CN109817381B - Preparation method of copper grid composite ionic liquid gel flexible transparent electrode - Google Patents
Preparation method of copper grid composite ionic liquid gel flexible transparent electrode Download PDFInfo
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- CN109817381B CN109817381B CN201711163610.3A CN201711163610A CN109817381B CN 109817381 B CN109817381 B CN 109817381B CN 201711163610 A CN201711163610 A CN 201711163610A CN 109817381 B CN109817381 B CN 109817381B
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 132
- 239000010949 copper Substances 0.000 title claims abstract description 132
- 239000002608 ionic liquid Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 239000000758 substrate Substances 0.000 claims abstract description 62
- 239000010410 layer Substances 0.000 claims abstract description 43
- 239000011241 protective layer Substances 0.000 claims abstract description 30
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 164
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 145
- 229910052709 silver Inorganic materials 0.000 claims description 145
- 239000004332 silver Substances 0.000 claims description 145
- 239000002105 nanoparticle Substances 0.000 claims description 139
- 239000000243 solution Substances 0.000 claims description 103
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 84
- 239000006185 dispersion Substances 0.000 claims description 77
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 71
- 239000007788 liquid Substances 0.000 claims description 69
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 61
- 238000005234 chemical deposition Methods 0.000 claims description 49
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 42
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 36
- -1 polyethylene terephthalate Polymers 0.000 claims description 35
- 239000012046 mixed solvent Substances 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 27
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 18
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 18
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 18
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 18
- 239000002202 Polyethylene glycol Substances 0.000 claims description 16
- 229920001223 polyethylene glycol Polymers 0.000 claims description 16
- 230000035484 reaction time Effects 0.000 claims description 16
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 15
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 claims description 15
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 15
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims description 15
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical group O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 239000008098 formaldehyde solution Substances 0.000 claims description 14
- 239000011229 interlayer Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 239000001476 sodium potassium tartrate Substances 0.000 claims description 14
- 125000001889 triflyl group Chemical group FC(F)(F)S(*)(=O)=O 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- PBKADZMAZVCJMR-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;dihydrate Chemical compound O.O.OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O PBKADZMAZVCJMR-UHFFFAOYSA-N 0.000 claims description 13
- RWRDLPDLKQPQOW-UHFFFAOYSA-N Pyrrolidine Chemical group C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 claims description 9
- 238000006116 polymerization reaction Methods 0.000 claims description 9
- 239000003431 cross linking reagent Substances 0.000 claims description 7
- 239000000178 monomer Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical group C1CCNCC1 NQRYJNQNLNOLGT-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
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 6
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 5
- 239000003999 initiator Substances 0.000 claims description 5
- 229920000831 ionic polymer Polymers 0.000 claims description 5
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 4
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000004642 Polyimide Substances 0.000 claims description 4
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 claims description 4
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 claims description 4
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 claims description 4
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 4
- 239000012965 benzophenone Substances 0.000 claims description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 4
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Chemical compound CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 4
- 150000004714 phosphonium salts Chemical group 0.000 claims description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 4
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 4
- 229920000515 polycarbonate Polymers 0.000 claims description 4
- 239000004417 polycarbonate Substances 0.000 claims description 4
- 229920001721 polyimide Polymers 0.000 claims description 4
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 4
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 4
- 239000004800 polyvinyl chloride Substances 0.000 claims description 4
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 4
- 230000000977 initiatory effect Effects 0.000 claims description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 3
- OTKCEEWUXHVZQI-UHFFFAOYSA-N 1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(=O)CC1=CC=CC=C1 OTKCEEWUXHVZQI-UHFFFAOYSA-N 0.000 claims description 2
- KMNCBSZOIQAUFX-UHFFFAOYSA-N 2-ethoxy-1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(OCC)C(=O)C1=CC=CC=C1 KMNCBSZOIQAUFX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- 239000004793 Polystyrene Substances 0.000 claims description 2
- PTWCMKMXLQGFND-UHFFFAOYSA-N [N+](=O)(O)[O-].C(=C)N1CN(C=C1)CCC(=O)O Chemical compound [N+](=O)(O)[O-].C(=C)N1CN(C=C1)CCC(=O)O PTWCMKMXLQGFND-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 2
- 125000005442 diisocyanate group Chemical group 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 2
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 238000004528 spin coating Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims 1
- 150000003949 imides Chemical class 0.000 claims 1
- 229920002521 macromolecule Polymers 0.000 claims 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 1
- 238000002834 transmittance Methods 0.000 abstract description 14
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 230000007774 longterm Effects 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 3
