CN101678658A - 透明导电层及其制备方法 - Google Patents
透明导电层及其制备方法 Download PDFInfo
- Publication number
- CN101678658A CN101678658A CN200880020373A CN200880020373A CN101678658A CN 101678658 A CN101678658 A CN 101678658A CN 200880020373 A CN200880020373 A CN 200880020373A CN 200880020373 A CN200880020373 A CN 200880020373A CN 101678658 A CN101678658 A CN 101678658A
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- CN
- China
- Prior art keywords
- acid
- ammonium
- group
- silver
- chemical formula
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000002360 preparation method Methods 0.000 title description 7
- 239000010410 layer Substances 0.000 claims abstract description 85
- 238000000034 method Methods 0.000 claims abstract description 60
- 150000007524 organic acids Chemical class 0.000 claims abstract description 35
- 229910052751 metal Inorganic materials 0.000 claims abstract description 33
- 239000002184 metal Substances 0.000 claims abstract description 33
- 229910052709 silver Inorganic materials 0.000 claims abstract description 33
- 239000004332 silver Substances 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 30
- 150000003839 salts Chemical class 0.000 claims abstract description 28
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 27
- 150000001875 compounds Chemical class 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 14
- 239000011241 protective layer Substances 0.000 claims abstract description 14
- -1 cyanate radical Chemical class 0.000 claims description 85
- 238000000576 coating method Methods 0.000 claims description 49
- 239000011248 coating agent Substances 0.000 claims description 46
- 239000000126 substance Substances 0.000 claims description 37
- 210000004276 hyalin Anatomy 0.000 claims description 36
- 239000000203 mixture Substances 0.000 claims description 33
- 239000010408 film Substances 0.000 claims description 29
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical class [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 25
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 24
- 235000005985 organic acids Nutrition 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000002253 acid Substances 0.000 claims description 21
- 238000007639 printing Methods 0.000 claims description 18
- YPIFGDQKSSMYHQ-UHFFFAOYSA-N 7,7-dimethyloctanoic acid Chemical compound CC(C)(C)CCCCCC(O)=O YPIFGDQKSSMYHQ-UHFFFAOYSA-N 0.000 claims description 16
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 16
- 150000007513 acids Chemical class 0.000 claims description 15
- ZSIQJIWKELUFRJ-UHFFFAOYSA-N azepane Chemical compound C1CCCNCC1 ZSIQJIWKELUFRJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 15
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 15
- 239000011521 glass Substances 0.000 claims description 14
- YOWAEZWWQFSEJD-UHFFFAOYSA-N quinoxalin-2-amine Chemical class C1=CC=CC2=NC(N)=CN=C21 YOWAEZWWQFSEJD-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 239000001099 ammonium carbonate Substances 0.000 claims description 12
- VIJKGBZMANAGQI-UHFFFAOYSA-M benzyl(triethyl)azanium;hydrogen carbonate Chemical compound OC([O-])=O.CC[N+](CC)(CC)CC1=CC=CC=C1 VIJKGBZMANAGQI-UHFFFAOYSA-M 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 11
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- 125000003118 aryl group Chemical group 0.000 claims description 10
- 229910052788 barium Inorganic materials 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 claims description 9
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 9
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 claims description 9
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 9
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 238000004528 spin coating Methods 0.000 claims description 9
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 8
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052791 calcium Inorganic materials 0.000 claims description 8
- 239000011575 calcium Substances 0.000 claims description 8
