CN109415798A - The cleaning method and flushing composition of the mask of vacuum evaporation - Google Patents
The cleaning method and flushing composition of the mask of vacuum evaporation Download PDFInfo
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- CN109415798A CN109415798A CN201880000486.5A CN201880000486A CN109415798A CN 109415798 A CN109415798 A CN 109415798A CN 201880000486 A CN201880000486 A CN 201880000486A CN 109415798 A CN109415798 A CN 109415798A
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- Prior art keywords
- cleaning
- mask
- composition
- hfe
- cleaning method
- Prior art date
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- 238000004140 cleaning Methods 0.000 title claims abstract description 128
- 238000000034 method Methods 0.000 title claims abstract description 89
- 239000000203 mixture Substances 0.000 title claims abstract description 69
- 238000011010 flushing procedure Methods 0.000 title claims abstract description 38
- 238000007738 vacuum evaporation Methods 0.000 title claims abstract description 19
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 66
- 238000004519 manufacturing process Methods 0.000 claims description 16
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 150000001408 amides Chemical class 0.000 claims description 3
- CWIFAKBLLXGZIC-UHFFFAOYSA-N 1,1,2,2-tetrafluoro-1-(2,2,2-trifluoroethoxy)ethane Chemical compound FC(F)C(F)(F)OCC(F)(F)F CWIFAKBLLXGZIC-UHFFFAOYSA-N 0.000 abstract description 19
- LMRGTZDDPWGCGL-UHFFFAOYSA-N 1,1,1,2,3,3-hexafluoro-3-(2,2,2-trifluoroethoxy)propane Chemical compound FC(F)(F)C(F)C(F)(F)OCC(F)(F)F LMRGTZDDPWGCGL-UHFFFAOYSA-N 0.000 abstract description 8
- YQQHEHMVPLLOKE-UHFFFAOYSA-N 1,1,2,2-tetrafluoro-1-methoxyethane Chemical compound COC(F)(F)C(F)F YQQHEHMVPLLOKE-UHFFFAOYSA-N 0.000 abstract description 8
- PCTQNZRJAGLDPD-UHFFFAOYSA-N 3-(difluoromethoxy)-1,1,2,2-tetrafluoropropane Chemical compound FC(F)OCC(F)(F)C(F)F PCTQNZRJAGLDPD-UHFFFAOYSA-N 0.000 abstract description 7
- 239000010410 layer Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 19
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 15
- 239000004615 ingredient Substances 0.000 description 15
- 239000007788 liquid Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 239000000758 substrate Substances 0.000 description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000003086 colorant Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 239000002585 base Substances 0.000 description 8
- -1 diphenyl naphthalene diamines Chemical class 0.000 description 8
- 235000019441 ethanol Nutrition 0.000 description 8
- 239000011521 glass Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000009835 boiling Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 4
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 4
- 230000006837 decompression Effects 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 239000002346 layers by function Substances 0.000 description 4
- 239000005416 organic matter Substances 0.000 description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CSUFEOXMCRPQBB-UHFFFAOYSA-N 1,1,2,2-tetrafluoropropan-1-ol Chemical compound CC(F)(F)C(O)(F)F CSUFEOXMCRPQBB-UHFFFAOYSA-N 0.000 description 2
- IBXNCJKFFQIKKY-UHFFFAOYSA-N 1-pentyne Chemical compound CCCC#C IBXNCJKFFQIKKY-UHFFFAOYSA-N 0.000 description 2
- MJBPUQUGJNAPAZ-UHFFFAOYSA-N Butine Natural products O1C2=CC(O)=CC=C2C(=O)CC1C1=CC=C(O)C(O)=C1 MJBPUQUGJNAPAZ-UHFFFAOYSA-N 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- HGCIXCUEYOPUTN-UHFFFAOYSA-N cyclohexene Chemical compound C1CCC=CC1 HGCIXCUEYOPUTN-UHFFFAOYSA-N 0.000 description 2
- LPIQUOYDBNQMRZ-UHFFFAOYSA-N cyclopentene Chemical compound C1CC=CC1 LPIQUOYDBNQMRZ-UHFFFAOYSA-N 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- RWRIWBAIICGTTQ-UHFFFAOYSA-N difluoromethane Chemical compound FCF RWRIWBAIICGTTQ-UHFFFAOYSA-N 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 2
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 2
- 230000000269 nucleophilic effect Effects 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 2
- 239000002798 polar solvent Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- OKIYQFLILPKULA-UHFFFAOYSA-N 1,1,1,2,2,3,3,4,4-nonafluoro-4-methoxybutane Chemical compound COC(F)(F)C(F)(F)C(F)(F)C(F)(F)F OKIYQFLILPKULA-UHFFFAOYSA-N 0.000 description 1
- RIQRGMUSBYGDBL-UHFFFAOYSA-N 1,1,1,2,2,3,4,5,5,5-decafluoropentane Chemical compound FC(F)(F)C(F)C(F)C(F)(F)C(F)(F)F RIQRGMUSBYGDBL-UHFFFAOYSA-N 0.000 description 1
- QVLAWKAXOMEXPM-UHFFFAOYSA-N 1,1,1,2-tetrachloroethane Chemical class ClCC(Cl)(Cl)Cl QVLAWKAXOMEXPM-UHFFFAOYSA-N 0.000 description 1
- XRKOOHTZZDPJNE-UHFFFAOYSA-N 1,1,1-trifluorohexane Chemical compound CCCCCC(F)(F)F XRKOOHTZZDPJNE-UHFFFAOYSA-N 0.000 description 1
- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical class ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N 1,1,2-trichloroethane Chemical class ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical class CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical class ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- HNAGHMKIPMKKBB-UHFFFAOYSA-N 1-benzylpyrrolidine-3-carboxamide Chemical compound C1C(C(=O)N)CCN1CC1=CC=CC=C1 HNAGHMKIPMKKBB-UHFFFAOYSA-N 0.000 description 1