- 238000007639 printing Methods 0.000 description 41
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 38
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 30
- 238000011049 filling Methods 0.000 description 13
- 238000001914 filtration Methods 0.000 description 13
- 239000012528 membrane Substances 0.000 description 13
- 238000002156 mixing Methods 0.000 description 13
- 239000000843 powder Substances 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 12
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 12
- 238000001291 vacuum drying Methods 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 6
- OLLPKNZMCHWPAY-UHFFFAOYSA-N [Br-].C(CCC)C(=C(CCCC)CCCC)[PH3+] Chemical compound [Br-].C(CCC)C(=C(CCCC)CCCC)[PH3+] OLLPKNZMCHWPAY-UHFFFAOYSA-N 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 3
- 238000007641 inkjet printing Methods 0.000 description 3
- OVBJJZOQPCKUOR-UHFFFAOYSA-L EDTA disodium salt dihydrate Chemical compound O.O.[Na+].[Na+].[O-]C(=O)C[NH+](CC([O-])=O)CC[NH+](CC([O-])=O)CC([O-])=O OVBJJZOQPCKUOR-UHFFFAOYSA-L 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- GSGPKPPQAOUFFT-UHFFFAOYSA-M [Br-].C(=C)[N+]1(CCCCC1)C Chemical compound [Br-].C(=C)[N+]1(CCCCC1)C GSGPKPPQAOUFFT-UHFFFAOYSA-M 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical group [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 150000003053 piperidines Chemical class 0.000 description 1
- 229940074439 potassium sodium tartrate Drugs 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 150000003235 pyrrolidines Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- KSGONWKRYBVWGZ-UHFFFAOYSA-M tributyl(ethenyl)phosphanium;bromide Chemical compound [Br-].CCCC[P+](CCCC)(CCCC)C=C KSGONWKRYBVWGZ-UHFFFAOYSA-M 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/40—Electrodes ; Multistep manufacturing processes therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/68—Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
- H01L29/76—Unipolar devices, e.g. field effect transistors
- H01L29/772—Field effect transistors
- H01L29/78—Field effect transistors with field effect produced by an insulated gate
- H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/36—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the electrodes
- H01L33/40—Materials therefor
- H01L33/42—Transparent materials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to a preparation method of a copper grid composite ionic liquid gel flexible transparent electrode. The invention discloses a preparation method of the flexible transparent electrode, which improves the oxidation resistance of the electrode through an ionic liquid gel protective layer. The copper grid composite ionic liquid gel flexible transparent electrode provided by the invention comprises a commercial polymer flexible transparent substrate, a copper grid in the middle layer and ionic liquid gel in the outer layer, and has the characteristics of low cost, good light transmittance and long-term stability, and the resistance of the transparent flexible electrode is adjustable.
Description
Technical Field
The invention belongs to the field of preparation and application of electronic devices, and relates to a preparation method of a copper grid composite ionic liquid gel flexible transparent electrode.
Background
As an important component of optoelectronic devices, such as wearable electronic devices, flexible display screens, solar cells, thin film transistors, organic electroluminescent panels, and the like, flexible transparent electrodes face enormous opportunities and challenges. At present, the flexible transparent electrode is mainly prepared by a sol-gel method, chemical vapor deposition, vacuum evaporation deposition, sputtering deposition, pulse laser deposition and the like on a transparent organic polymer substrate to prepare a conductive film (nat. nanotechnol.2013,8, 421-. The conductive thin film that dominates the transparent electrode market is Indium Tin Oxide (ITO), which has not been able to meet the requirements of new flexible electronic devices due to its rigid and brittle characteristics, and limitations of indium resource scarcity, high cost of the manufacturing process, etc. In recent years, carbon nanotubes, graphene, and metal nanomaterials (including silver and copper) are successively used to replace ITO to prepare flexible transparent electrode materials. Among them, the preparation of carbon nanotube conductive thin films with low cost, high quality and uniform dispersion on a large scale still faces huge challenges, and the high cost and the uneven conductivity of high-quality graphene also limit the application of graphene materials in the field of flexible transparent electrodes (chem.rev.2016,116, 13413-13453; adv.mater.2016,28, 9491-9497). Compared with a carbon-based electrode material, the metal nano-material transparent electrode has excellent conductivity and optical characteristics, can be prepared by a low-cost solution method, and is widely concerned by research institutions and the industry. However, silver nanomaterials are expensive and are easily sulfided to reduce conductivity (nat. commun.2016, 11402). The conductivity of copper is close to that of silver, but the storage capacity of copper is more than 1000 times of that of silver, the price of copper is only one percent of that of silver, and the copper has wider application prospect. Similar to the sulfidation of silver nanomaterials, copper nanomaterials are also susceptible to oxidation (Nano res.2016,9, 2138-. Therefore, a simple, convenient and economic method is sought to improve the oxidation resistance of the flexible transparent electrode made of the copper nano material, the problems of resource shortage and high process cost can be solved, and the requirement of long-term use can be met.
Disclosure of Invention
The invention aims to provide a preparation method of a copper grid composite ionic liquid gel flexible transparent electrode. The method has the characteristics of low cost, good light transmission, long-term stability and adjustable resistance.
The invention also provides a copper grid composite ionic liquid gel flexible transparent electrode, which is prepared by the preparation method of the copper grid composite ionic liquid gel flexible transparent electrode and consists of a flexible transparent substrate, copper grids and transparent ionic liquid gel; the flexible electrode is prepared into a copper grid in the middle layer of the flexible electrode by an ink-jet printing method; the oxidation resistance of the electrode is improved through the ionic liquid gel protective layer.