- 230000014509 gene expression Effects 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 claims description 8
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 8
- PMBXCGGQNSVESQ-UHFFFAOYSA-N 1-Hexanethiol Chemical compound CCCCCCS PMBXCGGQNSVESQ-UHFFFAOYSA-N 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 125000000217 alkyl group Chemical group 0.000 claims description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 6
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 claims description 6
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 6
- KXDHJXZQYSOELW-UHFFFAOYSA-N carbonic acid monoamide Natural products NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 6
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 6
- 229910052738 indium Inorganic materials 0.000 claims description 6
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims description 6
- 239000003381 stabilizer Substances 0.000 claims description 6
- 229910052718 tin Inorganic materials 0.000 claims description 6
- KJAMZCVTJDTESW-UHFFFAOYSA-N tiracizine Chemical compound C1CC2=CC=CC=C2N(C(=O)CN(C)C)C2=CC(NC(=O)OCC)=CC=C21 KJAMZCVTJDTESW-UHFFFAOYSA-N 0.000 claims description 6
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 6
- 229910052720 vanadium Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000005864 Sulphur Substances 0.000 claims description 5
- CTIHZTFULZJBGQ-UHFFFAOYSA-L cobalt(2+);decanoate Chemical compound [Co+2].CCCCCCCCCC([O-])=O.CCCCCCCCCC([O-])=O CTIHZTFULZJBGQ-UHFFFAOYSA-L 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- OFUAIAKLWWIPTC-UHFFFAOYSA-L magnesium;naphthalene-2-carboxylate Chemical compound [Mg+2].C1=CC=CC2=CC(C(=O)[O-])=CC=C21.C1=CC=CC2=CC(C(=O)[O-])=CC=C21 OFUAIAKLWWIPTC-UHFFFAOYSA-L 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 239000011572 manganese Substances 0.000 claims description 5
- SGGOJYZMTYGPCH-UHFFFAOYSA-L manganese(2+);naphthalene-2-carboxylate Chemical compound [Mn+2].C1=CC=CC2=CC(C(=O)[O-])=CC=C21.C1=CC=CC2=CC(C(=O)[O-])=CC=C21 SGGOJYZMTYGPCH-UHFFFAOYSA-L 0.000 claims description 5
- 229940100890 silver compound Drugs 0.000 claims description 5
- 150000003379 silver compounds Chemical class 0.000 claims description 5
- WSFQLUVWDKCYSW-UHFFFAOYSA-M sodium;2-hydroxy-3-morpholin-4-ylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(O)CN1CCOCC1 WSFQLUVWDKCYSW-UHFFFAOYSA-M 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- JMPXSWBXXUOKFP-UHFFFAOYSA-N 2-ethylhexylazanium;n-(2-ethylhexyl)carbamate Chemical compound CCCCC(CC)C[NH3+].CCCCC(CC)CNC([O-])=O JMPXSWBXXUOKFP-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 4
- 239000004642 Polyimide Substances 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 229910052787 antimony Inorganic materials 0.000 claims description 4
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 4
- WQAQPCDUOCURKW-UHFFFAOYSA-N butanethiol Chemical compound CCCCS WQAQPCDUOCURKW-UHFFFAOYSA-N 0.000 claims description 4
- 229910052792 caesium Inorganic materials 0.000 claims description 4
- PFRGXCVKLLPLIP-UHFFFAOYSA-N diallyl disulfide Chemical compound C=CCSSCC=C PFRGXCVKLLPLIP-UHFFFAOYSA-N 0.000 claims description 4
- 238000003618 dip coating Methods 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 4
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 claims description 4
- 229910052733 gallium Inorganic materials 0.000 claims description 4
- 229910052732 germanium Inorganic materials 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 238000007641 inkjet printing Methods 0.000 claims description 4
- 229910052741 iridium Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- 150000002576 ketones Chemical class 0.000 claims description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 4
- 229940070765 laurate Drugs 0.000 claims description 4
- 229910052745 lead Inorganic materials 0.000 claims description 4
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 claims description 4