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
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- OHMHBGPWCHTMQE-UHFFFAOYSA-N 2,2-dichloro-1,1,1-trifluoroethane Chemical compound FC(F)(F)C(Cl)Cl OHMHBGPWCHTMQE-UHFFFAOYSA-N 0.000 description 1
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 description 1
- ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 2,3-dimethylbutane Chemical group CC(C)C(C)C ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 0.000 description 1
- STTGYIUESPWXOW-UHFFFAOYSA-N 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline Chemical compound C=12C=CC3=C(C=4C=CC=CC=4)C=C(C)N=C3C2=NC(C)=CC=1C1=CC=CC=C1 STTGYIUESPWXOW-UHFFFAOYSA-N 0.000 description 1
- POXIZPBFFUKMEQ-UHFFFAOYSA-N 2-cyanoethenylideneazanide Chemical group [N-]=C=[C+]C#N POXIZPBFFUKMEQ-UHFFFAOYSA-N 0.000 description 1
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- COAUHYBSXMIJDK-UHFFFAOYSA-N 3,3-dichloro-1,1,1,2,2-pentafluoropropane Chemical compound FC(F)(F)C(F)(F)C(Cl)Cl COAUHYBSXMIJDK-UHFFFAOYSA-N 0.000 description 1
- ZNJRONVKWRHYBF-VOTSOKGWSA-N 4-(dicyanomethylene)-2-methyl-6-julolidyl-9-enyl-4h-pyran Chemical compound O1C(C)=CC(=C(C#N)C#N)C=C1\C=C\C1=CC(CCCN2CCC3)=C2C3=C1 ZNJRONVKWRHYBF-VOTSOKGWSA-N 0.000 description 1
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- DIVZFUBWFAOMCW-UHFFFAOYSA-N 4-n-(3-methylphenyl)-1-n,1-n-bis[4-(n-(3-methylphenyl)anilino)phenyl]-4-n-phenylbenzene-1,4-diamine Chemical compound CC1=CC=CC(N(C=2C=CC=CC=2)C=2C=CC(=CC=2)N(C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C=C(C)C=CC=2)C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C=C(C)C=CC=2)=C1 DIVZFUBWFAOMCW-UHFFFAOYSA-N 0.000 description 1
- SCZWJXTUYYSKGF-UHFFFAOYSA-N 5,12-dimethylquinolino[2,3-b]acridine-7,14-dione Chemical compound CN1C2=CC=CC=C2C(=O)C2=C1C=C1C(=O)C3=CC=CC=C3N(C)C1=C2 SCZWJXTUYYSKGF-UHFFFAOYSA-N 0.000 description 1
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- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 1
- IBHBKWKFFTZAHE-UHFFFAOYSA-N n-[4-[4-(n-naphthalen-1-ylanilino)phenyl]phenyl]-n-phenylnaphthalen-1-amine Chemical compound C1=CC=CC=C1N(C=1C2=CC=CC=C2C=CC=1)C1=CC=C(C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C3=CC=CC=C3C=CC=2)C=C1 IBHBKWKFFTZAHE-UHFFFAOYSA-N 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- QMMOXUPEWRXHJS-UHFFFAOYSA-N pent-2-ene Chemical group CCC=CC QMMOXUPEWRXHJS-UHFFFAOYSA-N 0.000 description 1
- BNIXVQGCZULYKV-UHFFFAOYSA-N pentachloroethane Chemical compound ClC(Cl)C(Cl)(Cl)Cl BNIXVQGCZULYKV-UHFFFAOYSA-N 0.000 description 1
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 1
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical group CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 1
- 229960004624 perflexane Drugs 0.000 description 1
- ZJIJAJXFLBMLCK-UHFFFAOYSA-N perfluorohexane Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F ZJIJAJXFLBMLCK-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- YYMBJDOZVAITBP-UHFFFAOYSA-N rubrene Chemical compound C1=CC=CC=C1C(C1=C(C=2C=CC=CC=2)C2=CC=CC=C2C(C=2C=CC=CC=2)=C11)=C(C=CC=C2)C2=C1C1=CC=CC=C1 YYMBJDOZVAITBP-UHFFFAOYSA-N 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- TVIVIEFSHFOWTE-UHFFFAOYSA-K tri(quinolin-8-yloxy)alumane Chemical compound [Al+3].C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1 TVIVIEFSHFOWTE-UHFFFAOYSA-K 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000005406 washing Methods 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
- C11D7/28—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3263—Amides or imides
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3281—Heterocyclic 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
- C11D7/50—Solvents
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/04—Coating on selected surface areas, e.g. using masks
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/04—Coating on selected surface areas, e.g. using masks
- C23C14/042—Coating on selected surface areas, e.g. using masks using masks
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
- C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
- H10K71/166—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering using selective deposition, e.g. using a mask
-
- C11D2111/22—
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
- H10K71/164—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering using vacuum deposition
Abstract
Cleaning method, this method is the cleaning method of the mask of vacuum evaporation, wherein with containing selected from n-methyl-2-pyrrolidone and N, at least one kind of cleaning combination of dinethylformamide cleans mask, is rinsed with the flushing composition containing at least one kind of hydrofluoroether selected from HFE-347pc-f, HFE-254pc, HFE-356pcf and HFE-449mec-f to the mask after cleaning.In the cleaning method, in the cleaning of mask used in vacuum evaporation process when organic EL element manufactures, when rinsing cleaning combination, cleaning masks can be obtained in the Undec situation of effective component extremely clean.
Description
Technical field
Method (Japanese: is cleaned) the present invention relates to the cleaning of the mask of vacuum evaporation and rinses (Japanese: リ Application ス) combination
Object.