The preparation method of the copper grid composite ionic liquid gel flexible transparent electrode comprises the following steps:
(1) preparing a silver nanoparticle dispersion;
(2) preparing a silver nanoparticle grid on the surface of a flexible transparent substrate:
preparing silver nanoparticle grids on the surface of a flexible transparent substrate by using the silver nanoparticle dispersion liquid prepared in the step (1); the resistance of the flexible transparent electrode is adjusted by changing the size of the silver nanoparticle grid;
(3) preparing a copper grid of the flexible electrode interlayer:
and (3) catalyzing chemical deposition of copper by the silver nanoparticle grid prepared in the step (2) to form a copper network structure. Adjusting the resistance of the flexible transparent electrode by changing the concentration and reaction time of the solution for copper chemical deposition;
(4) preparing an ionic liquid gel protective layer of the outer layer of the flexible electrode:
covering a layer of ionic liquid pre-polymerization liquid on the surface of the copper grid in the step (3) by a spin coating method, and preparing a transparent ionic liquid gel protective layer by adopting light or heat initiation to prepare the flexible transparent electrode. The flexible transparent electrode is composed of a flexible transparent substrate, a copper grid and transparent ionic liquid gel, and is shown in figure 1.
In the step (1) of the present invention, preparing silver nanoparticles and preparing a silver nanoparticle dispersion solution includes the following steps:
1.1 the step of preparing silver nanoparticles comprises:
dissolving silver nitrate and polyvinylpyrrolidone in ethylene glycol according to a certain proportion, uniformly stirring, heating to enable the silver nanoparticles to completely react, washing with acetone, ethanol and water for several times respectively, and drying in vacuum to obtain silver nanoparticle powder.
1.2 the step of preparing the silver nanoparticle dispersion liquid comprises:
dispersing silver nanoparticles in a mixed solvent of ethylene glycol and water to prepare a silver nanoparticle dispersion liquid with a certain concentration. The prepared silver nanoparticle dispersion liquid is used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate in the next step.
The weight ratio of the silver nitrate to the polyvinylpyrrolidone in the invention is 1: 5-1: 50, the weight ratio of the total amount of the silver nitrate and the polyvinylpyrrolidone to the ethylene glycol is 1: 5-1: 20.
the weight ratio of the silver nanoparticles to the mixed solvent in the silver nanoparticle dispersion liquid of the present invention is 1: 10-1: 100.
in the invention, the heating temperature in the step 1.1 is 60-120 ℃.
The solvent in the invention is one or more of glycol, water, ethanol and acetone.
The size of the silver nanoparticle grid is (0.1-1) × (0.1-1) mm2。
In the step (2) of the present invention, the flexible transparent substrate is polyethylene terephthalate, polyvinyl chloride, polyethylene, polypropylene, polystyrene, polymethyl methacrylate, acrylonitrile-butadiene-styrene copolymer, polyimide, polydimethylsiloxane, or polycarbonate.
In the invention, the prepared silver nanoparticle dispersion liquid is preferably used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate through an ink-jet printer, and the distance between two adjacent printing points of ink-jet printing is 20-50 mu m. The method comprises the steps of printing a silver nanoparticle grid through an ink-jet printer, filtering silver nanoparticle dispersion liquid through a filter membrane with the aperture of 0.2-1 mu m, filling the silver nanoparticle dispersion liquid into an ink box, putting the ink box into the printer, inputting a pre-designed printing pattern into a computer, setting the distance between two adjacent printing points, and placing a corresponding printing substrate for printing.
In the step (3) of the present invention, the solution for copper electroless deposition is prepared to include a solution a and a solution B. The solution A comprises copper chloride dihydrate, sodium hydroxide, ethylene diamine tetraacetic acid disodium salt dihydrate and sodium potassium tartrate; the solution B is formaldehyde solution. Mixing the solution A and the solution B in a ratio of 10: 1-1: 1 to obtain the solution for copper chemical deposition.
The concentration of the solution A for copper chemical deposition is respectively as follows: 9.6-96 g/L of copper chloride dihydrate, 11.2-112 g/L of sodium hydroxide, 20-200 g/L of disodium ethylenediaminetetraacetate dihydrate and 11.2-112 g/L of potassium sodium tartrate.
The concentration of the solution B for copper chemical deposition is 12-120 g/L.
The reaction time of the copper chemical deposition is 5-30 min.
In the invention, the copper chemical deposition operation method is to soak the silver nanoparticle grid in the solution for copper chemical deposition. The invention has no specific requirement on the dosage of the mixed solution as long as the silver nano-particle grid can be submerged.
In the ionic liquid pre-polymerization solution in the step (4), the ionic liquid pre-polymerization solution is prepared by dissolving an ionic liquid monomer containing double bonds, an initiator and a cross-linking agent in a solvent, and/or the ionic liquid pre-polymerization solution is prepared by dissolving a functional polyionic liquid and a cross-linking agent in a solvent; wherein the double-bond ionic liquid monomer is one or more of pyridine ionic liquids, quaternary ammonium salts, quaternary phosphonium salts, pyrrolidine ionic liquids and piperidine ionic liquids. Preferably, pyridines such as N-vinylpyridine tetrafluoroborate; quaternary ammonium salts such as tributylvinylammonium (trifluoromethanesulfonyl) imide salt; quaternary phosphonium salts such as tributyl vinyl phosphonium bromide; pyrrolidines such as N-vinyl-N-methylpyrrolidine bromide; piperidines such as N-vinyl-N-methylpiperidinium bromide. The functional polyionic liquid is one or more of poly (1-vinyl-3-carboxyethylimidazole nitrate), poly (1-vinyl-3-hydroxyethyl imidazole tetrafluoroborate) and poly (1-vinyl-3-aminopropylimidazole nitrate).
