정력 평가(1) Evaluation of cleaning power of a metal-deposited mask
마스크 세정액 조성물의 세정 효과를 확인하기 위하여 통상적인 방법에 따라 대표적은 금속(Ag, Mg, Al)이 증착된 마스크(재질: Invar)에 대한 세정력 평가를 실시 하였다. 제조한 화합물 및 혼합물을 항온조를 이용하여 40도로 승온 후 약액을 교반한다. 교반되고 있는 약액에 금속이 증착된 마스크를 2x2cm 사이즈로 절단하여 30분 침적 후 탈이온수로 1분 세정하여 SEM을 이용하여 금속의 마스크표면 잔류 유/무 및 마스크 표면의 금속 잔류 함량을 분석하여(EDS) 초기 함량과 비교하여 세정력을 평가 하였다. 세정액 침적 시간은 5분 단위로 진행되었으며 마스크표면에 잔류 물이 잔류 하지 않는 시간을 표시 하여 세정력을 비교 하였다.In order to confirm the cleaning effect of the mask cleaning liquid composition, cleaning power was evaluated for a mask (material: Invar) deposited with representative metals (Ag, Mg, Al) according to a conventional method. After raising the temperature of the prepared compound and mixture to 40 degrees using a thermostat, the chemical solution is stirred. The mask in which the metal is deposited in the chemical solution being stirred is cut into 2x2cm size, immersed for 30 minutes, washed with deionized water for 1 minute, and the presence/absence of metal remaining on the mask surface and the metal residual content on the mask surface are analyzed using SEM ( EDS) The cleaning power was evaluated by comparing with the initial content. The cleaning solution immersion time was carried out in units of 5 minutes, and the cleaning power was compared by displaying the time when no residue remained on the mask surface.
<세정력 평가기준> <Evaluation criteria for detergency>
×: 50% 미만 제거×: less than 50% removal
△: 50%이상 70%미만 제거△: 50% or more and less than 70% removed
○: 70%이상 90%미만 제거○: 70% or more and less than 90% removed
◎: 90%이상 제거◎: 90% or more removed
(2) 마스크 및 마스크 지지체 부식성 평가(2) Evaluation of mask and mask support corrosion resistance
마스크 공정의 재질에 대한 부식성 평가는 실시예 및 비교예에 따라 마스크 패턴 형성을 하는 재질(Invar)와 마스크를 지지하는 지지체(프레임) 재질 STS(Stainless steel)에 대하여 평가 하였으며, 세정액 조성물 200ml를 각각 용량 250ml의 비이커에 넣고 세정액을 40도로 승온시키고, 2x5cm 샘플을 투입하여 5일간 침적한 후 표면의 육안상 변화 및 무게변화를 관찰하였다.Corrosiveness evaluation of the material of the mask process was evaluated for the material for forming the mask pattern (Invar) and the support (frame) material for supporting the mask according to the Examples and Comparative Examples, STS (Stainless steel), and 200 ml of the cleaning liquid composition, respectively After putting it in a beaker with a capacity of 250ml, the cleaning solution was heated to 40 degrees, and a 2x5cm sample was added and deposited for 5 days, and then the surface change and weight change were observed.
<Invar 및 STS 재질 부식성 무게변화 평가기준><Invar and STS material corrosive weight change evaluation criteria>
○: 색변화 없음○: no color change
×: 색변화 있음×: color change
○: 무게변화 없음 (무게감소율 0.01% 미만)○: No weight change (weight reduction rate less than 0.01%)
×: 무게변화 있음 (무게감소율 0.01% 이상)×: Weight change (weight reduction rate 0.01% or more)
상기 표 3에 나타낸 바와 같이, 본 발명에 따른 실시예의 세정액 조성물은 금속 마스크상에 증착된 Ag, Mg, Al 모두에 대하여 우수한 제거력을 나타냈으며, 마스크에 대한 부식 문제도 발생시키지 않았다. As shown in Table 3, the cleaning liquid composition of the embodiment according to the present invention exhibited excellent removal power for all of Ag, Mg, and Al deposited on the metal mask, and did not cause a problem of corrosion on the mask.
반면, 비교예 1 내지 비교예 8의 세정액 조성물은 금속 마스크상에 증착된 Ag, Mg, Al에 대하여 제거력이 부족하거나, 금속 마스크에 대한 부식성도 나타나는 것으로 확인되었다.On the other hand, it was confirmed that the cleaning liquid compositions of Comparative Examples 1 to 8 lacked removal power for Ag, Mg, and Al deposited on the metal mask, or exhibited corrosiveness to the metal mask.