- 235000020778 linoleic acid Nutrition 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 238000007645 offset printing Methods 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- 229910052762 osmium Inorganic materials 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- IUGYQRQAERSCNH-UHFFFAOYSA-N pivalic acid Chemical compound CC(C)(C)C(O)=O IUGYQRQAERSCNH-UHFFFAOYSA-N 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 229920001230 polyarylate Polymers 0.000 claims description 4
- 229920002530 polyetherether ketone Polymers 0.000 claims description 4
- 229920005644 polyethylene terephthalate glycol copolymer Polymers 0.000 claims description 4
- 229920001721 polyimide Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 229910052702 rhenium Inorganic materials 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 229910052712 strontium Inorganic materials 0.000 claims description 4
- 229910052715 tantalum Inorganic materials 0.000 claims description 4
- RAOIDOHSFRTOEL-UHFFFAOYSA-N tetrahydrothiophene Chemical compound C1CCSC1 RAOIDOHSFRTOEL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 229940005605 valeric acid Drugs 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- UDXBSNUCGGXUNH-UHFFFAOYSA-N 2-cyanoethylazanium;2-cyanoethyl carbonate Chemical compound [NH3+]CCC#N.[O-]C(=O)OCCC#N UDXBSNUCGGXUNH-UHFFFAOYSA-N 0.000 claims description 3
- BHRGYSLLXICIEL-UHFFFAOYSA-N 2-cyanoethylazanium;n-(2-cyanoethyl)carbamate Chemical compound [NH3+]CCC#N.[O-]C(=O)NCCC#N BHRGYSLLXICIEL-UHFFFAOYSA-N 0.000 claims description 3
- WRJRTLNJQQNHLC-UHFFFAOYSA-N 2-ethylhexylazanium;2-ethylhexyl carbonate Chemical compound CCCCC(CC)C[NH3+].CCCCC(CC)COC([O-])=O WRJRTLNJQQNHLC-UHFFFAOYSA-N 0.000 claims description 3
- HTBCQGGKQJBADY-UHFFFAOYSA-N 2-methoxyethylazanium;2-methoxyethyl carbonate Chemical compound COCC[NH3+].COCCOC([O-])=O HTBCQGGKQJBADY-UHFFFAOYSA-N 0.000 claims description 3
- FEPKTMACMPNCGN-UHFFFAOYSA-N 2-methoxyethylazanium;n-(2-methoxyethyl)carbamate Chemical compound COCC[NH3+].COCCNC([O-])=O FEPKTMACMPNCGN-UHFFFAOYSA-N 0.000 claims description 3
- PFDJIMKTGBPMEC-UHFFFAOYSA-N 2-methylpropylcarbamic acid Chemical compound CC(C)CNC(O)=O PFDJIMKTGBPMEC-UHFFFAOYSA-N 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 3
- FNEYFBSZTIOFQC-UHFFFAOYSA-N C(CCC)[NH3+].C(OCC(C)C)([O-])=O Chemical compound C(CCC)[NH3+].C(OCC(C)C)([O-])=O FNEYFBSZTIOFQC-UHFFFAOYSA-N 0.000 claims description 3
- VQHNLMYBSCCEIL-UHFFFAOYSA-M C(CCCCCCCCCCCCCCC)[N+](CC1=CC=CC=C1)(C)C.C(C1=CC=CC=C1)NC([O-])=O Chemical compound C(CCCCCCCCCCCCCCC)[N+](CC1=CC=CC=C1)(C)C.C(C1=CC=CC=C1)NC([O-])=O VQHNLMYBSCCEIL-UHFFFAOYSA-M 0.000 claims description 3
- XHWPOJFDBKAVGT-UHFFFAOYSA-M CCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1.[O-]C(OCC1=CC=CC=C1)=O Chemical compound CCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1.[O-]C(OCC1=CC=CC=C1)=O XHWPOJFDBKAVGT-UHFFFAOYSA-M 0.000 claims description 3
- USKPAYUKZBVYDE-UHFFFAOYSA-N CCCN.CC(C)COC(OC(C)C)=O Chemical compound CCCN.CC(C)COC(OC(C)C)=O USKPAYUKZBVYDE-UHFFFAOYSA-N 0.000 claims description 3
- WSMMLDOKFFGIGD-UHFFFAOYSA-N CCCSSSS[Si](OCC)(OCC)OCC.CCCSSSS[Si](OCC)(OCC)OCC.NC(O)=O.N Chemical compound CCCSSSS[Si](OCC)(OCC)OCC.CCCSSSS[Si](OCC)(OCC)OCC.NC(O)=O.N WSMMLDOKFFGIGD-UHFFFAOYSA-N 0.000 claims description 3
- ARGZXRKHMZYPAK-UHFFFAOYSA-N CCCSSSS[Si](OCC)(OCC)OCC.CCCSSSS[Si](OCC)(OCC)OCC.OC(O)=O.N Chemical compound CCCSSSS[Si](OCC)(OCC)OCC.CCCSSSS[Si](OCC)(OCC)OCC.OC(O)=O.N ARGZXRKHMZYPAK-UHFFFAOYSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- HWVVYUPLWARZKN-UHFFFAOYSA-N N-butylbutan-1-amine dibutyl carbonate Chemical compound CCCCNCCCC.CCCCOC(=O)OCCCC HWVVYUPLWARZKN-UHFFFAOYSA-N 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- CDVOLRIULPDDAB-UHFFFAOYSA-N [NH4+].OC([O-])=O.C1COCCN1.C1COCCN1 Chemical compound [NH4+].OC([O-])=O.C1COCCN1.C1COCCN1 CDVOLRIULPDDAB-UHFFFAOYSA-N 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- 239000004840 adhesive resin Substances 0.000 claims description 3
- 229920006223 adhesive resin Polymers 0.000 claims description 3
- 125000001931 aliphatic group Chemical group 0.000 claims description 3
- 125000002947 alkylene group Chemical group 0.000 claims description 3