The weight ratio of the ionic liquid to the solvent in the invention is 1: 0-1: 2; the solvent can be one or more of water, ethanol and acetone.
The monomer initiator can be one or more of benzoin ethyl ether, diphenylethanone, benzophenone, potassium persulfate, ammonium persulfate, benzoyl peroxide, di-tert-butyl peroxide and azobisisobutyronitrile.
The cross-linking agent is one or more of N, N-methylene bisacrylamide, polyethylene glycol dimethacrylate, glutaraldehyde, a calcium chloride aqueous solution and diisocyanate.
The mass ratio of the initiator to the polymer monomer is 1: 50-1: 1000.
the mass ratio of the cross-linking agent to the polymer monomer is 1: 20-1: 1000.
the photoinitiation wavelength in the invention is 250-420 nm.
The thermal initiation temperature in the invention is 60-90 ℃.
The invention also provides the copper grid composite ionic liquid gel flexible transparent electrode prepared by the preparation method.
Further, an application of the copper grid composite ionic liquid gel flexible transparent electrode is also provided, and the application is preferably used for preparing foldable electronic displays, such as mobile phones, computer displays, watches, visual glasses and the like. Can also be used for preparing a bendable thin film transistor or a bendable solar cell.
The copper grid composite ionic liquid gel flexible transparent electrode provided by the invention overcomes the defects of high cost, complex process, scarce raw materials and easiness in oxidation in the prior transparent electrode technology. By changing the concentration of the silver nanoparticle dispersion liquid, the ink-jet printing parameters, the size of the copper grid, the concentration of the solution for copper chemical deposition and the reaction time, the resistance of the flexible transparent electrode can be adjusted. The flexible transparent electrode obtained by the invention can not be damaged or the conductivity is reduced after being placed for up to one year, and the conductivity of the flexible transparent electrode is not influenced by ultraviolet illumination for one hour. The flexible transparent electrode obtained by the invention has the characteristics of low cost, good light transmittance, long-term stability and adjustable resistance, and is particularly suitable for preparing screens of visual electronic equipment, wearable electronic equipment, bendable solar cells, bendable light-emitting diodes and organic electroluminescent panels.
Drawings
Fig. 1 is a schematic diagram of a copper mesh composite ionic liquid gel flexible transparent electrode of the present invention.
Detailed Description
The technical solution of the present invention will be further described with reference to the following examples.
Example 1
(1) Preparation of silver nanoparticle dispersion
Silver nitrate and polyvinylpyrrolidone were dissolved in ethylene glycol at a weight ratio of 1/5 (the weight ratio of silver nitrate/ethylene glycol was 1/50), and stirred to a uniform state. The silver nitrate is uniformly dispersed in a heating state at 60 ℃, and then the temperature is raised to 120 ℃ and kept for 1 hour to ensure that the silver nanoparticles completely react. And washing the silver nanoparticles obtained by the reaction with acetone, ethanol and water for three times, and drying the silver nanoparticles in a vacuum drying oven at 60 ℃ for 0.5h to obtain silver nanoparticle powder. Silver nanoparticles were dispersed in a mixed solvent of ethylene glycol and water (the volume ratio of ethylene glycol/water was 1/1) (the weight ratio of silver nanoparticles/mixed solvent was 2/100) to form a silver nanoparticle dispersion liquid. The prepared silver nanoparticle dispersion liquid is used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate in the next step.
(2) Preparation of silver nanoparticle grid on surface of flexible transparent substrate
Selecting polyethylene glycol terephthalate as a flexible transparent substrate, filtering silver nanoparticle dispersion liquid through a filter membrane of 1 mu m, filling the silver nanoparticle dispersion liquid into an ink box, putting the ink box into a printer, inputting a pre-designed printing graph into a computer, setting the distance between two adjacent printing points to be 20 mu m, placing the corresponding polyethylene glycol terephthalate substrate for printing, wherein the size of a printed silver nanoparticle grid is 0.5 multiplied by 0.5mm2。
(3) Copper grid for preparing flexible electrode interlayer
Preparing a solution for copper chemical deposition: the solution A comprises copper chloride dihydrate (9.6g/L), sodium hydroxide (11.2g/L), ethylene diamine tetraacetic acid dihydrate (20g/L) and sodium potassium tartrate (11.2 g/L); the B solution is formaldehyde solution (12 g/L). And mixing the solution A and the solution B according to the volume ratio of 1/1 to obtain the solution for copper chemical deposition. The reaction time of copper chemical deposition is 10min, and the copper grid structure of the flexible electrode middle layer is obtained.