Background technique
In recent years, it is attracted attention as flat-panel monitor, liquid crystal display device or the display device for having organic EL element.
The power consumption of liquid crystal display device is few, but in order to obtain bright picture, needs exterior lighting (backlight).In this regard, having
The organic EL element of the display device of organic EL element is the element of emissive type, therefore does not need as liquid crystal display device
Backlight.Therefore, have the display device of organic EL element while with power saving features, also there is high luminance and wide viewing angle
Feature.
Organic EL element has the functional layer containing the luminescent layer being made of organic compound between anode and cathode.As
The method for forming this functional layer, it is known to which the vapor phase methods such as vacuum vapour deposition (also referred to as dry method) use functional layer forming material
Solution obtained by being dissolved or dispersed in solvent liquid phase method (also referred to as wet process or rubbing method) (referring for example to patent document 1~
3)。
In the case where forming functional layer by vacuum evaporation, make mask close to substrate, via mask to cathode, hole (day
Text: positive hole) implanted layer, hole transporting layer, luminescent layer, each layer of electron supplying layer, anode carry out pattern and formed.The spy used at this time
Be not the fine pattern for RGB layer vapor deposition it is very accurate with mask, therefore, it is difficult to manufacture and very expensive.But
During the pattern of the organic layer of organic EL element is formed, it is deposited if same mask is used for multiple times, organic matter is on mask
It accumulates and adheres to, accurate mask pattern accurately can not be transferred to substrate.Therefore, in order to realize the mask artwork of high-precision
Case, it has to which the expensive mask of discarded use for several times, this is one of the reason of be difficult to volume production from the aspect of production cost.
Then, it has attempted to propose by Reusability mask to reduce cost for cleaning organic EL element manufacture
The cleaning liquid composition of the various organic matters of mask is attached in vacuum evaporation process (for example, referring to patent document 4).
It describes in patent document 4 after having cleaned mask with cleaning liquid composition, is rinsed with hydrofluoroether.But specially
" ノ ベ ッ Network the HFE7100 " (C used in sharp document 4 as flushing liquor4F9OCH3) for example in n-methyl-2-pyrrolidone and N,
It can be decomposed in the presence of dinethylformamide and generate fluorine ion (for example, referring to patent document 5).Therefore, the above method is sometimes
Mask surface can not be cleaned up.
Existing technical literature
Patent document
Patent document 1: Japanese Patent Laid-Open 2002-110345 bulletin
Patent document 2: Japanese Patent Laid-Open 2002-305079 bulletin
Patent document 3: Japanese Patent Laid-Open 2002-313564 bulletin
Patent document 4: Japanese Patent Laid-Open 2005-162947 bulletin
Patent document 5: Japanese patent special table 2009-518857 bulletin
Summary of the invention
The technical problems to be solved by the invention
The present invention completes the vacuum evaporation, and it is an object of the present invention to provide when for example organic EL element manufactures in order to solve the above problem
The cleaning method and flushing composition of mask used in process, wherein cleaned with the cleaned composition of composition flushing is rinsed
When the mask crossed, cleaning masks can be obtained in the Undec situation of effective component for rinsing composition extremely clean.
Technical scheme applied to solve the technical problem
The cleaning method of embodiment is the cleaning method of the mask of vacuum evaporation, wherein with containing selected from N- methyl-
2-Pyrrolidone (NMP) and at least one kind of cleaning combination of n,N-Dimethylformamide (DMF) clean mask, are selected with containing
From CF3CH2-O-CF2CHF2(HFE-347pc-f)、CHF2CF2-O-CH3(HFE-254pc)、CHF2-O-CH2CF2CHF2(HFE-
356pcf) and CF3CHFCF2-O-CH2CF3(HFE-449mec-f) after the flushing composition of at least one kind of hydrofluoroether is to cleaning
Mask is rinsed.
In the cleaning method of embodiment, the ratio of the content for rinsing the hydrofluoroether in composition is preferably 80
Quality % or more 100 mass % or less.
In the cleaning method of embodiment, cleaning combination preferably comprises n-methyl-2-pyrrolidone.
In the cleaning method of embodiment, rinses composition and preferably comprise CF3CH2-O-CF2CHF2。
In the cleaning method of embodiment, the cleaning and flushing of mask are preferably carried out at 10 DEG C or more 40 DEG C or less, more
It is preferred that being carried out at 20 DEG C or more 30 DEG C or less.
In the cleaning method of embodiment, vacuum evaporation is preferably carried out in the manufacture of low molecule type organic EL element.
In the cleaning method of embodiment, the mask after being rinsed by flushing composition is preferably dried.
The flushing composition of embodiment is to containing selected from n-methyl-2-pyrrolidone and N,N-dimethylformamide
The flushing composition that is rinsed of the mask of vacuum evaporation that cleaned of at least one kind of cleaning combination, containing being selected from
CF3CH2-O-CF2CHF2、CHF2CF2-O-CH3、CHF2-O-CH2CF2CHF2And CF3CHFCF2-O-CH2CF3At least one kind of hydrogen fluorine
Ether.
In the flushing composition of embodiment, the ratio of the content of the hydrofluoroether 100 matter preferably more than 80 mass %
Measure % or less.
In addition, in the present specification, the abbreviation of compound is remembered in the bracket after chemical combination name sometimes, as needed
Using its abbreviation to replace chemical combination name.In addition, the symbol of "~" in this specification indicate the numerical value recorded before it with
Numerical value range below that is upper and recording after which.
Invention effect
Pass through the cleaning method and flushing composition of present embodiment, such as the vacuum evaporation in organic EL element manufacture
In the cleaning of mask used in process, when being rinsed with the mask that flushing composition cleaned cleaned composition, energy
It is enough cleaning masks are obtained in the Undec situation of effective component for rinsing composition it is extremely clean.