Claims (17)
상기 암모늄염 화합물은 아세트산암모늄, 질산암모늄, 인산암모늄, 제1인산암모늄, 제2인산암모늄, 황산암모늄 및 과황산암모늄으로 이루어진 군으로부터 선택되는 1종 이상의 것이며,
상기 하이드록실기를 포함하는 알칼리 화합물은 수산화 암모늄 및 암모니아를 포함하지 않는 것을 특징으로 하는 마스크 세정액 조성물.alkali compounds containing a hydroxyl group; ammonium salt compounds; organic acids; hydrogen peroxide; and water;
The ammonium salt compound is at least one selected from the group consisting of ammonium acetate, ammonium nitrate, ammonium phosphate, monobasic ammonium phosphate, dibasic ammonium phosphate, ammonium sulfate and ammonium persulfate,
The mask cleaning liquid composition, characterized in that the alkali compound containing the hydroxyl group does not include ammonium hydroxide and ammonia.
하이드록실기를 포함하는 알칼리 화합물 0.1 내지 10 중량%;
암모늄염 화합물 0.1 내지 10 중량%;
유기산 0.5 내지 10 중량%;
과산화수소 1 내지 60 중량%; 및
잔부의 물을 포함하는 마스크 세정액 조성물.The method of claim 1, with respect to the total weight of the composition,
0.1 to 10% by weight of an alkali compound containing a hydroxyl group;
0.1 to 10% by weight of an ammonium salt compound;
0.5 to 10% by weight of an organic acid;
1 to 60% by weight of hydrogen peroxide; and
A mask cleaning liquid composition containing the balance of water.
상기 하이드록실기를 포함하는 알칼리 화합물은 알칼리금속 하이드록사이드 또는 테트라 알킬암모늄 하이드록사이드인 마스크 세정액 조성물.
According to claim 1,
The alkali compound containing the hydroxyl group is an alkali metal hydroxide or a tetra alkylammonium hydroxide mask cleaning liquid composition.
상기 알칼리금속 하이드록사이드는 리튬하이드록사이드, 나트륨하이드록사이드, 칼륨하이드록사이드, 칼슘하이드록사이드, 및 바륨하이드록사이드로 이루어진 군으로부터 선택되는 1종 이상의 것인 것을 특징으로 하는 마스크 세정액 조성물.
According to claim 3,
The alkali metal hydroxide is a mask cleaning liquid composition, characterized in that at least one selected from the group consisting of lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium hydroxide, and barium hydroxide .
상기 테트라 알킬암모늄 하이드록사이드는 테트라메틸암모늄 하이드록사이드(TMAH), 에틸트리메틸암모늄 하이드록사이드(ETMAH), 테트라에틸암모늄 하이드 록사이드(TEAH), 테트라프로필암모늄 하이드록사이드(TPAH) 및 테트라부틸암모늄 하이드록사이드(TBAH)이루어진 군으로부터 선택되는 1종 이상의 것인 것을 특징으로 하는 마스크 세정액 조성물.
According to claim 3,
The tetraalkylammonium hydroxide is tetramethylammonium hydroxide (TMAH), ethyltrimethylammonium hydroxide (ETMAH), tetraethylammonium hydroxide (TEAH), A mask cleaning liquid composition, characterized in that at least one selected from the group consisting of tetrapropylammonium hydroxide (TPAH) and tetrabutylammonium hydroxide (TBAH).
상기 유기산은 카르복실기를 2개 이상 포함하는 화합물인 것을 특징으로 하는 마스크 세정액 조성물.According to claim 1,
The organic acid is a mask cleaning liquid composition, characterized in that the compound containing two or more carboxyl groups.
상기 카르복실기를 2개 이상 포함하는 화합물은 구연산, 에틸렌디아민테트라아세트산, 옥살산, 타타르산, 말산, 말론산, 말레산, 프탈산, 락트산, 숙신산, 글루타르산, 아디프산, 피메르산, 세바스산, 푸마르산, 이타콘산, 수베르산, 아젤라인산 및 시트라콘산으로 이루어진 군으로부터 선택되는 1종 이상의 것인 것을 특징으로 하는 마스크 세정액 조성물.