(4) Ionic liquid gel protective layer for preparing flexible electrode outer layer
N-vinylpyridine tetrafluoroborate, potassium persulfate, N-methylenebisacrylamide were dissolved in ethanol (the weight ratio of N-vinylpyridine tetrafluoroborate/potassium persulfate/N, N-methylenebisacrylamide/ethanol was 1000/10/40/1000), and spin-coated on the sample surface. Heating at 80 ℃ for 1h to obtain the ionic liquid gel protective layer on the outer layer of the flexible electrode.
(5) Application of copper grid composite ionic liquid gel flexible transparent electrode
The prepared copper grid composite ionic liquid gel flexible transparent electrode has the light transmittance of more than 85 percent and the square resistance of 100-.
Example 2
(1) Preparation of silver nanoparticle dispersion
Silver nitrate and polyvinylpyrrolidone were dissolved in ethylene glycol at a weight ratio of 1/10 (the weight ratio of silver nitrate/ethylene glycol was 1/55), and stirred to a uniform state. The silver nitrate is uniformly dispersed in a heating state at 60 ℃, and then the temperature is raised to 120 ℃ and kept for 1 hour to ensure that the silver nanoparticles completely react. And washing the silver nanoparticles obtained by the reaction with acetone, ethanol and water for three times, and drying the silver nanoparticles in a vacuum drying oven at 60 ℃ for 0.5h to obtain silver nanoparticle powder. Silver nanoparticles were dispersed in a mixed solvent of ethylene glycol and water (the volume ratio of ethylene glycol/water was 1/1) (the weight ratio of silver nanoparticles/mixed solvent was 5/100) to form a silver nanoparticle dispersion liquid. The prepared silver nanoparticle dispersion liquid is used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate in the next step.
(2) Preparation of silver nanoparticle grid on surface of flexible transparent substrate
Selecting polyethylene glycol terephthalate as a flexible transparent substrate, filtering the silver nanoparticle dispersion liquid by a filter membrane of 1 micron, filling the silver nanoparticle dispersion liquid into an ink box, putting the ink box into a printer, inputting a pre-designed printing graph into a computer, setting the distance between two adjacent printing points to be 35 microns, placing the corresponding polyethylene glycol terephthalate substrate for printing,the printed silver nanoparticle grid size was 0.3 × 0.3mm2。
(3) Copper grid for preparing flexible electrode interlayer
Preparing a solution for copper chemical deposition: the solution A comprises copper chloride dihydrate (48g/L), sodium hydroxide (56g/L), ethylene diamine tetraacetic acid dihydrate (100g/L) and sodium potassium tartrate (56 g/L); the solution B is formaldehyde solution (60 g/L). And mixing the solution A and the solution B according to the volume ratio of 1/1 to obtain the solution for copper chemical deposition. The reaction time of copper chemical deposition is 15min, and the copper grid structure of the flexible electrode middle layer is obtained.
(4) Ionic liquid gel protective layer for preparing flexible electrode outer layer
Tributylvinylammonium (trifluoromethanesulfonyl) imide salt, potassium persulfate, N-methylenebisacrylamide were dissolved in water (weight ratio of tributylvinylammonium (trifluoromethanesulfonyl) imide salt/potassium persulfate/N, N-methylenebisacrylamide/water is 1000/10/40/1000), and spin-coated on the sample surface. Heating at 80 ℃ for 1h to obtain the ionic liquid gel protective layer on the outer layer of the flexible electrode.
(5) Application of copper grid composite ionic liquid gel flexible transparent electrode
The prepared copper grid composite ionic liquid gel flexible transparent electrode has the light transmittance of more than 85 percent and the square resistance of 5-20 omega/sq, and can be used for preparing wearable electronic equipment, flexible display screens, solar cells, electrochromic displays and LCD displays.
Example 3
(1) Preparation of silver nanoparticle dispersion
Silver nitrate and polyvinylpyrrolidone were dissolved in ethylene glycol at a weight ratio of 1/20 (the weight ratio of silver nitrate/ethylene glycol was 1/210), and stirred to a uniform state. The silver nitrate is uniformly dispersed in a heating state at 60 ℃, and then the temperature is raised to 120 ℃ and kept for 1 hour to ensure that the silver nanoparticles completely react. And washing the silver nanoparticles obtained by the reaction with acetone, ethanol and water for three times, and drying the silver nanoparticles in a vacuum drying oven at 60 ℃ for 0.5h to obtain silver nanoparticle powder. Silver nanoparticles were dispersed in a mixed solvent of ethylene glycol and water (the volume ratio of ethylene glycol/water was 1/1) (the weight ratio of silver nanoparticles/mixed solvent was 5/100) to form a silver nanoparticle dispersion liquid. The prepared silver nanoparticle dispersion liquid is used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate in the next step.