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 3
- 125000003710 aryl alkyl group Chemical group 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 3
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- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
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- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
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- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
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- XNGYKPINNDWGGF-UHFFFAOYSA-L silver oxalate Chemical compound [Ag+].[Ag+].[O-]C(=O)C([O-])=O XNGYKPINNDWGGF-UHFFFAOYSA-L 0.000 claims description 2
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- VNTDZUDTQCZFKN-UHFFFAOYSA-L zinc 2,2-dimethyloctanoate Chemical compound [Zn++].CCCCCCC(C)(C)C([O-])=O.CCCCCCC(C)(C)C([O-])=O VNTDZUDTQCZFKN-UHFFFAOYSA-L 0.000 claims description 2
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 9
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Images
Classifications
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- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3405—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of organic materials
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/018—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of a noble metal or a noble metal alloy
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
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Abstract
本发明涉及用于制造透明导电膜的方法,所述膜为包括使用具有特定结构的银络合物和有机酸金属盐的至少一层的复合多层膜。使用一种以上溶液工艺制造透明导电膜的方法包括以下步骤:(1)在透明衬底上形成透明层以改善透光率;和(2)形成导电层以赋予导电性,该方法还包括(3)形成保护层以防止导电层随时间改变的步骤。根据本发明,可以获得具有优异的导电性和透光率的大尺度的透明导电膜,并实现简单的工艺过程。
Description
技术领域
本发明涉及用于制造透明导电膜的方法,所述膜为包括使用具有特定结构的银络合物和有机酸金属盐的至少一层的复合多层膜,本发明特别涉及经由溶液工艺而具有优异的电阻特性和透光率的透明导电膜以及所述导电膜的制造方法。
背景技术
通常,透明导电膜用作电气/电子设备的必要元件,例如,将电源应用于显示器的手段、用于屏蔽消费电子产品的电磁波的层和如LCD、OLED、FED、PDP、柔性显示器和电子纸等各种显示器领域中的透明电极。如今,作为透明导电层的材料,使用诸如ITO(铟-锡氧化物)、ATO(锑-锡氧化物)、AZO(锑-锌氧化物)等无机氧化物导电材料。
如果透明导电膜通过通常使用的溅射法、离子束法或气相沉积法制造,则制得的导电层可能具有较高的导电率和优异的透光率。不过,因提供真空设备而产生的成本耗费较大,因此难以进行大批量大规模生产,而且,诸如塑料膜等透明衬底因需要低温工艺而受限。依照通过溅射工艺进行沉积时的氧分压和温度等条件,薄膜的透光率和电阻可能会随着透明导电膜组成的改变而快速改变,因此,提出通过旋涂、喷涂、敷涂和印刷等适于低成本大规模的湿式涂布来制备透明导电膜,然后进行烧结。例如,在韩国1999-011487号专利申请公报中公开了一种通过使用金属颗粒和粘合剂制备的透明导电膜,在韩国1999-064113号专利申请公报中公开了将中空碳纳米纤维添加至氧化锡中的用于透明导电膜的组合物,在韩国2000-009405号专利申请公报中公开了将氧化钕添加至氧化锡或氧化铟中的用于形成透明导电和选择性光吸收的膜的喷雾溶液。此外,还公开了一种用于制造透明导电层形成用溶液的方法,该溶液包含金属纳米颗粒,如金和银。
通过上述方法制得的透明导电膜的表面电阻高达103Ω/□~104Ω/□,而且由于周围环境的变化所致随时间增大,由此不能保持初期导电率,因而透明导电膜的使用受限。
因此,本发明人努力解决这些问题,由此获得本发明。也就是说,本发明涉及用于制造透明导电膜的方法,所述膜为包括使用具有特定结构的银络合物和有机酸金属盐的至少一层的复合多层膜,本发明特别涉及经由溶液工艺而具有优异的电阻特性和透光率的透明导电膜以及所述导电膜的制造方法。
发明内容
技术问题
通过努力解决这些问题,本发明人由此能够提供具有优异电阻特性和透光率的透明导电膜,所述膜形成为包括使用具有特定结构的银络合物和有机酸金属盐的至少一层的复合多层膜形式的透明导电膜,并提供所述透明导电膜的制造方法。
此外,本发明可提供经由溶液工艺简单制造复合多层膜形式的透明导电膜的方法。
此外,本发明可提供具有优异导电性和透光率的大尺度透明导电膜,以及简单工艺。
技术方案
本发明涉及制造透明导电膜的方法,所述膜为包括使用具有特定结构的银络合物和有机酸金属盐的至少一层的复合多层膜,本发明特别涉及经由溶液工艺而具有优异的电阻特性和透光率的透明导电膜。
下面将详细描述本发明。
如图1所示,本发明的用于制造透明导电膜的方法制得了包括使用一种或两种以上银络合物和一种或两种以上有机酸金属盐的至少一层的复合多层膜。所述方法使用一种以上的溶液工艺,其包括下列步骤:(1)在透明衬底1上形成透明层2以改善透光率;和(2)形成导电层3以赋予导电率,此外,该方法还包括(3)形成保护层4以防止导电层随时间改变的步骤。尽管透明导电膜10的制造方法以图1的结构进行解释,不过该结构仅仅是示例性的,并非意图限制本发明的范围。
下面,将具体描述本发明的方法的每一步。
上述步骤(1)是通过将包含有机酸金属盐的透明层溶液涂布在透明衬底上来形成透明层。
该步骤是使用包含有机酸金属盐的组合物在透明衬底上形成透明层从而改善透光率。
所述透明衬底可使用经由涂布或印刷工艺可以在该衬底上容易地形成薄膜或图案层的各种衬底。例如,所述衬底可选自玻璃衬底或透明塑料膜,如聚酰亚胺(PI)、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、尼龙、聚四氟乙烯(PTFE)、聚醚醚酮(PEEK)、聚碳酸酯(PC)和聚芳酯(PAR)。这样的衬底可以在漂洗和油脂脱除之后进行使用,或特别是在预处理过程之后进行使用,其中所述预处理过程可选自但不限于等离子体、离子束、电晕、氧化或还原、加热、蚀刻、紫外线照射以及使用粘合剂或添加剂的底涂处理。
有机酸金属盐不作必要限定。即,可以使用任何已知种类,只要其符合本发明的目的即可。
尽管用于本发明的有机酸金属盐不做必要限定,只要符合本发明即可,不过优选碳数为3~28的有机酸金属盐或包含碳数为3~28的有机金属盐与有机酸的有机酸金属盐混合物。有机酸以丁酸、戊酸、丙烯酸、特戊酸、正己酸、叔辛酸、2-乙基己酸、新癸酸、月桂酸、硬脂酸、油酸、环烷酸、十二烷酸和亚油酸为例。有机酸金属盐的金属成分以Li、Na、K、Rb、Cs、Be、Mg、Ca、Sr、Ba、Ti、V、Mn、Fe、Co、Ni、Cu、Zn、Y、Zr、Nb、Mo、Ru、Rh、Pd、Ag、Cd、Hf、Ta、W、Re、Os、Ir、Pt、Au、Hg、Al、Ga、In、Tl、Ge、Sn、Pb、Sb、Bi、La、Ce、Pr、Nd、Sm和Eu为例。通过从正己酸锰、叔辛酸镁、环烷酸锂、新癸酸钾、2-乙基己酸银、新癸酸锌、硬脂酸钴、环烷酸镍、环烷酸铝、环烷酸镁、环烷酸钡、环烷酸锰、环烷酸锌、环烷酸钒、环烷酸锆、环烷酸锶、油酸锡、叔辛酸铟、二丙烯酸锡、新癸酸钴、2-乙基己酸铜、硬脂酸铁、油酸镍、新癸酸钙、新癸酸钡、十二烷酸铯、亚油酸铅和环烷酸铈中选择一种以上的金属材料而使用有机金属盐。
