TWI814855B - 透明導電膜 - Google Patents
透明導電膜 Download PDFInfo
- Publication number
- TWI814855B TWI814855B TW108123523A TW108123523A TWI814855B TW I814855 B TWI814855 B TW I814855B TW 108123523 A TW108123523 A TW 108123523A TW 108123523 A TW108123523 A TW 108123523A TW I814855 B TWI814855 B TW I814855B
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- Prior art keywords
- layer
- layers
- transparent conductive
- conductive film
- film
- Prior art date
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- 150000002894 organic compounds Chemical class 0.000 claims abstract description 55
- 229910052751 metal Inorganic materials 0.000 claims abstract description 51
- 239000002184 metal Substances 0.000 claims abstract description 51
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 29
- 239000011701 zinc Substances 0.000 claims abstract description 29
- 239000002019 doping agent Substances 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims description 39
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 27
- 238000003475 lamination Methods 0.000 claims description 23
- 238000000231 atomic layer deposition Methods 0.000 claims description 21
- 238000000151 deposition Methods 0.000 claims description 18
- 230000008021 deposition Effects 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 150000003573 thiols Chemical class 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract 4
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 abstract 2
- 239000010410 layer Substances 0.000 description 146
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 78
- 239000010408 film Substances 0.000 description 48
- 239000011787 zinc oxide Substances 0.000 description 37
- 150000001875 compounds Chemical class 0.000 description 36
- 235000016804 zinc Nutrition 0.000 description 27
- 238000010926 purge Methods 0.000 description 24
- 229910052717 sulfur Inorganic materials 0.000 description 16
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 14
- 239000011593 sulfur Substances 0.000 description 14
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical compound CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 description 12
- 229910052760 oxygen Inorganic materials 0.000 description 11
- 239000002243 precursor Substances 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- -1 polyethylene terephthalate Polymers 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 239000012528 membrane Substances 0.000 description 8