Detailed description of the invention
Fig. 1 is the figure for illustrating the manufacturing method of organic EL display device.
Fig. 2 is the figure for showing schematically the mode that luminescent layer is formed via mask.
Specific embodiment
In the following, referring to attached drawing, detailed description of embodiments of the present invention.
The cleaning method of present embodiment is for example for cleaning in the vacuum evaporation process in organic EL element manufacture
The method of used mask, including cleaning process, flushing process and drying process.In the cleaning method of present embodiment,
It is combined in cleaning process using containing at least one kind of cleaning selected from n-methyl-2-pyrrolidone and N,N-dimethylformamide
Object cleans mask.Then, in rinsing process, by containing selected from HFE-347pc-f, HFE-254pc, HFE-356pcf and
The flushing composition of at least one kind of hydrofluoroether of HFE-449mec-f is rinsed the mask after being cleaned with cleaning combination.
Later, implement drying process as needed, mask is dry.
In the cleaning method of present embodiment, even if rinsing the above-mentioned specific hydrofluoroether contained in composition in cleaning group
It is also not easily decomposed in the presence of n-methyl-2-pyrrolidone and N,N-dimethylformamide in conjunction object.Therefore, even if cleaning
In the case that composition remains on the mask after cleaning, the above-mentioned specific hydrofluoroether rinsed in composition will not be because of cleaning group
It closes object and decomposes, do not generate fluorine ion.Therefore, mask surface can be cleaned extremely clean.
The mask of the cleaning object of cleaning method as present embodiment is, for example, to show in organic EL described below
Mask used in the vacuum evaporation process of the manufacturing process of device.
Hereinafter, for the manufacturing method of organic EL display device, the vacuum evaporation to mask has been used referring to Figures 1 and 2
Process is briefly described.TFT (thin film transistor (TFT)) and transparent electrode are formed on the glass substrate, are further formed cavity conveying
Layer.The glass substrate 1 of the TFT, transparent electrode and hole transporting layer is formed with the processed surface of glass substrate 1 side directed downwardly
Formula is carried in vacuum chamber.In vacuum chamber, in formation luminescent layer corresponding with each primary colors R, G, B on glass substrate 1
As colour display device.The process carries out in the separate chamber corresponding with each primary colors R, G, B as colour display device.
It is used to form the vacuum chamber of luminescent layer corresponding with primary colors R that is, glass substrate 1 is successively carried to, is used to form and primary colors G
The vacuum chamber of corresponding luminescent layer and the vacuum chamber for being used to form luminescent layer corresponding with primary colors B.
In each vacuum chamber, mode as shown in Figure 1 is provided in advance to be covered with the shape of luminescent layer matched opening
Mould 20.The mask 20 is fixed by the mask frame 21 being configured in holding station 24.
It is corresponding with each primary colors of R, G, B as mask 20 in each vacuum chamber, be equipped with only with for defined original
The mask of the luminous corresponding outs open of transparent electrode (anode) 11 of color.It can be respectively in predetermined bits whereby in each chamber
It sets to form luminescent layer corresponding with each primary colors.
In Fig. 1, from material (organic EL material of the evaporation source (source) 30 for the lower section for being configured at holding station 24 heating luminescent layer
Material) and be allowed to evaporate, so that same material is deposited on 1 surface of glass substrate in the opening portion via mask.Fig. 2 shows schematically Jie
By the generation type of the luminescent layer of the mask 20.As shown in Fig. 2, in each transparent electrode (anode) 11, in each chamber in addition to this
20 coverings are masked other than the forming region of the corresponding transparent electrode of primary colors.Then, organic EL Material corresponding with the primary colors
It is heated and gasifies in source 30, be deposited that be formed in glass substrate 1 (be it for accurate via the opening portion 20h of mask 20
Hole transporting layer) on.In addition, the material as mask, alloy (such as the Fe-Ni of the stainless steels such as SUS, Ni simple substance, Ni can be enumerated
Alloy, Mg-Ni alloy) or the semiconductors such as silicon etc..
In the vapor deposition process, the various organic matters being made of evaporation material are attached to mask.As evaporation material, in addition to upper
It states except organic EL Material, can also enumerate hole-injecting material, hole transporting material, the electricity used when manufacturing organic EL element
Son conveying material etc..As hole-injecting material, copper phthalocyanine (CuPC), poly- (3,4- ethylene dioxy thiophene phenol) (PEDOT) can be enumerated
With compound (PEDOT/PSS), 4,4 ' of polystyrolsulfon acid (PSS), 4 ' '-three [phenyl (tolyl) amino] triphenylamine
(m-MTDATA) etc..As hole transporting material, triphen amine (TPD), diphenyl naphthalene diamines (α-NPD), three can be enumerated
(4- carbazyl -9- base phenyl) amine (TCTA) etc..As organic EL Material, bis styryl benzene derivatives, three (8- hydroxyls can be enumerated
Base quinoline) aluminium (Alq3), bis- [2- (2- benzoxazolyl) phenol] zinc (II) (Zn-PBO), rubrene, dimethylquinacridone, N,
N '-dimethyl quinacridone (DMQ), 4- (dicyano methylene) -2- methyl -6- [2- (2,3,6,7- tetrahydro -1H, 5H- benzo
[ij] quinolizine -9- base) vinyl] -4H- pyrans (DCM2) etc..As electron transport materials, Alq can be enumerated3, 2,9- dimethyl-
4,7- diphenyl -1,10- phenanthroline (BCP), 2- phenyl -5- (4- xenyl) -1,3,4- oxadiazole compound (PBD), thiophene are coughed up
Derivative etc..