此外,所述有机酸金属盐可以为球型、直线型、板型或这些类型的混合型,并且以各种状态使用,例如包括纳米颗粒在内的颗粒、粉末、薄片、胶体、混合物、浆料、溶胶、溶液状态或者将其中一种以上混合的状态。
有机酸金属盐的用量不必限定,只要其符合本发明的墨水特性即可。优选的是相对于透明层溶液的总重量为0.01重量%~10重量%,更优选0.01重量%~1重量%。
所述透明层溶液至少包含一种以上的所述有机酸金属盐以改善透光率,并在必要时包含溶剂、稳定剂、分散剂、粘合剂树脂、还原剂、表面活性剂、润湿剂、触变剂或流平剂。
考虑到薄膜的物理性质时,透明层的热处理优选在80℃~400℃,更优选90℃~300℃,进而更优选100℃~150℃的温度范围进行。另外,理想的是对薄膜实施于上述范围内的低温和高温进行的两步以上的热处理,目的在于使得薄膜均匀。例如,优选的是在80℃~150℃处理1分钟~30分钟和在150℃~300℃处理1分钟~30分钟。
根据墨水的物理性质,透明层的涂布方法可选自旋涂、辊涂、喷涂、浸涂、浇涂、刮刀式分配、喷墨印刷、胶印、丝网印刷、压印、凹版印刷、柔版印刷、刻版印刷、盖印、静电印刷和平版印刷方法。
本发明的步骤(2)是通过涂布导电层溶液来形成导电层,从而形成可赋予导电性的导电层。
用于形成导电层的银络合物通过使由以下化学式1表示的银化合物与选自由以下化学式2表示的氨基甲酸铵类化合物、由化学式3表示的碳酸铵类化合物、由化学式4表示的碳酸铵类化合物或其混合物中的一种或多种化合物反应而制得。
[化学式1]
AgnX
[化学式2]
[化学式3]
[化学式4]
[X是选自由氧、硫、卤素、氰基、氰酸根、碳酸根、硝酸根、亚硝酸根、硫酸根、磷酸根、硫氰酸根、氯酸根、高氯酸根、四氟硼酸根、乙酰丙酮根、羧酸根及其衍生物组成的组中的取代基,
n是1~4的整数,R1~R6是独立地选自氢、C1~C30脂肪族或环状烷基、芳基或芳烷基、取代有官能团的烷基和芳基、杂环化合物或高分子化合物或其衍生物中的取代基,其中R1和R2,或R4和R5,能够经由包含或不包含杂原子的亚烃基而相互连接以成环。]
化学式1中的化合物可举出但不限于氧化银、硫氰酸银、硫化银、氯化银、氰化银、氰酸银、碳酸银、硝酸银、亚硝酸银、硫酸银、磷酸银、高氯酸银、四氟硼酸银、乙酰丙酮银、乙酸银、乳酸银、草酸银及其衍生物。
此外,R1~R6可选自但不限于由氢、甲基、乙基、丙基、异丙基、丁基、异丁基、戊基、己基、乙基己基、庚基、辛基、异辛基、壬基、癸基、十二烷基、十六烷基、十八烷基、二十二烷基、环丙基、环戊基、环己基、烯丙基、羟基、甲氧基、羟基乙基、甲氧基乙基、2-羟基丙基、甲氧基丙基、氰基乙基、乙氧基、丁氧基、己氧基、甲氧基乙氧基乙基、甲氧基乙氧基乙氧基乙基、六亚甲基亚胺、吗啉、哌啶、哌嗪、乙二胺、丙二胺、六亚甲基二胺、三乙二胺、吡咯、咪唑、吡啶、羧甲基、三甲氧基甲硅烷基丙基、三乙氧基甲硅烷基丙基、苯基、甲氧基苯基、氰基苯基、苯氧基、甲苯基、苄基及其衍生物、以及诸如聚烯丙基胺或聚乙烯亚胺等聚合物及其衍生物组成的组。
化学式2中的氨基甲酸铵类化合物可以是选自由氨基甲酸铵、乙基氨基甲酸乙基铵、异丙基氨基甲酸异丙基铵、正丁基氨基甲酸正丁基铵、异丁基氨基甲酸异丁基铵、叔丁基氨基甲酸叔丁基铵、2-乙基己基氨基甲酸2-乙基己基铵、十八烷基氨基甲酸十八烷基铵、2-甲氧基乙基氨基甲酸2-甲氧基乙基铵、2-氰基乙基氨基甲酸2-氰基乙基铵、二丁基氨基甲酸二丁基铵、二(十八烷基)氨基甲酸二(十八烷基)铵、甲基癸基氨基甲酸甲基癸基铵、六亚甲基亚胺氨基甲酸六亚甲基亚胺铵、吗啉氨基甲酸吗啉鎓、乙基己基氨基甲酸吡啶鎓、异丙基二氨基甲酸三乙二铵、苄基氨基甲酸苄基铵、三乙氧基甲硅烷基丙基氨基甲酸三乙氧基甲硅烷基丙基铵及其衍生物组成的组中的一种或多种化合物。化学式3中的碳酸铵类化合物可以是选自由碳酸铵、乙基碳酸乙基铵、异丙基碳酸异丙基铵、正丁基碳酸正丁基铵、异丁基碳酸异丁基铵、叔丁基碳酸叔丁基铵、2-乙基己基碳酸2-乙基己基铵、2-甲氧基乙基碳酸2-甲氧基乙基铵、2-氰基乙基碳酸2-氰基乙基铵、十八烷基碳酸十八烷基铵、二丁基碳酸二丁基铵、二(十八烷基)碳酸二(十八烷基)铵、甲基癸基碳酸甲基癸基铵、六亚甲基亚胺碳酸六亚甲基亚胺铵、吗啉碳酸吗啉铵、苄基碳酸苄基铵、三乙氧基甲硅烷基丙基碳酸三乙氧基甲硅烷基丙基铵、异丙基碳酸三乙二铵及其衍生物组成的组中的一种或多种化合物。此外,化学式4中的碳酸氢铵类化合物可以是选自由碳酸氢铵、碳酸氢异丙基铵、碳酸氢叔丁基铵、碳酸氢2-乙基己基铵、碳酸氢2-甲氧基乙基铵、碳酸氢2-氰基乙基铵、碳酸氢二(十八烷基)铵、碳酸氢吡啶鎓、碳酸氢三乙二铵及其衍生物组成的组中的一种或多种化合物。
同时,不必对氨基甲酸铵类化合物、碳酸铵类化合物或碳酸氢铵类化合物的种类和制造方法做限定。例如,在美国专利号4,542,214(1985.9.17)中,氨基甲酸铵类化合物可由伯胺、仲胺、叔胺或包含其中至少一种的混合物与二氧化碳来制得,如果每1摩尔的胺进一步添加0.5摩尔的水则可制得碳酸铵类化合物,如果进一步添加至少1摩尔的水则可制得碳酸氢铵类化合物。此时,在恒压或加压下无需特定溶剂即可制得这些物质。所述溶剂选自:水;醇类,如甲醇、乙醇、异丙醇和丁醇;二醇类,如乙二醇和丙三醇;乙酸酯类,如乙酸乙酯、乙酸丁酯和卡必醇乙酸酯;醚类,如***、四氢呋喃和二噁烷;酮类,如甲基乙基酮和丙酮;烃类,如己烷和庚烷;芳香烃类,如苯和甲苯;卤代溶剂类,如氯仿或二氯甲烷、四氯化碳,或者它们的混合物。二氧化碳可以以气相鼓泡,或者使用固相的干冰,甚至可在超临界状态反应。氨基甲酸铵类化合物、碳酸铵类化合物或碳酸氢铵类化合物的衍生物可以用上述方法之外的任何公知的方法制造,只要所得结构相同即可。也就是说,不必限定溶剂、反应温度、浓度或催化剂。
有机银络合物或银络合物可通过使氨基甲酸铵类、碳酸铵类或碳酸氢铵类化合物与银化合物反应而制得。例如,至少一种由化学式1表示的银化合物与由化学式2~4表示的化合物或其混合物可以在氮气氛围的恒压或加压下无需溶剂直接反应。此时,溶剂选自:水;醇类,如甲醇、乙醇、异丙醇和丁醇;二醇类,如乙二醇和丙三醇;乙酸酯类,如乙酸乙酯、乙酸丁酯和卡必醇乙酸酯;醚类,如***、四氢呋喃和二噁烷;酮类,如甲基乙基酮和丙酮;烃类,如己烷和庚烷;芳香烃类,如苯和甲苯;卤代溶剂类,如氯仿或二氯甲烷、四氯化碳,或者它们的混合物。
在由本申请的发明人申请的韩国10-2006-0011083号专利申请中已经描述了本发明的制造银络合物或银络合物混合物的方法。
导电层的组成包括银络合物或银络合物混合物,并且在必要时可包含诸如溶剂、稳定剂、分散剂、薄层补充物、粘合剂树脂、还原剂、表面活性剂、润湿剂、触变剂或流平剂等添加剂。
稳定剂例如可选自:如伯胺、仲胺或叔胺等胺化合物;氨基甲酸铵类化合物;碳酸铵类化合物;碳酸氢铵类化合物;或诸如膦、磷酸盐或磷酸酯等磷化合物;诸如硫醇或硫化物等硫化合物;以及它们的混合物。
也就是说,所述胺化合物可例示为甲基胺、乙基胺、正丙基胺、异丙基胺、正丁基胺、异丁基胺、异戊基胺、正己基胺、2-乙基己基胺、正庚基胺、正辛基胺、异辛基胺、壬基胺、癸基胺、十二烷基胺、十六烷基胺、十八烷基胺、二十二烷基胺、环丙基胺、环戊基胺、环己基胺、烯丙基胺、羟基胺、氢氧化铵、甲氧基胺、2-乙醇胺、甲氧基乙基氨基、2-羟基丙基胺、2-羟基-2-甲氧基丙基胺、甲氧基丙基胺、氰基乙基胺、乙氧基胺、正丁氧基胺、2-己氧基胺、甲氧基乙氧基乙基胺、甲氧基乙氧基乙氧基乙基胺、二乙基胺、二丙基胺、二乙醇胺、六亚甲基亚胺、吗啉、哌啶、哌嗪、乙二胺、丙二胺、六亚甲基二胺、三乙二胺、2,2-(乙二氧基)双乙胺、三乙胺、三乙醇胺、吡咯、咪唑、吡啶、氨基乙醛二甲基乙缩醛、3-氨基丙基三甲氧基硅烷、3-氨基丙基三乙氧基硅烷、苯胺、茴香胺、氨基苄腈、苄基胺及其衍生物、诸如聚烯丙基胺或聚乙烯亚胺等聚合物及其衍生物。
所述氨基甲酸铵类化合物例示为氨基甲酸铵、乙基氨基甲酸乙基铵、异丙基氨基甲酸异丙基铵、正丁基氨基甲酸正丁基铵、异丁基氨基甲酸异丁基铵、叔丁基氨基甲酸叔丁基铵、2-乙基己基氨基甲酸2-乙基己基铵、十八烷基氨基甲酸十八烷基铵、2-甲氧基乙基氨基甲酸2-甲氧基乙基铵、2-氰基乙基氨基甲酸2-氰基乙基铵、二丁基氨基甲酸二丁基铵、二(十八烷基)氨基甲酸二(十八烷基)铵、甲基癸基氨基甲酸甲基癸基铵、六亚甲基亚胺氨基甲酸六亚甲基亚胺铵、吗啉氨基甲酸吗啉鎓、乙基己基氨基甲酸吡啶鎓、异丙基二氨基甲酸三乙二铵、苄基氨基甲酸苄基铵、三乙氧基甲硅烷基丙基氨基甲酸三乙氧基甲硅烷基丙基铵及其衍生物。所述碳酸铵类化合物例示为碳酸铵、乙基碳酸乙基铵、异丙基碳酸异丙基铵、正丁基碳酸正丁基铵、异丁基碳酸异丁基铵、叔丁基碳酸叔丁基铵、2-乙基己基碳酸2-乙基己基铵、2-甲氧基乙基碳酸2-甲氧基乙基铵、2-氰基乙基碳酸2-氰基乙基铵、十八烷基碳酸十八烷基铵、二丁基碳酸二丁基铵、二(十八烷基)碳酸二(十八烷基)铵、甲基癸基碳酸甲基癸基铵、六亚甲基亚胺碳酸六亚甲基亚胺铵、吗啉碳酸吗啉铵、苄基碳酸苄基铵、三乙氧基甲硅烷基丙基碳酸三乙氧基甲硅烷基丙基铵、异丙基碳酸三乙二铵及其衍生物。所述碳酸氢铵类化合物例示为碳酸氢铵、碳酸氢异丙基铵、碳酸氢叔丁基铵、碳酸氢2-乙基己基铵、碳酸氢2-甲氧基乙基铵、碳酸氢2-氰基乙基铵、碳酸氢二(十八烷基)铵、碳酸氢吡啶鎓、碳酸氢三乙二铵及其衍生物。