- 229920000139 polyethylene terephthalate Polymers 0.000 description 8
- 239000005020 polyethylene terephthalate Substances 0.000 description 8
- 125000004434 sulfur atom Chemical group 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 4
- 238000005452 bending Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 229920000620 organic polymer Polymers 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000002356 single layer Substances 0.000 description 4
- 238000002207 thermal evaporation Methods 0.000 description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 4
- 229910001868 water Inorganic materials 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- WQABCVAJNWAXTE-UHFFFAOYSA-N dimercaprol Chemical compound OCC(S)CS WQABCVAJNWAXTE-UHFFFAOYSA-N 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910052755 nonmetal Inorganic materials 0.000 description 3
- 150000002843 nonmetals Chemical class 0.000 description 3
- 230000005693 optoelectronics Effects 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- BXAVKNRWVKUTLY-UHFFFAOYSA-N 4-sulfanylphenol Chemical compound OC1=CC=C(S)C=C1 BXAVKNRWVKUTLY-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 2
- 229910052688 Gadolinium Inorganic materials 0.000 description 2
- 229910052689 Holmium Inorganic materials 0.000 description 2
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 229910052777 Praseodymium Inorganic materials 0.000 description 2
- 229910052772 Samarium Inorganic materials 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 229910052775 Thulium Inorganic materials 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 238000004630 atomic force microscopy Methods 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- 229910052790 beryllium Inorganic materials 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- 229910052792 caesium Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical class C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 2
- CEEHFWSNEHHQPJ-UHFFFAOYSA-N ethyl 5-hydroxy-7-oxo-2-phenyl-8-prop-2-enylpyrido[2,3-d]pyrimidine-6-carboxylate Chemical compound N1=C2N(CC=C)C(=O)C(C(=O)OCC)=C(O)C2=CN=C1C1=CC=CC=C1 CEEHFWSNEHHQPJ-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 2
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 125000005647 linker group Chemical group 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229910001507 metal halide Inorganic materials 0.000 description 2