In the cleaning process of the cleaning method of present embodiment, by containing selected from n-methyl-2-pyrrolidone and N, N-
At least one kind of cleaning combination of dimethylformamide cleans the organic matter for being attached to the mask.As cleaning method,
Have the method for impregnating mask in cleaning combination, sprayed cleaning combination to the method for mask by injection water etc..Separately
Outside, when cleaning mask, also can be used in combination ultrasonic cleaning, can be improved solvability whereby and shortens scavenging period.From
From the point of view of cleaning, cleaning combination used in cleaning process preferably comprises n-methyl-2-pyrrolidone.
N- methyl-from the point of view of it can sufficiently clean mask, in cleaning combination used in cleaning process
The content ratio of 2-Pyrrolidone or n,N-Dimethylformamide is preferably 80~100 mass %, more preferably 95~100 matter
Measure %, further preferably 98~100 mass %.Cleaning combination contains n-methyl-2-pyrrolidone and N, N- dimethyl methyl
In the case where amide the two, from the point of view of it sufficiently can clean mask, total content ratio of the two is preferably located
In above-mentioned preferred scope.
Within the scope of the effect without prejudice to the mode of implementation, cleaning combination can also be containing except N- methyl -2- pyrrolidines
Ingredient other than ketone and N,N-dimethylformamide.This ingredient can enumerate such as pentane, hexane, heptane, octane, nonane, ring
The saturated hydrocarbons such as butane, pentamethylene, hexamethylene, hexamethylene, 1- butylene, 2- butylene, 2- metering system, 1- amylene, 2- amylene, 1-
The unsaturation hydro carbons such as butine, 2- butine, pentyne, cyclopropylene, cyclobutane, cyclopentene, cyclohexene, it is methanol, ethyl alcohol, normal propyl alcohol, different
The alcohols such as propyl alcohol, n-butanol, isobutanol, sec-butyl alcohol, the tert-butyl alcohol, dimethyl ether, ethyl-methyl ether, Anaesthetie Ether, diisopropyl
The ethers such as ether, methyl t-butyl ether, four fluoroethanols, acetone, methyl ethyl ketone, diethyl ketone, methyl acetone, methylisobutylketone, ring penta
The ketones such as ketone, cyclohexanone, methyl formate, Ethyl formate, propyl formate, methyl acetate, ethyl acetate, propyl acetate, butyric acid first
The esters such as ester, ethyl butyrate, gamma-butyrolacton, the amines such as monomethylamine, dimethylamine, trimethylamine, methylene chloride, 1,1- dichloroethanes,
1,2- dichloroethanes, 1,1,2- trichloroethanes, 1,1,1,2- tetrachloroethanes, 1,1,2,2- tetrachloroethanes, pentachloroethane, 1,1- bis-
Vinyl chloride, cis- -1,2- dichloroethylene, anti-form-1, the chlorine such as 2- dichloroethylene, trichloro ethylene, tetrachloro-ethylene, 1,2- dichloropropane
For hydro carbons, 1,1,1,3,3- 3-pentafluorobutane, 1,1,1,2,2,3,4,5,5,5- Decafluoropentane, 1,1,2,2,3,3,4- seven fluorine ring penta
Alkane, nine fluorine hexane of 1,1,1,2,2,3,3,4,4-, ten trifluorohexane of 1,1,1,2,2,3,3,4,4,5,5,6,6-, 1,1,1,2,2,
HFC (hydrofluorocarbon) classes such as 3,3,4,4,5,5,6,6- ten three fluoro-octanes, ten fluorine butane, R-4112, Tetradecafluorohexane, 16
Fluorine heptane, ten octafluoro octanes etc. PFC (perfluoroparaffin) class, dichloro pentafluoropropane, the chloro- 1- fluoroethane of 1,1- bis-, chloro- 1, the 1- difluoro of 1-
Ethane, 2,2- bis- chloro- 1,1,1- trifluoroethane etc. HCFC (hydrochlorofluorocarbons) class etc., but not limited to this.In addition, these ingredients can be single
Solely contain, can also contain there are many.
Cleaning combination contains the case where ingredient in addition to n-methyl-2-pyrrolidone and N,N-dimethylformamide
Under, the content ratio of these ingredients is preferably in 20 mass % hereinafter, more preferably in 5 mass % hereinafter, further preferably in 2 matter
Measure % or less.The ingredient in addition to n-methyl-2-pyrrolidone and N,N-dimethylformamide contained in cleaning combination
It can be the ingredient without cleaning effect among the above.If moisture can be attached in addition, cleaning combination contains moisture
Mask surface generates stain (Japanese: body) sometimes, and the cleaning force of solvent compositions reduces, therefore water in cleaning combination
Content preferably in 5 mass % hereinafter, more preferably in 3 mass % hereinafter, further preferably below 1 mass %.Particularly preferably
It is not aqueous in cleaning combination.
The time for implementing cleaning process is different because of the size of mask and the type of the organic matter of attachment and amount etc., for example,
5~15 minutes.The temperature of cleaning combination about cleaning process is adjusted to room temperature, preferably 10 without temperature
~40 DEG C, further preferably 20~30 DEG C.As such, using containing selected from n-methyl-2-pyrrolidone and N, N- dimethyl methyl
At least one kind of cleaning combination of amide is cleaned with above-mentioned temperature range, will not be because of cleaning while cleaning is excellent
When thermal conductivity cause mask deformation and distortion etc..
In addition, in cleaning process, just can will be only attached to above-mentioned cleaning combination a kind of various mask surfaces or
Organic matter of more than two kinds sufficiently removes.It therefore, there is no need to select different rinse baths according to the type of cleaning solution, as a result make
It is very easy to obtain cleaning process.
In addition, cleaning combination reuses after capable of distilling used cleaning liquid composition.Cleaning liquid composition contains
It, also can be by using in the case where having the ingredient in addition to n-methyl-2-pyrrolidone and n,N-Dimethylformamide
Cleaning liquid composition be distilled to recover obtained by liquid composition could be adjusted to realize recycle.