According to claim 7,
Compounds containing two or more carboxyl groups include citric acid, ethylenediaminetetraacetic acid, oxalic acid, tartaric acid, malic acid, malonic acid, maleic acid, phthalic acid, lactic acid, succinic acid, glutaric acid, adipic acid, pimeric acid, and sebacic acid. , Mask washing composition, characterized in that at least one selected from the group consisting of fumaric acid, itaconic acid, suberic acid, azelaic acid and citraconic acid.
상기 유기산은 설포살리실산, 글루코닉산, 구연산, 에틸렌디아민테트라아세트산, 초산, 개미산, 옥살산, 타타르산, 말산, 말론산, 말레산, 프탈산, 락트산, 숙신산, 글루타르산, 아디프산, 피메르산, 세바스산, 푸마르산, 이타콘산, 수베르산, 아젤라인산, 및 시트라콘산으로 이루어진 군으로부터 선택되는 1종 이상의 것인 것을 특징으로 하는 마스크 세정액 조성물.
According to claim 1,
The organic acid is sulfosalicylic acid, gluconic acid, citric acid, ethylenediaminetetraacetic acid, acetic acid, formic acid, oxalic acid, tartaric acid, malic acid, malonic acid, maleic acid, phthalic acid, lactic acid, succinic acid, glutaric acid, adipic acid, pimer A mask cleaning liquid composition, characterized in that at least one selected from the group consisting of acid, sebacic acid, fumaric acid, itaconic acid, suberic acid, azelaic acid, and citraconic acid.
상기 마스크 세정액 조성물은 은, 마그네슘, 칼슘, 리튬, 알루미늄 및 이터븀으로 이루어진 군에서 선택되는 1종 이상의 금속 또는 이의 합금을 제거하기 위한 것인 마스크 세정액 조성물.According to claim 1,
The mask cleaning liquid composition is for removing one or more metals or alloys thereof selected from the group consisting of silver, magnesium, calcium, lithium, aluminum and ytterbium.
상기 마스크는 철, 크롬, 니켈, 구리, 규소 및 이들의 조합으로 이루어진 군에서 선택되는 1 이상의 재료 또는 이들의 합금을 포함하는 것인 마스크 세정액 조성물.According to claim 1,
The mask is a mask cleaning liquid composition comprising at least one material selected from the group consisting of iron, chromium, nickel, copper, silicon, and combinations thereof, or alloys thereof.
상기 마스크는 STS(Stainless steel), Ni단체, Fe와 Ni의 합금, Cu 또는 실리콘을 포함하는 것인 마스크 세정액 조성물. According to claim 11,
The mask is a mask cleaning liquid composition comprising STS (Stainless steel), Ni alone, an alloy of Fe and Ni, Cu or silicon.
상기 암모늄염 화합물은 아세트산암모늄, 질산암모늄, 인산암모늄, 제1인산암모늄, 제2인산암모늄, 황산암모늄 및 과황산암모늄으로 이루어진 군으로부터 선택되는 1종 이상의 것이며,
상기 하이드록실기를 포함하는 알칼리 화합물은 수산화 암모늄 및 암모니아를 포함하지 않는 것을 특징으로 하는 마스크 세정액 예비-조성물.It contains an alkali compound containing a hydroxyl group, an organic acid, and water, and has a use for mixing with an ammonium salt compound and hydrogen peroxide, or an ammonium salt compound and hydrogen peroxide and water,
The ammonium salt compound is at least one selected from the group consisting of ammonium acetate, ammonium nitrate, ammonium phosphate, monobasic ammonium phosphate, dibasic ammonium phosphate, ammonium sulfate and ammonium persulfate,
The mask cleaning liquid pre-composition, characterized in that the alkali compound containing a hydroxyl group does not contain ammonium hydroxide and ammonia.
상기 암모늄염 화합물은 아세트산암모늄, 질산암모늄, 인산암모늄, 제1인산암모늄, 제2인산암모늄, 황산암모늄 및 과황산암모늄으로 이루어진 군으로부터 선택되는 1종 이상의 것이며,
상기 하이드록실기를 포함하는 알칼리 화합물은 수산화 암모늄 및 암모니아를 포함하지 않는 것을 특징으로 하는 마스크 세정액 예비-조성물.It contains an ammonium salt compound and hydrogen peroxide, or an ammonium salt compound and hydrogen peroxide and water, and has a use for mixing with an alkali compound containing a hydroxyl group, an organic acid, and water,
The ammonium salt compound is at least one selected from the group consisting of ammonium acetate, ammonium nitrate, ammonium phosphate, monobasic ammonium phosphate, dibasic ammonium phosphate, ammonium sulfate and ammonium persulfate,
The mask cleaning liquid pre-composition, characterized in that the alkali compound containing a hydroxyl group does not contain ammonium hydroxide and ammonia.