- 150000005309 metal halides Chemical class 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 229910052762 osmium Inorganic materials 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920006254 polymer film Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 229910052702 rhenium Inorganic materials 0.000 description 2
- 229910052703 rhodium Inorganic materials 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 229910052706 scandium Inorganic materials 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- 229910052713 technetium Inorganic materials 0.000 description 2
- 229910052716 thallium Inorganic materials 0.000 description 2
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- REGWTUWFNZIROQ-UHFFFAOYSA-N (1,3-dimethylimidazol-2-ylidene)zinc Chemical compound CN1C(N(C=C1)C)=[Zn] REGWTUWFNZIROQ-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical class [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229920001054 Poly(ethylene‐co‐vinyl acetate) Polymers 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 239000012965 benzophenone Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- AXAZMDOAUQTMOW-UHFFFAOYSA-N dimethylzinc Chemical compound C[Zn]C AXAZMDOAUQTMOW-UHFFFAOYSA-N 0.000 description 1
- 150000004662 dithiols Chemical class 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- HZVOZRGWRWCICA-UHFFFAOYSA-N methanediyl Chemical compound [CH2] HZVOZRGWRWCICA-UHFFFAOYSA-N 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920000636 poly(norbornene) polymer Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920003050 poly-cycloolefin Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920000379 polypropylene carbonate Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- ZGSOBQAJAUGRBK-UHFFFAOYSA-N propan-2-olate;zirconium(4+) Chemical compound [Zr+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] ZGSOBQAJAUGRBK-UHFFFAOYSA-N 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical class SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- JXNCWJJAQLTWKR-UHFFFAOYSA-N zinc;methanolate Chemical compound [Zn+2].[O-]C.[O-]C JXNCWJJAQLTWKR-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/80—Constructional details
- H10K30/81—Electrodes
- H10K30/82—Transparent electrodes, e.g. indium tin oxide [ITO] electrodes
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