In the flushing process of the cleaning method of present embodiment, cleaned with flushing composition flushing with cleaning combination
Mask.In this specification, flushing refers to, the cleaning combination adhered on the mask cleaned with cleaning combination is removed.
As the method being rinsed to the mask after cleaning, it can enumerate and the mask after cleaning is impregnated in flushing composition
Method, with rinsing the method for mask etc. after composition flush clean.No matter can be easily removed clear with any method
The cleaning combination of mask surface attachment after washing, can rinse mask surface extremely clean.Implement rinse process when
Between it is different because of size of mask etc., for example, 5~15 minutes.The temperature of flushing composition about flushing process, without
Temperature is adjusted to room temperature, preferably 10~40 DEG C, further preferably 20~30 DEG C.As such, can be with lower temperature
It is rinsed, mask deformation and distortion etc. will not be caused by thermal conductivity.
It rinses composition and contains the hydrogen selected from HFE-347pc-f, HFE-254pc, HFE-356pcf and HFE-449mec-f
At least one kind of of fluorine ether is used as effective component.The boiling of HFE-347pc-f, HFE-254pc, HFE-356pcf and HFE-449mec-f
Point is 74 DEG C of low values below, and drying property is excellent, is also easy evaporation at room temperature.In addition, even if boiling forms steam, also not
The component being affected by the heat easily easy to resin component etc. causes adverse effect.Rinse composition can be used alone a kind it is above-mentioned
Hydrofluoroether can also be applied in combination with two or more.
The Ozone Depletion Potential of HFE-347pc-f is 0, and chamber effect potential value is low.The boiling point of HFE-347pc-f is about
56℃.HFE-347pc-f can be for example, by aprotic polar solvent and catalyst (alkali metal alcoholates or alkali metal hydroxide
Object) in the presence of react 2,2,2 tfifluoroethyl alcohol with tetrafluoroethene method (referring to International Publication No. 2004/108644)
To manufacture.
As the commercially available product of HFE-347pc-f, such as " ア サ ヒ Network リ Application (registered trademark) AE-3000 " (rising sun nitre can be enumerated
Sub- Co., Ltd. (Asahi Glass society) system).
The Ozone Depletion Potential of HFE-254pc is 0, and chamber effect potential value is low.The boiling point of HFE-254pc is 37 DEG C.
HFE-254pc can for example be made by adding the method for tetrafluoroethene into the methanol coexisted with highly basic (such as sodium hydroxide)
It makes.
The Ozone Depletion Potential of HFE-356pcf is 0, and chamber effect potential value is low.The boiling point of HFE-356pcf is 74
℃.HFE-356pcf for example can be by adding a chlorine into the tetrafluoropropanol (TFPO) coexisted with highly basic (such as sodium hydroxide)
The method of difluoromethane (HCFC-22) manufactures.
The Ozone Depletion Potential of HFE-449mec-f is 0, and chamber effect potential value is low.The boiling point of HFE-449mec-f is
73℃.HFE-449mec-f can be for example, by aprotic polar solvent and catalyst (alkali metal alcoholates or alkali metal hydrogen-oxygen
Compound) in the presence of react 2,2,2 tfifluoroethyl alcohol with hexafluoropropene method (referring to Japanese Patent Laid-Open 9-263559
Number) manufacture.
N-methyl-2-pyrrolidone and N,N-dimethylformamide in cleaning combination liquidate any in cleaning composition
Kind hydrofluoroether all has excellent dissolubility.Therefore, cleaning combination easily passes through flushing composition and is removed.In addition, cleaning
The n-methyl-2-pyrrolidone and N,N-dimethylformamide contained in composition will not be such that above-mentioned hydrofluoroether decomposes.Therefore,
Mask surface after flushing does not have fluorine ion residual, can obtain cleaning masks extremely clean.
Herein, the n-methyl-2-pyrrolidone and n,N-Dimethylformamide contained in cleaning combination will not make to rush
The reason of hydrofluoroether used in cleaning composition is decomposed presumption is as follows.
For example, as methyl-perfluor n-butyl ether (C4F9OCH3, HFE-449sl) such there is strong electron-withdrawing CF3Base
Hydrofluoroether class CF3The electron deficiency for the carbon of base being combined.CF3The carbon of base being combined is combined with halogen atom etc. and is easy
Nucleophilic attack in the case where the atom or atomic group of disengaging, by n-methyl-2-pyrrolidone and n,N-Dimethylformamide
And it is easy to decompose.In contrast, the hydrofluoroether in flushing composition used in present embodiment does not have CF3Base, or i.e.
Make with CF3Base, CF3Also the atom or atomic group being easily separated from are not associated on the carbon that base is combined.Therefore, the electricity of intramolecular
Lotus is not susceptible to deviate, and is not easily susceptible to the nucleophilic attack from n-methyl-2-pyrrolidone and n,N-Dimethylformamide.
Composition is rinsed used in cleaning method as present embodiment, from can sufficiently remove cleaning combination
From the point of view of angle and drying property are excellent, HFE-347pc-f is preferably comprised.
From the point of view of it sufficiently can rinse mask, in flushing composition used in the cleaning method of present embodiment
The content ratio of above-mentioned hydrofluoroether be preferably 80~100 mass %, more preferably 95~100 mass %, further preferably
98~100 mass %.It rinses in the case that composition contains above-mentioned hydrofluoroether of more than two kinds, from can sufficiently rinse mask
Angle considers that total content ratio is preferably in above-mentioned preferred scope.
Rinsing composition can be within the scope of the effect of the invention containing the ingredient in addition to above-mentioned hydrofluoroether.
As the ingredient other than above-mentioned hydrofluoroether, can enumerate for example with except in above-mentioned cleaning combination n-methyl-2-pyrrolidone and
The same ingredient of ingredient other than n,N-Dimethylformamide, but not limited to this.In addition, these ingredients can individually contain, it can also
Containing there are many.