此外,锡化合物由R3P、(RO)3P或(RO)3PO表示,其中R表示碳数为1~20的烷基或芳基,代表性地例示为三丁基膦、三苯基膦、亚磷酸三乙酯、亚磷酸三苯酯、磷酸二苄酯和磷酸三乙酯。此外,硫化合物例示为丁硫醇、正己硫醇、二乙硫醚、四氢噻吩、烯丙基二硫化物、巯基苯并噻唑、巯基乙酸烷基酯、四氢噻吩和巯基乙酸辛酯。该稳定剂不作必要限制,只要其符合本发明的墨水特性即可。不过,其相对于银络合物优选具有的含量为0.1%~90%(摩尔比),更优选为1%~50%。高于上述范围时薄膜的导电率可能下降,而当低于该范围时墨水存储的稳定性可增大。
此外,薄膜补充物可使用有机酸和有机酸的衍生物,并且由一种或两种以上的混合物构成。有机酸例示为乙酸、草酸、柠檬酸、乳酸、马来酸、丙烯酸、丁酸、戊酸、特戊酸、正己酸、叔辛酸、2-乙基己酸、新癸酸、月桂酸、硬脂酸、油酸、环烷酸、十二烷酸和亚油酸。有机酸的衍生物例示为:有机酸的铵盐,如乙酸铵、柠檬酸铵、月桂酸铵、乳酸铵、马来酸铵和草酸铵,以及具有诸如Au、Cu、Zn、Ni、Co、Pd、Pt、Ti、V、Mn、Fe、Cr、Zr、Nb、Mo、W、Ru、Cd、Ta、Re、Os、Ir、Al、Ga、Ge、In、Sn、Sb、Pb、Bi、Sm、Eu、Ac和Th等金属的有机酸金属盐。所述有机酸金属盐可例示为草酸锰、乙酸金、草酸钯、2-乙基己酸银、辛酸银、新癸酸银、硬脂酸钴、环烷酸镍和环烷酸钴。不必限定薄膜补充物的用量,不过优选相对于银络合物或混合物为0.1%~25%。如果高于上述范围则不能形成均匀的薄膜,当低于上述范围时则薄膜上可能出现裂纹。
为控制银溶液的粘度或形成平滑的薄膜往往需要溶剂。所述溶剂例示为:水;醇类,如甲醇、乙醇、异丙醇、1-甲氧基丙醇、丁醇、乙基己基醇和萜品醇;二醇类,如乙二醇和丙三醇;乙酸酯类,如乙酸乙酯、乙酸丁酯、乙酸甲氧基丙酯、卡必醇乙酸酯和乙基卡必醇乙酸酯;醚类,如甲基溶纤剂、丁基溶纤剂、***、四氢呋喃和二噁烷;酮类,如甲基乙基酮、丙酮、二甲基甲酰胺和1-甲基-2-吡咯烷酮;烃类,如己烷、庚烷、十二烷、石蜡油和溶剂油;芳香烃类,如苯、甲苯和二甲苯;卤代溶剂,如氯仿、二氯甲烷和四氯化碳、乙腈和二甲亚砜,以及它们的混合物。
考虑到薄膜的物理性质时,导电层的热处理优选在80℃~400℃、更优选90℃~300℃,进而更优选100℃~150℃的温度进行。另外,理想的是对薄膜实施于上述范围内的低温和高温进行的两步以上的热处理,目的在于使得薄膜均匀。例如,优选的是在80℃~150℃处理1分钟~30分钟和在150℃~300℃处理1分钟~30分钟。
根据墨水的物理性质,导电层的涂布方法可选自旋涂、辊涂、喷涂、浸涂、浇涂、刮刀式分配、喷墨印刷、胶印、丝网印刷、压印、凹版印刷、柔版印刷、刻版印刷、盖印、静电印刷和平版印刷方法。
本发明的步骤(3)是通过涂布无机氧化物或硫醇化合物来形成导电层的保护层,从而防止导电层随时间改变。
上述保护层可使用溶胶或胶体状态的无机氧化物,如二氧化硅(SiO2)、氧化钛、氧化锆和氧化锌,或者硫醇化合物,例如优选其中引入了碳数为2~24的烷基或芳基的硫醇,如1-己基硫醇、十二烷基硫醇、月桂基硫醇、十六烷基硫醇、十八烷基硫醇、苯并硫醇、巯基乙酸、巯基苄醇、巯基乙醇、巯基***、巯基咪唑、巯基吡啶、巯基苯酚、1,2-乙二硫酚、1,2-丙二硫酚或2,3-二巯基-1-丙醇。保护层的材料可以通过混合一种或两种以上的材料而以各种方式使用。
考虑到薄膜的物理性质时,保护层的热处理优选在50℃~300℃、更优选60℃~200℃、进而更优选70℃~150℃的温度进行。另外,理想的是对薄膜实施于上述范围内的低温和高温进行的两步以上的热处理,目的在于使得薄膜均匀。例如,优选的是在80℃~150℃处理1分钟~30分钟和在150℃~300℃处理1分钟~30分钟。
根据墨水的物理性质,保护层的涂布方法可选自旋涂、辊涂、喷涂、浸涂、浇涂、刮刀式分配、喷墨印刷、胶印、丝网印刷、压印、凹版印刷、柔版印刷、刻版印刷、盖印、静电印刷和平版印刷。
附图说明
本发明的上述和其他目的、特征和优点将由下列结合附图的优选实施方式的具体描述而更加清楚,图中:
图1是显示本发明的透明导电层的截面图。
图2是描述根据本发明的实施方式18的透光率测定结果的图。
图3是描述根据本发明的实施方式23的透光率测定结果的图。
主要要素的详细说明
1:衬底层
2:透明层
3:导电层
4:保护层
10:透明导电膜
具体实施方式
下面参照附图详细描述本发明的实施方式,不过所述实施方式仅仅是本发明的实例而非意图限制本发明的范围。
透明层溶液的制造
实施方式1
将10ml甲醇和5g环烷酸装入配有搅拌机的250ml的Schlenk烧瓶中,并加入28重量%的氨水溶液2ml,同时于80℃的温度进行搅拌,由此使其反应1小时。然后,通过向Schlenk烧瓶中缓慢添加20重量%的硝酸钡的水溶液9.3ml来制造环烷酸钡溶液。过滤上述溶液以获取环烷酸钡,然后将其再次溶解在己烷中并过滤,由此制得去除杂质的环烷酸钡溶液。在己烷中稀释该溶液至钡含量为0.3重量%,制得用于透明层的墨水组合物。
实施方式2
将10ml甲醇和5g新癸酸装入配有搅拌机的250ml的Schlenk烧瓶中,并加入28重量%的氨水溶液4ml,同时于80℃的温度进行搅拌,由此使其反应1小时。然后,通过向Schlenk烧瓶中缓慢添加30重量%的硝酸钙的水溶液8ml来制造新癸酸钙溶液。过滤上述溶液以获取新癸酸钙,然后将其再次溶解在己烷中并过滤,由此制得去除杂质的新癸酸钙溶液。在己烷中稀释该溶液至钙含量为0.3重量%,制得用于透明层的墨水组合物。
实施方式3
将10ml甲醇和5g环烷酸装入配有搅拌机的250ml的Schlenk烧瓶中,并加入28重量%的氨水溶液2ml,同时于80℃的温度进行搅拌,由此使其反应1小时。然后,通过向Schlenk烧瓶中缓慢添加20重量%的硝酸铝的水溶液13.4ml来制造环烷酸铝溶液。过滤上述溶液以获取环烷酸铝,然后将其再次溶解在己烷中并过滤,由此制得去除杂质的环烷酸铝溶液。在己烷中稀释该溶液至铝含量为0.2重量%,制得用于透明层的墨水组合物。
实施方式4
将10ml甲醇和5g新癸酸装入配有搅拌机的250ml的Schlenk烧瓶中,并加入28重量%的氨水溶液4ml,同时于80℃的温度进行搅拌,由此使其反应1小时。然后,通过向Schlenk烧瓶中缓慢添加20重量%的硝酸钴的水溶液21.1ml来制造新癸酸钴溶液。过滤上述溶液以获取新癸酸钴,然后将其再次溶解在己烷中并过滤,由此制得去除杂质的新癸酸钴溶液。在己烷中稀释该溶液至钴含量为0.2重量%,制得用于透明层的墨水组合物。
实施方式5
将10ml甲醇和5g环烷酸装入配有搅拌机的250ml的Schlenk烧瓶中,并加入28重量%的氨水溶液2ml,同时于80℃的温度进行搅拌,由此使其反应1小时。然后,通过向Schlenk烧瓶中缓慢添加45重量%的硝酸锰的水溶液1.9ml来制造环烷酸锰溶液。过滤上述溶液以获取环烷酸锰,然后将其再次溶解在己烷中并过滤,由此制得去除杂质的环烷酸锰溶液。在己烷中稀释该溶液至锰含量为0.4重量%,制得用于透明层的墨水组合物。
实施方式6
将10ml甲醇和5g环烷酸装入配有搅拌机的250ml的Schlenk烧瓶中,并加入28重量%的氨水溶液2ml,同时于80℃的温度进行搅拌,由此使其反应1小时。然后,通过向Schlenk烧瓶中缓慢添加20重量%的硝酸锌的水溶液10.6ml来制造环烷酸锌溶液。过滤上述溶液以获取环烷酸锌,然后将其再次溶解在己烷中并过滤,由此制得去除杂质的环烷酸锌溶液。在己烷中稀释该溶液至锌含量为0.3重量%,制得用于透明层的墨水组合物。
实施方式7
将10ml甲醇和5g环烷酸装入配有搅拌机的250ml的Schlenk烧瓶中,并加入28重量%的氨水溶液2ml,同时于80℃的温度进行搅拌,由此使其反应1小时。然后,通过向Schlenk烧瓶中缓慢滴加20重量%的硝酸镁的水溶液9.2ml来制造环烷酸镁溶液。过滤上述溶液以获取环烷酸镁,然后将其再次溶解在己烷中并过滤,由此制得去除杂质的环烷酸镁溶液。在己烷中稀释该溶液至镁含量为0.2重量%,制得用于透明层的墨水组合物。
实施方式8
以50体积%∶50体积%的比例混合实施方式1中制得的溶液与实施方式2中制得的溶液,制备透明层溶液。
实施方式9
以50体积%∶50体积%的比例混合实施方式4中制得的溶液与实施方式7中制得的溶液,制备透明层溶液。
导电层溶液的制造
实施方式10
将33.7g(141.9mmol)的2-乙基己基氨基甲酸2-乙基己基铵装入配有搅拌机的250ml的Schlenk烧瓶中,并加入10.0g(43.1mmol)氧化银以使其在室温下进行搅拌的情况下反应2小时。随着反应的进行,首先获得黑色浆料,随后其变为络合物,且颜色逐渐变浅,最终成为43.7g的黄色透明液相银络合物,粘度为0.31pa.s。热分析(TGA)的结果为银含量是22.0重量%。用甲醇稀释该银络合物至银含量为0.75重量%,制得导电层溶液。
实施方式11
用甲醇稀释实施方式10制得的银络合物至银含量为1.0重量%,制得导电层溶液。
实施方式12
用甲醇稀释实施方式10制得的银络合物至银含量为0.3重量%,制得导电层溶液。
保护层溶液的制造
实施方式13
用甲醇稀释尺寸为5nm的硅溶胶(产品名:NYASIL 5,制造公司:NYACOL)溶液至二氧化硅的含量为1重量%,制得保护层溶液。
实施方式14
通过混合10g 1-己基硫醇(制造公司:Aldrich)和350g甲醇然后搅拌1小时以制得保护层溶液。
透明导电膜的制造
实施方式15
准备用于旋涂的玻璃衬底以制造透明导电层,并在使用乙醇除去衬底表面上的灰尘后用干燥器于50℃干燥至少30分钟。透明层如下制造:将干燥过的玻璃衬底放置在旋涂机上并在整个玻璃衬底上倾倒20ml实施方式2的组合物,其以300rpm旋转随后于100℃的温度干燥1分钟。在整个透明层上倾倒20ml实施方式12的组合物之后,其以300rpm旋转从而形成导电层,随后在120℃的温度干燥2分钟,由此制得透明导电膜。表1中显示了透明导电膜的表面电阻、透光率和随时间的改变的结果。