- C23C28/3455—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer with a refractory ceramic layer, e.g. refractory metal oxide, ZrO2, rare earth oxides or a thermal barrier system comprising at least one refractory oxide layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/60—Deposition of organic layers from vapour phase
-
- 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
- C03C17/36—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 being a metal
- C03C17/38—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 being a metal at least one coating being a coating of an organic 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/405—Oxides of refractory metals or yttrium
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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Abstract
本發明係關於透明導電膜領域。具體而言，本發明係關於透明導電膜，其包含
(a) 第一壓層，其包含：
- 至少兩個含TiO2
、ZrO2
或HfO2
之層，及
- 含有機化合物之層，其位於該兩個含TiO2
、ZrO2
或HfO2
之層之間，
(b) 金屬層，及
(c) 第二壓層，其包含：
- 至少兩個含ZnO之層，及
- 含有機化合物之層，其位於該兩個含ZnO之層之間，
- 除鋅以外之金屬摻雜劑。
Description
本發明係透明導電膜、特定地有機-無機混成透明導電膜之領域。
透明導電膜廣泛用作光電裝置(例如太陽能電池或發光二極體)中之電極。通常，銦-錫氧化物(ITO)作為導電膜中之材料。然而，ITO膜易碎且因此對於撓性裝置之適用性係有限的。超晶格結構提供另一選擇。
US 5 523 585揭示由在電子運動之方向上週期性重複之第一及第二半導體材料區域形成之超晶格結構。然而，導電性及撓性有限。
US 2011 / 0 212 336 A1揭示具有高電導率之導電壓層。然而，此壓層易碎且因此對彎曲很敏感。
JP 2016 / 012 555 A揭示據說為撓性之透明導電膜。然而，所用金屬氧化物為脆性的，因此不可能在不產生裂紋的情形下以小半徑彎曲。
US 2017 / 0 121 812 A1揭示用於濕氣及氧障壁應用之有機-無機超晶格。然而，其並未指示如何自此途徑獲得透明導電膜。
本發明之目標係提供在彎曲後維持其導電性之透明導電膜。本發明進一步旨在製造該等膜之方法，該方法容易且可靠地產生高品質膜。
該等目標係藉由透明導電膜達成，該透明導電膜包含
(a) 第一壓層，其包含：
- 至少兩個含TiO2
、ZrO2
或HfO2
之層，及
- 含有機化合物之層，其位於該兩個含TiO2
、ZrO2
或HfO2
之層之間，
(b) 金屬層，及
(c) 第二壓層，其包含：
- 至少兩個含ZnO之層，及
- 含有機化合物之層，其位於該兩個含ZnO之層之間，
- 除鋅以外之金屬摻雜劑。
本發明進一步係關於製備透明導電膜之方法，其包含將以下各項沈積於基板上
(a) 第一壓層，其包含：
- 至少兩個含TiO2
、ZrO2
或HfO2
之層，及
- 含有機化合物之層，其位於該兩個含TiO2
、ZrO2
或HfO2
之層之間，
(b) 金屬層，及
(c) 第二壓層，其包含：
- 至少兩個含ZnO之層，及
- 含有機化合物之層，其位於該兩個含ZnO之層之間，
- 除鋅以外之金屬摻雜劑。
本發明進一步係關於本發明之膜在光電裝置中作為電極之用途。
本發明之較佳實施例可參見實施方式及申請專利範圍。不同實施例之組合屬本發明之範圍內。
本發明之膜係透明的。在本發明之情形中，透明意指導電金屬氧化物膜透射平行於表面法線照射於膜上之波長為550 nm的光之強度的至少50%、更佳至少70%、特定地至少80%。
本發明之膜係導電的，此意味著該膜具導電性。較佳地，膜之薄片電阻為1 000 Ω/sq或以下、更佳500 Ω/sq或以下、甚至更佳200 Ω/sq或以下、特定地100 Ω/sq或以下。較佳地，膜之電阻率為0.01 Ω·cm或以下、更佳3 · 10-3
Ω·cm或以下、甚至更佳10-3
Ω·cm或以下、特定地3 · 10-4
Ω·cm或以下。薄片電阻及電阻率二者通常均係在20℃之溫度下量測。較佳地，膜之薄片電阻及電阻率係使用四點探針技術量測。
本發明之膜包含第一壓層，其包含：含有TiO2
、ZrO2
或HfO2
、較佳TiO2
之層。較佳地，該等層含有至少50 wt.-% TiO2
、ZrO2
或HfO2
、更佳至少70 wt.-% TiO2
、ZrO2
或HfO2
、特定地至少90 wt.-% TiO2
、ZrO2
或HfO2
。含TiO2
、ZrO2
或HfO2
之層可為非晶形、部分結晶或結晶，較佳其係結晶。該至少兩個含TiO2
、ZrO2
或HfO2