In the case that flushing composition contains the ingredient in addition to above-mentioned hydrofluoroether, the content ratio of these ingredients preferably exists
20 mass % are hereinafter, more preferably in 5 mass % hereinafter, further preferably below 2 mass %.
If moisture is attached to mask surface sometimes as described above, cleaning combination contains moisture, stain is formed.
Rinse composition contain selected from methanol, ethyl alcohol, normal propyl alcohol, isopropanol at least one kind of alcohol in the case where, even if in cleaning combination
In the case where containing moisture, also the moisture can be made to dissolve and removed, therefore preferably.Rinse the case where composition contains above-mentioned alcohol
Under, from can sufficiently dewatered angle consider, rinse the content ratio of the alcohol in composition preferably in 10 mass % hereinafter,
More preferably 1~8 mass %, further preferably 2~5 mass %.
In the drying process of the cleaning method of present embodiment, the mask after rinsing process and rinsing is dried.It is dry
Drying method can be used by spontaneously dry by method that the mask after flushing is dried, by method that air-flow is dried, pass through
Depressurize the method etc. being dried.Wherein, it from the point of view of it efficiently can dry mask, is preferably dried by decompression
Method.
It in the method being dried by air-flow, such as can be preferably 10~40 DEG C, more preferably 20~30 by injection
DEG C dry air be dried.As such, can be dried with lower temperature, mask deformation and distortion will not be caused by thermal conductivity
Deng.
Since decompression expends the time, the degree of decompression by pressure when being dried under reduced pressure mask is the smaller the better.Wherein, such as
Adhesion amount of the fruit flushing composition on mask is few, then can dry in decompression process, therefore can be according to the size of mask
Or it rinses adhesion amount of the composition on mask and is appropriately configured, such as be preferably set to rinse 20 DEG C of steam of composition
In the range for pressing the above 101.3kPa or less.For example, in the case where flushing composition is made of HFE-347pc-f, in drying
The pressure of 25~101.3kPa is preferably decompressed in process.
Using the cleaning method of embodiments described above, it is used as by using specific hydrofluoroether and rinses composition,
The n-methyl-2-pyrrolidone and N,N-dimethylformamide being attached in the cleaning combination of mask when cleaning will not make hydrogen
Fluorine ether decomposes, and will not generate fluorine ion.Therefore, cleaning masks can be obtained extremely clean.The cleaning method of present embodiment can
The cleaning method of mask when as by vacuum vapour deposition manufacture organic EL element, is preferred for manufacturing low molecule type EL element
When vacuum evaporation process.
Embodiment
Test example and embodiment are illustrated below.The present invention is not limited to these test examples and embodiments.
(test example 1)
In this test example to being heated with the stipulated time in the case where NMP and DMF liquidate cleaning composition decomposability into
Research is gone.The NMP or DMF, similarly of 5 mass % are added to HFE-347pc-f (Asahi Glass Co., Ltd's system, AE-3000)
To HFE-449sl ((ス リ ー エ system society, 3M company) system, Novec7100) addition 5 mass % NMP or DMF, be prepared for sample
Liquid.Each test liquid 3 days have been stood in 55 DEG C of thermostat.With fluoride ion determinator (DKK Toa Corp. (eastern Ami デ ィ
ー ケ ー ケ ー society) system, IM-55G, fluoride ion electrode: DKK Toa Corp.'s system, F-2021) determine stand after it is each molten
Fluorinion concentration in agent test liquid.In addition, the detectable limit of fluorinion concentration is 0.5ppm.As a result shown in table 1.
[table 1]
(test example 2)
In this test example, as accelerated test, having studied makes containing HFE-347pc-f's or HFE-449sl and NMP
The decomposability as caused by NMP of flushing composition of the test liquid when being heated to reflux.To HFE-347pc-f similar to the above
NMP of 5 mass % of addition in (Asahi Glass Co., Ltd's system, AE-3000), is added flask for resulting 250g test liquid, with adding
Hot device is heated to fluidized state, has carried out reflux in 4 hours.Then it with the distillate of 80 minutes acquisition 175g, determines remaining
Distillation still extraction raffinate (Japanese: kettle raffinate) pH, fluorinion concentration and sour component.As a result it is shown in table 2.
In addition, the NMP of 5 mass % is added into HFE-449sl similar to the above (3M corporation, Novec7100), it will
Flask is added in resulting 250g test liquid, is allowed to boil with heater heating, has carried out reflux in 4 hours.Then with 80 points
Clock acquires the distillate of 175g, determines pH, fluorinion concentration and the sour component of remaining distillation still extraction raffinate.In addition, the survey of pH
Surely by pH analyzer (DKK Toa Corp.'s system, HM-25R, electrode: DKK Toa Corp.'s system, GST-5741C) into
The measurement of row, fluorinion concentration passes through fluoride ion determinator (DKK Toa Corp.'s system, IM-55G, fluoride ion electrode: East Asia
DKK Co. Ltd. system, F-2021) it carries out, the measurement of sour component is carried out using phenolphthalein as indicator by titration.Fluorinion concentration and
The detectable limit of sour component is 0.5ppm.As a result it is shown in table 2.
[table 2]
Even if being rinsed in composition it is found that having carried out heating in 3 days or 80 minutes are heated to reflux by table 1, table 2
HFE-347pc-f is not also because NMP or DMF is decomposed, and not formed fluorine ion, in contrast, HFE-449sl is divided due to NMP or DMF
Solution produces fluorine ion.