实施方式16
准备用于旋涂的玻璃衬底以制造透明导电层,并在使用乙醇除去衬底表面上的灰尘后用干燥器于50℃干燥至少30分钟。透明层如下制造:将干燥过的玻璃衬底放置在旋涂机上并在整个玻璃衬底上倾倒20ml实施方式2的组合物,其以300rpm旋转随后于100℃的温度干燥1分钟。在整个透明层上倾倒20ml实施方式12的组合物之后,其以300rpm旋转从而形成导电层,随后在120℃的温度干燥2分钟,接着以300rpm旋转实施方式13的组合物以形成保护层,由此制得透明导电膜。表1中显示了制得的透明导电膜的表面电阻、透光率和随时间的改变的结果。
实施方式17
以与实施方式16相同的方式进行,不同之处在于使用实施方式11来形成导电层。表1中显示了制得的透明导电膜的表面电阻、透光率和随时间的改变的结果。
实施方式18
以与实施方式16相同的方式进行,不同之处在于使用实施方式1来形成透明层和使用实施方式14来形成保护层。表1中显示了制得的透明导电膜的表面电阻、透光率和随时间的改变的结果。
实施方式19
以与实施方式16相同的方式进行,不同之处在于使用实施方式3来形成透明层。表1中显示了制得的透明导电膜的表面电阻、透光率和随时间的改变的结果。
实施方式20
以与实施方式16相同的方式进行,不同之处在于使用实施方式4来形成透明层。表1中显示了制得的透明导电膜的表面电阻、透光率和随时间的改变的结果。
实施方式21
以与实施方式16相同的方式进行,不同之处在于使用实施方式5来形成透明层。表1中显示了制得的透明导电膜的表面电阻、透光率和随时间的改变的结果。
实施方式22
以与实施方式16相同的方式进行,不同之处在于使用实施方式6来形成透明层。表1中显示了制得的透明导电膜的表面电阻、透光率和随时间的改变的结果。
实施方式23
以与实施方式16相同的方式进行,不同之处在于使用实施方式7来形成透明层。表1中显示了制得的透明导电膜的表面电阻、透光率和随时间的改变的结果。
实施方式24
以与实施方式16相同的方式进行,不同之处在于使用实施方式8来形成透明层。表1中显示了制得的透明导电膜的表面电阻、透光率和随时间的改变的结果。
实施方式25
以与实施方式16相同的方式进行,不同之处在于使用实施方式9来形成透明层。表1中显示了制得的透明导电膜的表面电阻、透光率和随时间的改变的结果。
比较例1
准备用于旋涂的玻璃衬底以制造透明导电层,并在使用乙醇除去衬底表面上的灰尘后用干燥器于50℃干燥至少30分钟。透明导电层如下制造:将干燥过的玻璃衬底放置在旋涂机上并在整个玻璃衬底上倾倒20ml实施方式12的组合物,其以300rpm旋转随后于120℃的温度干燥2分钟。表1中显示了制得的透明导电膜的表面电阻、透光率和随时间的改变的结果。
比较例2
准备用于旋涂的玻璃衬底以制造透明导电层,并在使用乙醇除去衬底表面上的灰尘后用干燥器于50℃干燥至少30分钟。透明导电层如下制造:将干燥过的玻璃衬底放置在旋涂机上并在整个玻璃衬底上倾倒20mlPEDOT/PSS(可从Bayer company获得),其以300rpm旋转随后于120℃的温度干燥2分钟。表1中显示了制得的透明导电膜的表面电阻、透光率和随时间的改变的结果。
表1各实施方式和比较例中制得的透明导电层的物理数据
实施方式 | 形成导电层后的热处理的温度(℃) | 表面电阻(Ω/□) | 透光率(%于50nm) | 随时间的改变 | 评价 |
实施方式15 | 120 | 25 | 74 | △ | - |
实施方式16 | 120 | 23 | 84 | ○ | - |
实施方式17 | 120 | 16 | 74 | ○ | - |
实施方式18 | 120 | 25 | 78 | ○ | - |
实施方式19 | 120 | 27 | 76 | ○ | - |
实施方式20 | 120 | 30 | 78 | ○ | - |
实施方式21 | 120 | 25 | 79 | ○ | - |
实施方式22 | 120 | 28 | 81 | ○ | - |
实施方式23 | 120 | 30 | 82 | ○ | - |
实施方式24 | 120 | 27 | 79 | ○ | - |
实施方式25 | 120 | 28 | 78 | ○ | - |
比较例1 | 120 | 33 | 53 | × | - |
比较例2 | 120 | 4500 | 91 | ○ | - |
(1)随时间改变的评估:自透明导电膜制得起30天后表面电阻的变化的测定。
○:表面电阻没有变化
△:表面电阻的变化在10%以内
×:表面电阻的变化大于10%
(2)导电性的评估:制得式样为1cm×3cm的矩形样品后,用AITCMT-SR1000N测定表面电阻。
(3)透光率的评估:制得式样为2cm×2cm的矩形样品后,通过分光光度计(PerkinElmer Model lambla-650)测定透光率。
工业实用性
本发明涉及透明导电膜以及所述膜的制造方法,所述膜为包括使用具有特定结构的银络合物和有机酸金属盐的至少一层的复合多层膜。
本发明提供具有优异的表面电阻和透光率的透明导电膜及其制造方法。
根据本发明,可以获得具有优异的导电性和透光率的透明导电膜,并实现简单的制造工艺。
此外,还可以提供可用作电气/电子设备的必要元件的导电膜,例如,将电源应用于显示器的手段、用于屏蔽消费电子产品的电磁波的层和如LCD、OLED、FED、PDP、柔性显示器和电子纸等各种显示器领域中的透明电极。
Claims (23)
1.一种用于制造透明导电膜的方法,所述方法包括下列步骤:
将包含有机酸金属盐的透明层溶液涂布在透明衬底上以形成透明层;和
将包含银络合物的导电层溶液涂布在所述透明层上以形成导电层,所述银络合物通过使由以下化学式1表示的银化合物与选自由以下化学式2表示的氨基甲酸铵类化合物、由化学式3表示的碳酸铵类化合物、由化学式4表示的碳酸铵类化合物或其混合物中的一种或多种化合物反应而制得
[化学式1]
AgnX
[化学式2]
[化学式3]
[化学式4]
其中,X是选自由氧、硫、卤素、氰基、氰酸根、碳酸根、硝酸根、亚硝酸根、硫酸根、磷酸根、硫氰酸根、氯酸根、高氯酸根、四氟硼酸根、乙酰丙酮根、羧酸根及其衍生物组成的组中的取代基,
n是1~4的整数,R1~R6是独立地选自氢、C1~C30脂肪族或环状烷基、芳基或芳烷基、取代有官能团的烷基和芳基、杂环化合物或高分子化合物或其衍生物中的取代基,其中R1和R2,或R4和R5,能够经由包含或不包含杂原子的亚烃基而相互连接以成环。
2.如权利要求1所述的方法,其中,所述透明衬底是聚酰亚胺(PI)、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、尼龙、聚四氟乙烯(PTFE)、聚醚醚酮(PEEK)、聚碳酸酯(PC)和聚芳酯(PAR)或玻璃。
3.如权利要求1所述的方法,其中,所述有机酸金属盐包括碳数为3~28的有机酸。
4.如权利要求3所述的方法,其中,所述有机酸金属盐的有机酸选自由丁酸、戊酸、丙烯酸、特戊酸、正己酸、叔辛酸、2-乙基己酸、新癸酸、月桂酸、硬脂酸、油酸、环烷酸、十二烷酸和亚油酸组成的组。
5.如权利要求3所述的方法,其中,所述有机酸金属盐的金属选自由Li、Na、K、Rb、Cs、Be、Mg、Ca、Sr、Ba、Ti、V、Mn、Fe、Co、Ni、Cu、Zn、Y、Zr、Nb、Mo、Ru、Rh、Pd、Ag、Cd、Hf、Ta、W、Re、Os、Ir、Pt、Au、Hg、Al、Ga、In、Tl、Ge、Sn、Pb、Sb、Bi、La、Ce、Pr、Nd、Sm和Eu组成的组。
6.如权利要求5所述的方法,其中,所述有机酸金属盐单独使用,或者与选自由正己酸锰、叔辛酸镁、环烷酸锂、新癸酸钾、2-乙基己酸银、新癸酸锌、硬脂酸钴、环烷酸镍、环烷酸铝、环烷酸镁、环烷酸钡、环烷酸锰、环烷酸锌、环烷酸钒、环烷酸锆、环烷酸锶、油酸锡、叔辛酸铟、二丙烯酸锡、新癸酸钴、2-乙基己酸铜、硬脂酸铁、油酸镍、新癸酸钙、新癸酸钡、十二烷酸铯、亚油酸铅和环烷酸铈组成的组中的至少一种物质组合使用。
7.如权利要求1所述的方法,其中,所述有机酸金属盐相对于所述透明层溶液的总重量为0.01重量%~10重量%。
8.如权利要求1所述的方法,其中,所述银化合物是选自由氧化银、硫氰酸银、硫化银、氯化银、氰化银、氰酸银、碳酸银、硝酸银、亚硝酸银、硫酸银、磷酸银、高氯酸银、四氟硼酸银、乙酰丙酮银、乙酸银、乳酸银、草酸银及其衍生物组成的组中的一种或两种以上物质的混合物。
9.如权利要求1所述的方法,其中,R1~R6选自由氢、甲基、乙基、丙基、异丙基、丁基、异丁基、戊基、己基、乙基己基、庚基、辛基、异辛基、壬基、癸基、十二烷基、十六烷基、十八烷基、二十二烷基、环丙基、环戊基、环己基、烯丙基、羟基、甲氧基、羟基乙基、甲氧基乙基、2-羟基丙基、甲氧基丙基、氰基乙基、乙氧基、丁氧基、己氧基、甲氧基乙氧基乙基、甲氧基乙氧基乙氧基乙基、六亚甲基亚胺、吗啉、哌啶、哌嗪、乙二胺、丙二胺、六亚甲基二胺、三乙二胺、吡咯、咪唑、吡啶、羧甲基、三甲氧基甲硅烷基丙基、三乙氧基甲硅烷基丙基、苯基、甲氧基苯基、氰基苯基、苯氧基、甲苯基、苄基及其衍生物、以及诸如聚烯丙基胺或聚乙烯亚胺这样的聚合物及其衍生物组成的组。