之層可具有相同厚度或不同厚度，較佳地其具有相同厚度。含TiO2
、ZrO2
或HfO2
之層較佳具有0.1至100 nm、更佳1至10 nm、特定地2至5 nm之厚度。較佳地，含TiO2
、ZrO2
或HfO2
之層具有均勻厚度，此意味著在層之最厚位置之厚度小於最薄位置之厚度的2倍、更佳小於最薄位置之厚度的1.5倍。本發明之膜包含至少兩個含TiO2
、ZrO2
或HfO2
之層，較佳至少三個、更佳至少五個、特定地至少十個層。
第一壓層進一步包含含有機化合物之層。若膜包含多於兩個含TiO2
、ZrO2
或HfO2
之層，則該膜較佳交替地包含含TiO2
、ZrO2
或HfO2
之層及含有機化合物之層，使得每一含有機分子之層位於兩個含TiO2
、ZrO2
或HfO2
之層之間，其中其他層可位於該等層之間。含有機化合物之層較佳較含TiO2
、ZrO2
或HfO2
之層薄。若存在多於一個含有機化合物之層，則其可具有相同厚度或不同厚度，較佳其具有相同厚度。含有機化合物之層較佳具有0.05至5 nm、更佳0.1至1 nm之厚度。含有機化合物之層可為單層(即，具有約一個分子之厚度)或亞單層。
含有機化合物之層較佳含有多於98 wt.-%之非金屬、較佳多於99 wt.-%，特定地完全或基本上完全為非金屬。甚至更佳地，非金屬係C、H、O、N、S、Se及/或P。含有機化合物之層可含有一種有機化合物或多於一種有機化合物，例如兩種或三種。含有機化合物之層較佳含有含硫化合物。含硫化合物中之硫較佳呈氧化態-2、-1或0，其為負二、負一或零，例如有機硫醇、有機硫醚或有機二甲基二硫醚。有機硫醇係較佳的。含硫化合物可含有一個或一個以上硫原子。較佳地，含硫化合物含有一個硫原子。更佳地，含硫化合物係芳香族硫醇。硫醇可直接或經由連接體(例如亞甲基)鍵結至分子之芳香族部分，較佳地其直接鍵結至芳香族基團。含硫化合物甚至更佳地係硫酚衍生物。較佳地，含硫分子進一步含有一或多個羥基。下文給出含硫化合物之一些較佳實例。
尤佳者係4-巰基苯酚(C-1)、4-巰基苯甲醇(C-2)及2,3-二巰基丙醇(C-15)。亦可製得具有不同有機分子之有機層，前提係至少一種有機分子係含硫分子。
較佳地，含硫化合物含有至少兩個硫原子、更佳兩個硫原子。含硫化合物中之硫原子彼此獨立地係如上文所闡述官能基之部分。較佳者係硫醇，更佳者係二硫酚。較佳地，兩個硫醇基團直接或經由連接體(例如亞甲基)連接至芳香族系統(例如苯)。下文給出含有兩個硫原子之含硫化合物之一些較佳實例。
若含有機化合物之層中之有機化合物含有羥基、硫醇或可去質子化之其他基團，則該基團可保持質子化或其可經去質子化並締合至金屬，或一些經質子化且一些去質子化並締合至金屬。
第一壓層具有高相對介電係數。較佳地，在室溫及1 MHz下之相對介電係數係至少10、更佳至少20、特定地至少50。第一壓層之厚度較佳為2至60 nm、更佳5至40 nm、特定地10至30 nm。
本發明之膜進一步包含金屬層。金屬層可含有Li、Be、Na、Mg、Al、K、Ca、Sc、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Ga、Rb、Sr、Y、Zr、Nb、Mo、Tc、Ru、Rh、Pd、Ag、Cd、In、Sn、Cs、Ba、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Hf、Ta、W、Re、Os、Ir、Pt、Au、Hg、Tl、Bi。較佳地，金屬層含有Al、Cu、Ag、Au，特定地Ag。膜可含有一種金屬或多於一種(例如兩種或三種)金屬。金屬層具有較佳至少105
S/m、更佳至少106
S/m、特定地至少107
S/m之金屬導電率。金屬層與第一壓層之間可存在其他層。然而，較佳地，金屬層與第一壓層接觸。金屬層足夠薄以允許可見光透射，較佳金屬層之厚度為1至100 nm、更佳2至50 nm、甚至更佳3至30 nm、特定地5至20 nm，例如8至15 nm，例如10 nm。
本發明之膜包含第二壓層，其含有至少兩個含有ZnO (即氧化鋅)之層。較佳地，該等層含有至少50 wt.-% ZnO、更佳至少70 wt.-% ZnO、特定地至少90 wt.-% ZnO。含ZnO之層可為非晶形、部分結晶或結晶，較佳其係結晶。至少兩個含ZnO之層可具有相同厚度或不同厚度，較佳其具有相同厚度。含ZnO之層較佳具有0.1至100 nm、更佳1至10 nm、特定地2至5 nm之厚度。較佳地，含ZnO之層具有均勻厚度，此意味著在層之最厚位置處之厚度小於最薄位置處厚度的2倍、更佳小於最薄位置處厚度的1.5倍。本發明之膜包含至少兩個含ZnO之層，較佳至少三個、更佳至少五個、特定地至少十個。
第二壓層進一步包含含有機化合物之層。若膜包含多於兩個含ZnO之層，則膜較佳交替地包含含ZnO之層及含有機化合物之層，使得含有機分子之各層位於兩個含ZnO之層之間，其中其他層可位於該等層之間。含有機化合物之層較佳較含ZnO之層薄。若存在多於一個含有機化合物之層，則其可具有相同厚度或不同厚度，較佳其具有相同厚度。含有機化合物之層較佳具有0.05至5 nm、更佳0.1至1 nm之厚度。含有機化合物之層可為單層(即，具有約一個分子之厚度)或亞單層。
關於第一壓層中之有機化合物之相同定義及較佳實施例適用於第二壓層。第一壓層中之有機化合物可為與第二壓層中相同之有機化合物或其可不同，較佳其係相同的。