(2) Preparation of silver nanoparticle grid on surface of flexible transparent substrate
Selecting polyethylene glycol terephthalate as a flexible transparent substrate, filtering silver nanoparticle dispersion liquid through a filter membrane of 1 mu m, filling the silver nanoparticle dispersion liquid into an ink box, putting the ink box into a printer, inputting a pre-designed printing graph into a computer, setting the distance between two adjacent printing points to be 40 mu m, placing the corresponding polyethylene glycol terephthalate substrate for printing, wherein the size of a printed silver nanoparticle grid is 0.4 multiplied by 0.4mm2。
(3) Copper grid for preparing flexible electrode interlayer
Preparing a solution for copper chemical deposition: the solution A comprises copper chloride dihydrate (12g/L), sodium hydroxide (14g/L), ethylene diamine tetraacetic acid dihydrate (25g/L) and sodium potassium tartrate (14 g/L); the solution B is formaldehyde solution (15 g/L). And mixing the solution A and the solution B according to the volume ratio of 1/1 to obtain the solution for copper chemical deposition. The reaction time of copper chemical deposition is 15min, and the copper grid structure of the flexible electrode middle layer is obtained.
(4) Ionic liquid gel protective layer for preparing flexible electrode outer layer
The N-vinylpyridine tetrafluoroborate, benzophenone and polyethylene glycol dimethacrylate were dissolved in ethanol (the weight ratio of N-vinylpyridine tetrafluoroborate/benzophenone/polyethylene glycol dimethacrylate/ethanol was 1000/10/20/1000) and spin-coated on the sample surface. And irradiating for 1h under 255nm ultraviolet light to obtain the ionic liquid gel protective layer on the outer layer of the flexible electrode.
(5) Application of copper grid composite ionic liquid gel flexible transparent electrode
The prepared copper grid composite ionic liquid gel flexible transparent electrode has the light transmittance of more than 85 percent and the square resistance of 20-100 omega/sq, and can be used for preparing wearable electronic equipment, flexible display screens, solar cells, electrochromic displays and LCD displays.
Example 4
(1) Preparation of silver nanoparticle dispersion
Silver nitrate and polyvinylpyrrolidone were dissolved in ethylene glycol at a weight ratio of 1/50 (the weight ratio of silver nitrate/ethylene glycol was 1/255), and stirred to a uniform state. The silver nitrate is uniformly dispersed in a heating state at 60 ℃, and then the temperature is raised to 120 ℃ and kept for 1 hour to ensure that the silver nanoparticles completely react. And washing the silver nanoparticles obtained by the reaction with acetone, ethanol and water for three times, and drying the silver nanoparticles in a vacuum drying oven at 60 ℃ for 0.5h to obtain silver nanoparticle powder. Silver nanoparticles were dispersed in a mixed solvent of ethylene glycol and water (the volume ratio of ethylene glycol/water was 1/1) (the weight ratio of silver nanoparticles/mixed solvent was 4/100) to form a silver nanoparticle dispersion liquid. The prepared silver nanoparticle dispersion liquid is used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate in the next step.
(2) Preparation of silver nanoparticle grid on surface of flexible transparent substrate
Selecting polyethylene glycol terephthalate as a flexible transparent substrate, filtering silver nanoparticle dispersion liquid through a filter membrane of 1 mu m, filling the silver nanoparticle dispersion liquid into an ink box, putting the ink box into a printer, inputting a pre-designed printing graph into a computer, setting the distance between two adjacent printing points to be 40 mu m, placing the corresponding polyethylene glycol terephthalate substrate for printing, wherein the size of a printed silver nanoparticle grid is 0.3 multiplied by 0.3mm2。
(3) Copper grid for preparing flexible electrode interlayer
Preparing a solution for copper chemical deposition: the solution A comprises copper chloride dihydrate (48g/L), sodium hydroxide (56g/L), ethylene diamine tetraacetic acid dihydrate (100g/L) and sodium potassium tartrate (56 g/L); the solution B is formaldehyde solution (60 g/L). And mixing the solution A and the solution B according to the volume ratio of 1/1 to obtain the solution for copper chemical deposition. The reaction time of copper chemical deposition is 20min, and the copper grid structure of the flexible electrode middle layer is obtained.
(4) Ionic liquid gel protective layer for preparing flexible electrode outer layer
Poly (1-vinyl-3-aminopropylimidazole nitrate), glutaraldehyde were dissolved in water (weight ratio of poly (1-vinyl-3-aminopropylimidazole nitrate)/glutaraldehyde/water was 1000/20/1000) and spin coated on the sample surface. Heating at 60 ℃ for 1h to obtain the ionic liquid gel protective layer on the outer layer of the flexible electrode.
(5) Application of copper grid composite ionic liquid gel flexible transparent electrode
The prepared copper grid composite ionic liquid gel flexible transparent electrode has the light transmittance of more than 85 percent and the square resistance of 5-20 omega/sq, and can be used for preparing wearable electronic equipment, flexible display screens, solar cells, electrochromic displays and LCD displays.
Example 5
(1) Preparation of silver nanoparticle dispersion
Silver nitrate and polyvinylpyrrolidone were dissolved in ethylene glycol at a weight ratio of 1/5 (the weight ratio of silver nitrate/ethylene glycol was 1/120), and stirred to a uniform state. The silver nitrate is uniformly dispersed in a heating state at 60 ℃, and then the temperature is raised to 120 ℃ and kept for 1 hour to ensure that the silver nanoparticles completely react. And washing the silver nanoparticles obtained by the reaction with acetone, ethanol and water for three times, and drying the silver nanoparticles in a vacuum drying oven at 60 ℃ for 0.5h to obtain silver nanoparticle powder. Silver nanoparticles were dispersed in a mixed solvent of ethylene glycol and water (the volume ratio of ethylene glycol/water was 1/1) (the weight ratio of silver nanoparticles/mixed solvent was 4/100) to form a silver nanoparticle dispersion liquid. The prepared silver nanoparticle dispersion liquid is used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate in the next step.