상기 암모늄염 화합물은 아세트산암모늄, 질산암모늄, 인산암모늄, 제1인산암모늄, 제2인산암모늄, 황산암모늄 및 과황산암모늄으로 이루어진 군으로부터 선택되는 1종 이상의 것이며,
상기 하이드록실기를 포함하는 알칼리 화합물은 수산화 암모늄 및 암모니아를 포함하지 않는 것을 특징으로 하는 마스크 세정액 예비-조성물.Contains an alkali compound containing a hydroxyl group, an ammonium salt compound, an organic acid, and water, and has a use for use in combination with hydrogen peroxide or hydrogen peroxide solution,
The ammonium salt compound is at least one selected from the group consisting of ammonium acetate, ammonium nitrate, ammonium phosphate, monobasic ammonium phosphate, dibasic ammonium phosphate, ammonium sulfate and ammonium persulfate,
The mask cleaning liquid pre-composition, characterized in that the alkali compound containing a hydroxyl group does not contain ammonium hydroxide and ammonia.
(b) 암모늄염 화합물, 과산화수소, 및 물을 포함하는 마스크 세정액 예비-조성물을 제조하는 단계; 및
(c) 상기 (a)단계에서 제조된 예비-조성물과 (b)단계에서 제조된 예비-조성물을 혼합하는 단계;를 포함하고,
상기 암모늄염 화합물은 아세트산암모늄, 질산암모늄, 인산암모늄, 제1인산암모늄, 제2인산암모늄, 황산암모늄 및 과황산암모늄으로 이루어진 군으로부터 선택되는 1종 이상의 것이며,
상기 하이드록실기를 포함하는 알칼리 화합물은 수산화 암모늄 및 암모니아를 포함하지 않는 것을 특징으로 하는 마스크 세정액 조성물의 제조방법.(a) preparing a mask cleaning liquid pre-composition comprising an alkali compound containing a hydroxyl group, an organic acid, and water;
(b) preparing a mask cleaning liquid pre-composition comprising an ammonium salt compound, hydrogen peroxide, and water; and
(c) mixing the pre-composition prepared in step (a) and the pre-composition prepared in step (b);
The ammonium salt compound is at least one selected from the group consisting of ammonium acetate, ammonium nitrate, ammonium phosphate, monobasic ammonium phosphate, dibasic ammonium phosphate, ammonium sulfate and ammonium persulfate,
Method for producing a mask cleaning liquid composition, characterized in that the alkali compound containing the hydroxyl group does not contain ammonium hydroxide and ammonia.
(b) 상기 (a)단계에서 제조된 예비-조성물과 과산화수소 또는 과산화수소수를 혼합하는 단계;를 포함하고,
상기 암모늄염 화합물은 아세트산암모늄, 질산암모늄, 인산암모늄, 제1인산암모늄, 제2인산암모늄, 황산암모늄 및 과황산암모늄으로 이루어진 군으로부터 선택되는 1종 이상의 것이며,
상기 하이드록실기를 포함하는 알칼리 화합물은 수산화 암모늄 및 암모니아를 포함하지 않는 것을 특징으로 하는 마스크 세정액 조성물의 제조방법.(a) preparing a mask cleaning liquid pre-composition comprising an alkali compound containing a hydroxyl group, an ammonium salt compound, an organic acid, and water; and
(b) mixing the pre-composition prepared in step (a) with hydrogen peroxide or hydrogen peroxide;
The ammonium salt compound is at least one selected from the group consisting of ammonium acetate, ammonium nitrate, ammonium phosphate, monobasic ammonium phosphate, dibasic ammonium phosphate, ammonium sulfate and ammonium persulfate,
Method for producing a mask cleaning liquid composition, characterized in that the alkali compound containing the hydroxyl group does not contain ammonium hydroxide and ammonia.
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| CN115161650B (en) * | 2022-08-19 | 2024-05-10 | 福建省佑达环保材料有限公司 | Neutral metal cleaning agent for MASK MASK plate |
| KR20240033437A (en) | 2022-09-05 | 2024-03-12 | 재원산업 주식회사 | Composition for cleaning mask with increased stability to decomposition of hydrogen peroxide |
| KR20240033755A (en) | 2022-09-05 | 2024-03-13 | 재원산업 주식회사 | Cleaning composition for orgnic and inorganic materials on deposition mask used in deposition of organic light emitting display device |
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