10.如权利要求1所述的方法,其中,化学式2中的氨基甲酸铵类化合物是选自由氨基甲酸铵、乙基氨基甲酸乙基铵、异丙基氨基甲酸异丙基铵、正丁基氨基甲酸正丁基铵、异丁基氨基甲酸异丁基铵、叔丁基氨基甲酸叔丁基铵、2-乙基己基氨基甲酸2-乙基己基铵、十八烷基氨基甲酸十八烷基铵、2-甲氧基乙基氨基甲酸2-甲氧基乙基铵、2-氰基乙基氨基甲酸2-氰基乙基铵、二丁基氨基甲酸二丁基铵、二(十八烷基)氨基甲酸二(十八烷基)铵、甲基癸基氨基甲酸甲基癸基铵、六亚甲基亚胺氨基甲酸六亚甲基亚胺铵、吗啉氨基甲酸吗啉鎓、乙基己基氨基甲酸吡啶鎓、异丙基二氨基甲酸三乙二铵、苄基氨基甲酸苄基铵、三乙氧基甲硅烷基丙基氨基甲酸三乙氧基甲硅烷基丙基铵及其衍生物组成的组中的一种或多种化合物,化学式3中的碳酸铵类化合物是选自由碳酸铵、乙基碳酸乙基铵、异丙基碳酸异丙基铵、正丁基碳酸正丁基铵、异丁基碳酸异丁基铵、叔丁基碳酸叔丁基铵、2-乙基己基碳酸2-乙基己基铵、2-甲氧基乙基碳酸2-甲氧基乙基铵、2-氰基乙基碳酸2-氰基乙基铵、十八烷基碳酸十八烷基铵、二丁基碳酸二丁基铵、二(十八烷基)碳酸二(十八烷基)铵、甲基癸基碳酸甲基癸基铵、六亚甲基亚胺碳酸六亚甲基亚胺铵、吗啉碳酸吗啉铵、苄基碳酸苄基铵、三乙氧基甲硅烷基丙基碳酸三乙氧基甲硅烷基丙基铵、异丙基碳酸三乙二铵及其衍生物组成的组中的一种或多种化合物,化学式4中的碳酸氢铵类化合物是选自由碳酸氢铵、碳酸氢异丙基铵、碳酸氢叔丁基铵、碳酸氢2-乙基己基铵、碳酸氢2-甲氧基乙基铵、碳酸氢2-氰基乙基铵、碳酸氢二(十八烷基)铵、碳酸氢吡啶鎓、碳酸氢三乙二铵及其衍生物组成的组中的一种或多种化合物。
11.如权利要求1所述的方法,其中,所述导电层溶液必要时还包含选自由溶剂、稳定剂、薄膜补充物、分散剂、粘合剂树脂、还原剂、表面活性剂、润湿剂、触变剂或流平剂组成的组中的至少一种添加剂。
12.如权利要求11所述的方法,其中,所述溶剂是选自由水、醇、二醇、乙酸酯、醚、酮、脂肪烃、芳香烃或卤代烃组成的组中的一种或多种物质。
14.如权利要求13所述的方法,其中,所述磷化合物选自由以下化学式5~7表示的化合物:
[化学式5]
R3P
[化学式6]
(RO)3P
[化学式7]
(RO)3PO
其中,化学式5~7中的R是选自碳数为1~20的烷基或芳基中的取代基。
15.如权利要求13所述的方法,其中,所述硫化合物选自由丁硫醇、正己硫醇、二乙硫醚、四氢噻吩、烯丙基二硫化物、巯基苯并噻唑、巯基乙酸烷基酯、四氢噻吩和巯基乙酸辛酯组成的组。
16.如权利要求11所述的方法,其中,所述薄膜补充物是选自由有机酸、有机酸铵盐或有机酸金属盐组成的组中的一种物质或两种以上的混合物。
17.如权利要求16所述的方法,其中,所述有机酸选自由乙酸、草酸、柠檬酸、乳酸、马来酸、丙烯酸、丁酸、戊酸、特戊酸、正己酸、叔辛酸、2-乙基己酸、新癸酸、月桂酸、硬脂酸、油酸、环烷酸、十二烷酸和亚油酸组成的组,所述有机酸金属盐的金属选自由Au、Cu、Zn、Ni、Co、Pd、Pt、Ti、V、Mn、Fe、Cr、Zr、Nb、Mo、W、Ru、Cd、Ta、Re、Os、Ir、Al、Ga、Ge、In、Sn、Sb、Pb、Bi、Sm、Eu、Ac和Th组成的组。
18.如权利要求1所述的方法,所述方法还包括在形成所述导电层之后通过涂布无机氧化物或硫醇化合物以形成保护层的步骤。
19.如权利要求18所述的方法,其中,所述无机氧化物是选自由二氧化硅(SiO2)、氧化钛、氧化锆或氧化锌组成的组中的一种或两种以上的混合物。
20.如权利要求18所述的方法,其中,所述硫醇化合物选自其中引入有碳数为2~24的烷基或芳基的硫醇化合物。
21.如权利要求19所述的方法,其中,所述硫醇化合物是选自由1-己基硫醇、十二烷基硫醇、月桂基硫醇、十六烷基硫醇、十八烷基硫醇、苯并硫醇、巯基乙酸、巯基苄醇、巯基乙醇、巯基***、巯基咪唑、巯基吡啶、巯基苯酚、1,2-乙二硫醇、1,2-丙二硫醇或2,3-二巯基-1-丙醇组成的组中的一种物质或两种以上的混合物。
22.如权利要求1或权利要求18所述的方法,其中,所述涂布步骤选自由旋涂、辊涂、喷涂、浸涂、浇涂、刮刀式分配、喷墨印刷、胶印、丝网印刷、压印、凹版印刷、柔版印刷、刻版印刷、盖印、静电印刷和平版印刷方法组成的组。
23.如权利要求1或权利要求18所述的方法,所述方法还包括在涂布所述透明层溶液之后、涂布所述导电层溶液之后或涂布无机氧化物之后的热处理步骤。
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TW (1) | TWI386955B (zh) |
WO (1) | WO2008153356A2 (zh) |
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-
2007
- 2007-06-15 KR KR1020070059119A patent/KR100856508B1/ko active IP Right Grant
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2008
- 2008-06-13 WO PCT/KR2008/003352 patent/WO2008153356A2/en active Application Filing
- 2008-06-13 JP JP2010512086A patent/JP5260641B2/ja not_active Expired - Fee Related
- 2008-06-13 TW TW097122214A patent/TWI386955B/zh not_active IP Right Cessation
- 2008-06-13 CN CN2008800203738A patent/CN101678658B/zh not_active Expired - Fee Related
- 2008-06-13 US US12/663,933 patent/US9556065B2/en active Active
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Cited By (11)
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CN103189928A (zh) * | 2010-07-30 | 2013-07-03 | 印可得株式会社 | 透明导电膜的制备方法及由其制备的透明导电膜 |
CN103189928B (zh) * | 2010-07-30 | 2016-02-10 | 印可得株式会社 | 透明导电膜的制备方法及由其制备的透明导电膜 |
CN102074281A (zh) * | 2010-12-21 | 2011-05-25 | 苏州禾盛新型材料股份有限公司 | 射频等离子的透明导电膜 |
CN103788592A (zh) * | 2013-12-20 | 2014-05-14 | 安徽国星生物化学有限公司 | 一种高透光率的pet复合材料 |
CN103788592B (zh) * | 2013-12-20 | 2016-02-10 | 安徽国星生物化学有限公司 | 一种高透光率的pet复合材料 |
CN104217819A (zh) * | 2014-09-02 | 2014-12-17 | 上海交通大学 | 一种基于有机金属银盐的导电薄膜及其制备方法 |
CN104443772A (zh) * | 2014-09-25 | 2015-03-25 | 桐城市福润包装材料有限公司 | 一种薄膜 |
CN109935379A (zh) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | 导电薄膜及其制备方法 |
CN109935379B (zh) * | 2017-12-15 | 2020-06-23 | Tcl科技集团股份有限公司 | 导电薄膜及其制备方法 |
CN107967909A (zh) * | 2017-12-25 | 2018-04-27 | 钱月珍 | 防辐射护眼显示屏 |
CN107967909B (zh) * | 2017-12-25 | 2019-11-26 | 深圳市优聚显示技术有限公司 | 防辐射护眼显示屏 |
Also Published As
Publication number | Publication date |
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JP2010531033A (ja) | 2010-09-16 |
CN101678658B (zh) | 2012-06-27 |
JP5260641B2 (ja) | 2013-08-14 |
WO2008153356A2 (en) | 2008-12-18 |
JP5734337B2 (ja) | 2015-06-17 |
JP2014013750A (ja) | 2014-01-23 |
TW200912965A (en) | 2009-03-16 |
US9556065B2 (en) | 2017-01-31 |
KR100856508B1 (ko) | 2008-09-04 |
TWI386955B (zh) | 2013-02-21 |
WO2008153356A3 (en) | 2009-02-12 |
US20100166948A1 (en) | 2010-07-01 |
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