(2) Preparation of silver nanoparticle grid on surface of flexible transparent substrate
Selecting polyethylene glycol terephthalate as a flexible transparent substrate, filtering silver nanoparticle dispersion liquid through a filter membrane of 1 mu m, filling the silver nanoparticle dispersion liquid into an ink box, putting the ink box into a printer, inputting a pre-designed printing graph into a computer, setting the distance between two adjacent printing points to be 50 mu m, placing the corresponding polyethylene glycol terephthalate substrate for printing, wherein the size of a printed silver nanoparticle grid is 0.4 multiplied by 0.4mm2。
(3) Copper grid for preparing flexible electrode interlayer
Preparing a solution for copper chemical deposition: the solution A comprises copper chloride dihydrate (48g/L), sodium hydroxide (56g/L), ethylene diamine tetraacetic acid dihydrate (100g/L) and sodium potassium tartrate (56 g/L); the solution B is formaldehyde solution (60 g/L). And mixing the solution A and the solution B according to the volume ratio of 1/1 to obtain the solution for copper chemical deposition. The reaction time of copper chemical deposition is 10min, and the copper grid structure of the flexible electrode middle layer is obtained.
(4) Ionic liquid gel protective layer for preparing flexible electrode outer layer
N-vinyl-N-methylpyrrolidine bromide, ammonium persulfate and N, N-methylene bisacrylamide are dissolved in water (the weight ratio of the N-vinyl-N-methylpyrrolidine bromide to the ammonium persulfate to the N, N-methylene bisacrylamide to the water is 1000/10/20/1000), and the mixture is spin-coated on the surface of a sample. Heating at 90 ℃ for 1h to obtain the ionic liquid gel protective layer on the outer layer of the flexible electrode.
(5) Application of copper grid composite ionic liquid gel flexible transparent electrode
The prepared copper grid composite ionic liquid gel flexible transparent electrode has the light transmittance of more than 85 percent and the square resistance of 20-100 omega/sq, and can be used for preparing wearable electronic equipment, flexible display screens, solar cells, electrochromic displays and LCD displays.
Example 6
(1) Preparation of silver nanoparticle dispersion
Silver nitrate and polyvinylpyrrolidone were dissolved in ethylene glycol at a weight ratio of 1/5 (the weight ratio of silver nitrate/ethylene glycol was 1/50), and stirred to a uniform state. The silver nitrate is uniformly dispersed in a heating state at 60 ℃, and then the temperature is raised to 120 ℃ and kept for 1 hour to ensure that the silver nanoparticles completely react. And washing the silver nanoparticles obtained by the reaction with acetone, ethanol and water for three times, and drying the silver nanoparticles in a vacuum drying oven at 60 ℃ for 0.5h to obtain silver nanoparticle powder. Silver nanoparticles were dispersed in a mixed solvent of ethylene glycol and water (the volume ratio of ethylene glycol/water was 1/1) (the weight ratio of silver nanoparticles/mixed solvent was 5/100) to form a silver nanoparticle dispersion liquid. The prepared silver nanoparticle dispersion liquid is used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate in the next step.
(2) Preparation of silver nanoparticle grid on surface of flexible transparent substrate
Selecting polyethylene glycol terephthalate as a flexible transparent substrate, filtering silver nanoparticle dispersion liquid through a filter membrane of 1 mu m, filling the silver nanoparticle dispersion liquid into an ink box, putting the ink box into a printer, inputting a pre-designed printing graph into a computer, setting the distance between two adjacent printing points to be 30 mu m, placing the corresponding polyethylene glycol terephthalate substrate for printing, wherein the size of a printed silver nanoparticle grid is 0.4 multiplied by 0.4mm2。
(3) Copper grid for preparing flexible electrode interlayer
Preparing a solution for copper chemical deposition: the solution A comprises copper chloride dihydrate (48g/L), sodium hydroxide (56g/L), ethylene diamine tetraacetic acid dihydrate (100g/L) and sodium potassium tartrate (56 g/L); the solution B is formaldehyde solution (60 g/L). And mixing the solution A and the solution B according to the volume ratio of 1/1 to obtain the solution for copper chemical deposition. The reaction time of copper chemical deposition is 15min, and the copper grid structure of the flexible electrode middle layer is obtained.
(4) Ionic liquid gel protective layer for preparing flexible electrode outer layer
Tributyl vinyl phosphine bromide, ammonium persulfate and N, N-methylene bisacrylamide were dissolved in water (the weight ratio of tributyl vinyl phosphine bromide/ammonium persulfate/N, N-methylene bisacrylamide/water was 1000/10/20/1000), and spin-coated on the sample surface. Heating at 90 ℃ for 1h to obtain the ionic liquid gel protective layer on the outer layer of the flexible electrode.