(embodiment)
To use HFE-347pc-f as composition is rinsed in the case where the cleaning of made of metal mask ground
Study carefully.Metal (SUS) piece for being attached with low molecule type organic EL Material is impregnated 1 minute in the NMP of room temperature (25 DEG C).Then,
Sheet metal is impregnated to 1 minute in the HFE-347pc-f (Asahi Glass Co., Ltd's system, AE-3000) of room temperature (25 DEG C) to carry out
It rinses, then lifts.The sheet metal is spontaneously dried, is then impregnated in pure water, with fluoride ion determinator (East Asia DKK plants of formula
Commercial firm's system, IM-55G, fluoride ion electrode: DKK Toa Corp.'s system, F-2021) determine the fluorinion concentration extracted.Separately
Outside, the detectable limit of fluorinion concentration is 0.5ppm.The case where its result is detected fluorine ion is " detecting ", does not detect
To the case where be " not detecting ", be shown in table 3.
(comparative example)
To use HFE-449sl as composition is rinsed in the case where the cleaning of made of metal mask studied.
After metal (SUS) piece for being attached with low molecule type organic EL Material is impregnated 1 minute in the NMP of room temperature (25 DEG C), in room temperature
Dipping 1 minute, is rinsed whereby, then lifts in the HFE-449s1 (3M corporation, Novec7100) of (25 DEG C).By the gold
Belong to piece to spontaneously dry, is then impregnated in pure water, whether investigated has the fluorine ion extracted.The results are shown in tables 3.
[table 3]
| Rinse composition | Evaluation result | |
| Embodiment | HFE-347pc-f | It does not detect |
| Comparative example | HFE-449sI | It detects |
It as shown in Table 3, can be clean by cleaning masks by using HFE-347pc-f as composition is rinsed.Compared to it
Under, it is known that when using HFE-449s1, mask surface is attached with fluorine ion, can not be clean by cleaning masks.
Symbol description
1 ... glass substrate, 11 ... transparent electrodes, 20 ... masks, the opening portion 20h ..., 21 ... mask frames, 24 ... holding station,
30 ... sources.
Claims (10)
1. cleaning method, it is the cleaning method of the mask of vacuum evaporation, which is characterized in that
Institute is cleaned with containing at least one kind of cleaning combination selected from n-methyl-2-pyrrolidone and N,N-dimethylformamide
Mask is stated,
With containing selected from CF3CH2-O-CF2CHF2、CHF2CF2-O-CH3、CHF2-O-CH2CF2CHF2And CF3CHFCF2-O-CH2CF3
The flushing composition of at least one kind of hydrofluoroether the mask after cleaning is rinsed.
2. cleaning method as described in claim 1, which is characterized in that the content for rinsing the hydrofluoroether in composition
Ratio more than 80 mass % 100 mass % or less.
3. cleaning method as claimed in claim 1 or 2, which is characterized in that the cleaning combination contains N- methyl -2- pyrroles
Alkanone.
4. cleaning method according to any one of claims 1 to 3, which is characterized in that the flushing composition contains
CF3CH2-O-CF2CHF2。
5. cleaning method as described in any one of claims 1 to 4, which is characterized in that the cleaning and flushing of the mask are equal
It is carried out at 10 DEG C or more 40 DEG C or less.
6. such as cleaning method according to any one of claims 1 to 5, which is characterized in that the cleaning and flushing of the mask are equal
It is carried out at 20 DEG C or more 30 DEG C or less.
7. such as cleaning method according to any one of claims 1 to 6, which is characterized in that the vacuum evaporation is in low molecule type
It is carried out in the manufacture of organic EL element.
8. such as cleaning method according to any one of claims 1 to 7, which is characterized in that rinsed to the flushing composition
Mask afterwards is dried.
9. rinsing composition, the composition is for rinsing by containing selected from n-methyl-2-pyrrolidone and N, N- dimethyl methyl
The flushing composition for the vacuum evaporation mask that at least one kind of cleaning combination of amide cleaned, which is characterized in that
Containing selected from CF3CH2-O-CF2CHF2、CHF2CF2-O-CH3、CHF2-O-CH2CF2CHF2And CF3CHFCF2-O-CH2CF3's
At least one kind of hydrofluoroether.
10. rinsing composition as claimed in claim 9, which is characterized in that the hydrofluoroether rinsed in composition
The ratio of content 100 mass % or less more than 80 mass %.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2017124086 | 2017-06-26 | ||
| JP2017-124086 | 2017-06-26 | ||
| PCT/JP2018/016296 WO2019003605A1 (en) | 2017-06-26 | 2018-04-20 | Method for washing mask for vacuum vapor deposition and rinsing composition |
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| Publication Number | Publication Date |
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| CN109415798A true CN109415798A (en) | 2019-03-01 |
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| Country | Link |
|---|---|
| JP (1) | JP6849064B2 (en) |
| KR (1) | KR102478194B1 (en) |
| CN (1) | CN109415798A (en) |
| SG (1) | SG11201913385UA (en) |
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Cited By (2)
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|---|---|---|---|---|
| CN110846154A (en) * | 2019-08-30 | 2020-02-28 | 安徽富乐德科技发展有限公司 | Plate-attachment-preventing cleaning agent for OLED organic evaporation equipment and application |
| CN111172550A (en) * | 2020-02-14 | 2020-05-19 | 福建省佑达环保材料有限公司 | OLED mask cleaning agent and cleaning process thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116926466A (en) * | 2019-03-15 | 2023-10-24 | 凸版印刷株式会社 | Evaporation mask intermediate |
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Also Published As
| Publication number | Publication date |
|---|---|
| KR102478194B1 (en) | 2022-12-15 |
| JPWO2019003605A1 (en) | 2020-04-23 |
| SG11201913385UA (en) | 2020-01-30 |
| WO2019003605A1 (en) | 2019-01-03 |
| TWI781168B (en) | 2022-10-21 |
| TW201905191A (en) | 2019-02-01 |
| KR20200021444A (en) | 2020-02-28 |
| JP6849064B2 (en) | 2021-03-24 |
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