第二壓層進一步包含除鋅以外之金屬摻雜劑。金屬摻雜劑可為Li、Be、Na、Mg、Al、K、Ca、Sc、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Ga、Rb、Sr、Y、Zr、Nb、Mo、Tc、Ru、Rh、Pd、Ag、Cd、In、Sn、Cs、Ba、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Hf、Ta、W、Re、Os、Ir、Pt、Au、Hg、Tl、Bi。較佳地，金屬摻雜劑為Mo、Ta、In、V、Sn、W、Mn、Al、Ga、Ti、Zr或Hf，特定地Al。膜可含有除鋅以外之一種金屬摻雜劑或多於一種(例如兩種或三種)金屬摻雜劑。
膜通常含有較鋅少之金屬摻雜劑。較佳地，金屬摻雜劑與鋅之原子比為10-10
至0.1、更佳10-9
至0.01、特定地10-8
至10-3
。對金屬摻雜劑之放置位置沒有特別限制，此乃因據信至少一部分金屬摻雜劑可在膜中遷移。然而，金屬摻雜劑之濃度較佳在含氧化鋅之層與含有機化合物之層之間之界面處最高。
金屬層與第二壓層之間可存在其他層。然而，較佳地，金屬層與第二壓層接觸。因此，金屬層通常位於第一壓層與第二壓層之間，較佳地其位於第一壓層與第二壓層之間並與第一壓層與第二壓層直接接觸。第二壓層之厚度較佳為10至100 nm、更佳20至80 nm、特定地30至60 nm，例如35至50 nm。
膜較佳包含基板、特定地透明基板。基板較佳面向第一壓層，特定地第一壓層與基板接觸。可使用各種透明基板，例如玻璃或聚合物。較佳者係聚合物。聚合物包括聚酯，例如聚對苯二甲酸乙二酯(PET)或聚乙烯萘-二甲酸(PEN)；聚醯亞胺；聚丙烯酸酯，例如聚甲基丙烯酸甲酯(PMMA)；聚丙烯醯胺；聚碳酸酯，例如聚(雙酚A碳酸酯)；聚乙烯醇及其衍生物，如聚乙酸乙烯酯或聚乙烯醇縮丁醛；聚氯乙烯；聚烯烴，例如聚乙烯(PE)或聚丙烯(PP)；聚環烯，例如聚降莰烯；聚醚碸；聚醯胺，如聚己內醯胺或聚(六亞甲基己二酸醯胺)；纖維素衍生物，例如羥乙基纖維素、羥丙基纖維素、甲基纖維素、甲基羥丙基纖維素或硝基纖維素；聚胺基甲酸酯；環氧樹脂；三聚氰胺甲醛樹脂；酚甲醛樹脂。聚合物包括共聚物，例如聚(乙烯-共-降莰烯)或聚(乙烯-共-乙酸乙烯酯)。較佳者係聚酯及聚環烯。
基板可具有任何大小及形狀。較佳地，基板係膜。基板膜之厚度取決於應用。若障壁膜以大於10 mm之半徑彎曲，則基板膜之厚度較佳為100至1000 µm，更佳100至500 µm，例如100至200 µm。若障壁膜以小於10 mm之半徑彎曲，則基板膜之厚度較佳為1至100 µm，更佳10至70 µm，例如40至60 µm。
基板之表面較佳具有高平面性。在本發明之上下文中，高平面性意指表面上之最高點較表面上之最低點高不超過100 nm，較佳不超過50 nm。可利用原子力顯微術、較佳以輕敲模式量測平面性。
基板通常由於(例如)小劃痕或粒子(例如黏著至其表面之粉塵)而不具有高平面性。因此，障壁膜較佳進一步包含平面化層以避免損壞(例如刺穿)壓層。更佳地，平面化層在基板與壓層之間。在此情形中，平面化層可另外用於更好地將基板及壓層固持在一起，尤其在彎曲或加熱時。平面化層可包含有機聚合物(例如丙烯酸酯或環氧樹脂)、陶瓷(例如碳化物，例如SiC)或有機-無機雜合材料(例如聚烷基矽氧烷)。較佳者係有機聚合物。
通常，藉由以下製備平面化層：將構成平面化層之材料沈積於基板上，之後施加壓層。在有機聚合物之情形中，將包含單體之液體澆注於基板上，且然後藉由(例如)加熱或UV起始進行固化。較佳者係UV起始，更佳地，包含單體之液體進一步包含固化助劑，例如經官能化之二苯甲酮。較佳地，包含單體之液體包含單官能及雙官能單體之混合物使得在固化後獲得交聯有機聚合物。通常藉由將材料濺鍍至基板上獲得包含陶瓷之平面化層。包含有機-無機雜合材料之平面化層可藉由以下獲得：將包含有機-無機前體之溶液澆注於基板上，蒸發溶劑並藉由(例如)加熱使有機-無機前體凝結。此方法通常稱作溶膠-凝膠法。有機-無機前體之實例係烷基-三烷氧基矽烷。較佳地，利用UV可固化側基(例如丙烯酸酯)官能化前體。以此方式，可使有機-無機雜合材料交聯。
較佳地，構成平面化層之材料之彈性模數介於基板材料與壓層之間，例如10 GPa至30 GPa。測定彈性模數之方法闡述於ISO 527-1 (Plastics – Determination of tensile properties, 2012)中。
本發明之膜對機械應力或應變特別不敏感。較佳地，在膜以0.5 cm之半徑彎曲500次之後，膜之薄片電阻增加小於50%。
本發明之膜可以各種方式製作。層可自溶液或蒸氣沈積。蒸氣沈積方法係較佳的。該等方法包括化學氣相沈積(CVD)、熱蒸發、濺鍍或原子層沈積(ALD)。亦可將不同方法組合，例如藉由利用抑制方法沈積某些層及利用不同方法沈積其他層。ALD較佳用於第一及第二壓層之沈積。熱蒸發、濺鍍及ALD較佳用於金屬層，特定地熱蒸發。為簡單起見，在本發明之上下中，ALD包含原子層沈積以及分子層沈積二者或其混合物。
實施該方法之典型壓力在1500至10-5
毫巴(mbar)、較佳100至10-3
毫巴、更佳10至0.1毫巴之範圍內。因此，較佳在可調節壓力之設備中(例如在真空室中)運行該方法。該方法之溫度係在-20至500℃、較佳0至300℃、特定地50至220℃之範圍內。
為沈積含TiO2
、ZrO2
或HfO2
之層，可使用各種含有Ti-、Zr-或Hf-之化合物。較佳地，使用含有金屬-有機金屬之化合物，例如烷基金屬；金屬烷氧基化物，例如四異丙氧基鋯；環戊二烯加合物，例如二茂鈦；金屬碳烯；金屬鹵化物，例如四氯化鈦；一氧化碳錯合物。較佳者係金屬鹵化物、特定地氯化物。
為沈積含ZnO之層，可使用各種含鋅化合物。較佳地，使用含有金屬-有機鋅之化合物，例如，烷基鋅，例如二甲基鋅；鋅烷氧基化物，例如二甲氧基鋅；環戊二烯加合物，例如二茂鋅；鋅碳烯，例如N,N’-二甲基咪唑-2-亞基鋅；鋅鹵化物，例如氯化鋅。更佳地，含鋅化合物係烷基鋅、特定地C1
至C4
烷基鋅。
所沈積之含鋅化合物通常必須轉化為氧化鋅。此可藉由較佳在氧之存在下加熱高於含鋅化合物之分解溫度達成。較佳地，所沈積含鋅化合物係藉由使其與含氧化合物(例如氧、臭氧或氧電漿)接觸來分解。
若含ZnO之層係藉由ALD製得，則較佳將包含沈積含鋅化合物並藉由使其與含氧化合物接觸而沈積之序列進行至少一次、較佳至少五次、更佳至少10次、特定地至少20次。通常，該序列實施不超過1000次。
為沈積含有機化合物之層，較佳可使用上述化合物。較佳地，有機化合物係沈積於所沈積金屬-有機化合物上。然而，若有機化合物沈積於含氧化鋅之層上，則含氧化鋅之層的表面係反應性的，例如由於所沈積之含鋅化合物尚未與含氧化合物接觸。
較佳地，製備第二壓層之方法包含含有以下之序列：沈積含氧化鋅之層，沈積含有機化合物之層及沈積除鋅以外之金屬摻雜劑，其中該序列實施一次或較佳多於一次，例如至少兩次、至少三次、至少五次或特別地至少十次，且然後沈積另一層含氧化鋅之層。該序列可具有以下順序
(1) 沈積含氧化鋅之層
(2) 沈積含有機化合物之層，及
(3) 沈積除鋅以外之金屬摻雜劑。
或者，該序列可具有以下順序
(1) 沈積含氧化鋅之層
(2) 沈積除鋅以外之金屬摻雜劑，及
(3) 沈積含有機化合物之層。
該序列可包含例如以以下順序沈積除鋅以外之金屬摻雜劑兩次
(1) 沈積含氧化鋅之層
(2) 沈積除鋅以外之金屬摻雜劑，
(3) 沈積含有機化合物之層，及
(4) 沈積除鋅以外之金屬摻雜劑。
若該方法係ALD方法，通常，表面在一個ALD循環中暴露於含鋅化合物或有機化合物達1 ms至30 s、較佳10 ms至5 s、特定地50 ms至1 s。在將表面暴露於含(半)金屬之化合物或不同化學結構之含硫化合物之間，較佳利用惰性氣體吹掃基板達通常地0.1 s至10 min、較佳1 s至3 min、特定地10 s至1 min。
較佳地，本發明之方法係作為空間ALD方法實施，即，含鋅化合物、含金屬化合物、有機化合物及含氧化合物穿過相對於基板移動之單獨孔口。此意味著基板移動且孔口保持不動，或在孔口移動的同時基板保持不動，或基板及孔口二者均移動。較佳地，移動速度為0.01至10 m/s、更佳0.02至1 m/s、特定地0.05至0.3 m/s。孔口經配置，使得含鋅化合物、含金屬化合物、有機化合物及含氧化合物以如針對上述方法所述之順序撞擊基板之表面。為避免氣相中之反應，較佳將惰性氣體(例如氮氣或氬氣)穿過其朝向基板表面之孔口放置於含鋅化合物、含金屬化合物、含氧化合物及有機化合物穿過之該等孔口之間。
較佳地，孔口安裝於旋轉鼓上，基板圍繞旋轉鼓放置、較佳移動。此一設備闡述於WO 2011 / 099 858 A1中。在基板具有撓性之情形中，有機-無機基板由此可以所謂的捲對捲方法沈積於大基板上。
本發明之膜可用作光電裝置中之電極。光電裝置之實例包括發光二極體、雷射、太陽能電池或光學感測器。
實例
基板製備
聚合物膜基板係自聚對苯二甲酸乙二酯(PET)膜(厚度：125 µm)切割。將PET聚合物膜基板用丙酮、乙醇、去離子水清潔，並用氮吹乾以去除污染物。
表徵
含氧化鋅之層的厚度係使用光譜橢圓偏光計(FS-1多波長橢圓偏光計, Film Sense)量測。藉由原子力顯微鏡(AFM, XE-100)研究膜形態。膜之導電性係使用四點探針技術(HP4155C, Agilent Technologies)量測。UV-可見光譜係使用UV-VIS光譜儀(UV-VIS 8453, Agilent Technologies)獲得。
實例1 (比較)
TiO2
係使用氯化鈦(IV) (TiCl4
)及去離子水(H2
O)作為ALD前體沈積於PET基板上。氬(Ar)充當載體及吹掃氣體二者。將DEZ及H2
O在20℃下蒸發。循環係由1 s暴露於DEZ、5 s Ar吹掃、1 s暴露於H2
O及5 s Ar吹掃組成。Ar之總流速為100 sccm。在此程序期間，溫度在400毫巴之壓力下維持在100℃。將循環實施875次，獲得35 nm厚度之TiO2
膜。
藉由熱蒸發將Ag層沈積於TiO2
膜上。
使用二乙基鋅(DEZ)及去離子水(H2
O)作為ALD前體將含氧化鋅之層沈積於Ag層上。氬(Ar)充當載體及吹掃氣體二者。將DEZ及H2
O在20℃下蒸發。循環係由1 s暴露於DEZ、5 s Ar吹掃、1 s暴露於H2
O及5 s Ar吹掃組成。Ar之總流速為100 sccm。在此程序期間，溫度在400毫巴之壓力下維持在100℃。ZnO薄膜藉由ALD方法之生長速率為1.5 Å/循環。將循環實施233次。
隨後，使用三甲基鋁(TMA, Sigma Aldrich: 99%)及4-巰基苯酚(4MP, Sigma Aldrich: 97%)作為前體製得含有機化合物之層。將反應溫度降至145℃。Ar充當載體及吹掃氣體二者。分別在20℃及80℃下蒸發TMA及4MP。ALD循環係由1 s暴露於TMA、5 s Ar吹掃、5 s暴露於4MP、60 s Ar吹掃、1 s暴露於TMA及5 s Ar吹掃組成。將此循環實施一次。
實例2 (比較)
如同實例1在PET基板上沈積TiO2
膜及Ag膜。使用二乙基鋅(DEZ)及去離子水(H2
O)作為ALD前體將含氧化鋅之層沈積於Ag層上。氬(Ar)充當載體及吹掃氣體二者。將DEZ及H2
O在20℃下蒸發。循環係由1 s暴露於DEZ、5 s Ar吹掃、1 s暴露於H2
O及5 s Ar吹掃組成。Ar之總流速為100 sccm。在此程序期間，溫度在400毫巴之壓力下維持在100℃。ZnO薄膜藉由ALD方法之生長速率為1.5 Å/循環。將循環實施233次。
隨後，使用三甲基鋁(TMA, Sigma Aldrich: 99%)及2,3-二巰基-1-丙醇(DMP, Sigma Aldrich: 98%)作為前體製得含有機化合物之層。將反應溫度降至145℃。Ar充當載體及吹掃氣體二者。分別在20℃及80℃下蒸發TMA及4MP。ALD循環係由1 s暴露於TMA、5 s Ar吹掃、5 s暴露於4MP、60 s Ar吹掃、1 s暴露於TMA及5 s Ar吹掃組成。此循環實施一次。
將如上所述用於含氧化鋅之層及含有機化合物之層之沈積製程交替實施14次，獲得厚度為35 nm之第二壓層。
實例3 (本發明)
藉由使用氯化鈦(IV)(TiCl4
)及去離子水(H2
O)作為ALD前體首先沈積TiO2
層在PET基板上製得第一壓層。氬(Ar)充當載體及吹掃氣體二者。將DEZ及H2
O在20℃下蒸發。循環係由1 s暴露於DEZ、5 s Ar吹掃、1 s暴露於H2
O及5 s Ar吹掃組成。Ar之總流速為100 sccm。在此程序期間，溫度在400毫巴之壓力下維持在100℃。TiO2
薄膜藉由ALD方法之生長速率為1.5 Å/循環。循環實施266次。
隨後，使用氯化鈦(IV)(TiCl4
)及2,3-二巰基-1-丙醇(DMP, Sigma Aldrich: 98%)作為前體製得含有機化合物之層。將反應溫度降至145℃。Ar充當載體及吹掃氣體二者。分別在20℃及80℃下蒸發TiCl4
及DMP。ALD循環係由1 s暴露於TiCl4
、5 s Ar吹掃、5 s暴露於DMP、60 s Ar吹掃、1 s暴露於TiCl4
及5 s Ar吹掃組成。此循環實施一次。
將如上所述用於含有TiO2
之層及含有機化合物之層之沈積製程交替實施7次，獲得厚度為19 nm之第一壓層。
在第一壓層上，沈積如實例1中之Ag層及如實例2中之第二層壓板，不同之處在於第二壓層之厚度為40 nm，此乃因如前所述含氧化鋅之層及含有機化合物之層交替執行16次。
實例4 (本發明)
重複實例3，其中第一不同之處在於第一壓層具有24 nm之厚度，此乃因如前所述含TiO2
之層及含有機化合物之層的沈積交替執行11次。第二不同之處在於第二壓層具有45 nm之厚度，此乃因如前所述含氧化鋅之層及含有機化合物之層交替執行18次。
薄片電阻
在沈積後、在以0.5 cm之半徑彎曲500次及1000次之後量測實例1至4中所獲得膜之薄片電阻。
Claims (15)
- 一種透明導電膜，其包含(a)第一壓層，其包含：至少兩個含TiO2、ZrO2或HfO2之層，及含有機化合物之層，其位於該兩個含TiO2、ZrO2或HfO2之層之間，(b)金屬層，及(c)第二壓層，其包含：至少兩個含ZnO之層，含有機化合物之層，其位於該兩個含ZnO之層之間，除鋅以外之金屬摻雜劑。
- 如請求項1之透明導電膜，其中該等含TiO2、ZrO2或HfO2之層具有1至10nm之厚度。
- 如請求項1之透明導電膜，其中該等含ZnO之層具有1至10nm之厚度。
- 如請求項1至3中任一項之透明導電膜，其中該金屬層含有Al、Cu、Ag或Au。
- 如請求項1至3中任一項之透明導電膜，其中該金屬層具有3至30nm之厚度。
- 如請求項5之透明導電膜，其中該有機化合物係有機硫醇。
- 如請求項1至3中任一項之透明導電膜，其中該第一壓層具有5至40nm之厚度。
- 如請求項1至3中任一項之透明導電膜，其中該膜進一步包含透明撓性基板。
- 如請求項1至3中任一項之透明導電膜，其中該膜具有200Ω/sq或以下之薄片電阻。
- 如請求項1至3中任一項之透明導電膜，其中該膜具有0.02Ω．cm或以下之電阻率。
- 如請求項1至3中任一項之透明導電膜，其中在該膜以1cm之半徑彎曲500次之後，該膜之該薄片電阻增加小於10%。
- 一種製備透明導電膜之方法，其包含在基板上沈積以下各項(a)第一壓層，其包含：至少兩個含TiO2、ZrO2或HfO2之層，及含有機化合物之層，其位於該兩個含TiO2、ZrO2或HfO2之層之間，(b)金屬層，及 (c)第二壓層，其包含：至少兩個含ZnO之層，及含有機化合物之層，其位於該兩個含ZnO之層之間，除鋅以外之金屬摻雜劑。
- 如請求項12之方法，其中該沈積係藉由原子層沈積實施。
- 如請求項12或13之方法，其中該沈積係在100至220℃之溫度下實施。
- 一種如請求項1至11中任一項之透明導電膜在光電裝置中作為電極之用途。
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| EP (1) | EP3818192B1 (zh) |
| JP (1) | JP7451486B2 (zh) |
| KR (1) | KR20210029186A (zh) |
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| KR20210029186A (ko) | 2021-03-15 |
| TW202006752A (zh) | 2020-02-01 |
| EP3818192B1 (en) | 2024-05-15 |
| CN112334602A (zh) | 2021-02-05 |
| WO2020007900A1 (en) | 2020-01-09 |
| US20210269917A1 (en) | 2021-09-02 |
| EP3818192A1 (en) | 2021-05-12 |
| JP7451486B2 (ja) | 2024-03-18 |
| JP2021529884A (ja) | 2021-11-04 |
| CN112334602B (zh) | 2023-06-30 |
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