(5) Application of copper grid composite ionic liquid gel flexible transparent electrode
The prepared copper grid composite ionic liquid gel flexible transparent electrode has the light transmittance of more than 85 percent and the square resistance of 10-20 omega/sq, and can be used for preparing wearable electronic equipment, flexible display screens, solar cells, electrochromic displays and LCD displays.
Example 7
(1) Preparation of silver nanoparticle dispersion
Silver nitrate and polyvinylpyrrolidone were dissolved in ethylene glycol at a weight ratio of 1/5 (the weight ratio of silver nitrate/ethylene glycol was 1/50), and stirred to a uniform state. The silver nitrate is uniformly dispersed in a heating state at 60 ℃, and then the temperature is raised to 120 ℃ and kept for 1 hour to ensure that the silver nanoparticles completely react. And washing the silver nanoparticles obtained by the reaction with acetone, ethanol and water for three times, and drying the silver nanoparticles in a vacuum drying oven at 60 ℃ for 0.5h to obtain silver nanoparticle powder. Silver nanoparticles were dispersed in a mixed solvent of ethylene glycol and water (the volume ratio of ethylene glycol/water was 1/1) (the weight ratio of silver nanoparticles/mixed solvent was 5/100) to form a silver nanoparticle dispersion liquid. The prepared silver nanoparticle dispersion liquid is used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate in the next step.
(2) Preparation of silver nanoparticle grid on surface of flexible transparent substrate
Selecting polyvinyl chloride as a flexible transparent substrate, filtering silver nanoparticle dispersion liquid through a filter membrane of 1 mu m, filling the silver nanoparticle dispersion liquid into an ink box, putting the ink box into a printer, inputting a pre-designed printing pattern into a computer, setting the distance between two adjacent printing points to be 35 mu m, placing the corresponding polyvinyl chloride substrate for printing, wherein the size of a printed silver nanoparticle grid is 0.4 multiplied by 0.4mm2。
(3) Copper grid for preparing flexible electrode interlayer
Preparing a solution for copper chemical deposition: the solution A comprises copper chloride dihydrate (48g/L), sodium hydroxide (56g/L), ethylene diamine tetraacetic acid dihydrate (100g/L) and sodium potassium tartrate (56 g/L); the solution B is formaldehyde solution (60 g/L). And mixing the solution A and the solution B according to the volume ratio of 1/1 to obtain the solution for copper chemical deposition. The reaction time of copper chemical deposition is 15min, and the copper grid structure of the flexible electrode middle layer is obtained.
(4) Ionic liquid gel protective layer for preparing flexible electrode outer layer
Tributyl vinyl phosphine bromide, ammonium persulfate and N, N-methylene bisacrylamide were dissolved in water (the weight ratio of tributyl vinyl phosphine bromide/ammonium persulfate/N, N-methylene bisacrylamide/water was 1000/10/20/1000), and spin-coated on the sample surface. Heating at 90 ℃ for 1h to obtain the ionic liquid gel protective layer on the outer layer of the flexible electrode.
(5) Application of copper grid composite ionic liquid gel flexible transparent electrode
The prepared copper grid composite ionic liquid gel flexible transparent electrode has the light transmittance of more than 85 percent and the square resistance of 5-20 omega/sq, and can be used for preparing wearable electronic equipment, flexible display screens, solar cells, electrochromic displays and OLED displays.
Example 8
(1) Preparation of silver nanoparticle dispersion
Silver nitrate and polyvinylpyrrolidone were dissolved in ethylene glycol at a weight ratio of 1/5 (the weight ratio of silver nitrate/ethylene glycol was 1/50), and stirred to a uniform state. The silver nitrate is uniformly dispersed in a heating state at 60 ℃, and then the temperature is raised to 120 ℃ and kept for 1 hour to ensure that the silver nanoparticles completely react. And washing the silver nanoparticles obtained by the reaction with acetone, ethanol and water for three times, and drying the silver nanoparticles in a vacuum drying oven at 60 ℃ for 0.5h to obtain silver nanoparticle powder. Silver nanoparticles were dispersed in a mixed solvent of ethylene glycol and water (the volume ratio of ethylene glycol/water was 1/1) (the weight ratio of silver nanoparticles/mixed solvent was 5/100) to form a silver nanoparticle dispersion liquid. The prepared silver nanoparticle dispersion liquid is used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate in the next step.
(2) Preparation of silver nanoparticle grid on surface of flexible transparent substrate
Selecting polymethyl methacrylate as a flexible transparent substrate, filtering a silver nanoparticle dispersion liquid through a filter membrane of 1 mu m, filling the silver nanoparticle dispersion liquid into an ink box, putting the ink box into a printer, inputting a pre-designed printing pattern into a computer, setting the distance between two adjacent printing points to be 35 mu m, placing the corresponding polymethyl methacrylate substrate for printing, wherein the size of a printed silver nanoparticle grid is 0.4 multiplied by 0.4mm2。
(3) Copper grid for preparing flexible electrode interlayer
Preparing a solution for copper chemical deposition: the solution A comprises copper chloride dihydrate (48g/L), sodium hydroxide (56g/L), ethylene diamine tetraacetic acid dihydrate (100g/L) and sodium potassium tartrate (56 g/L); the solution B is formaldehyde solution (60 g/L). And mixing the solution A and the solution B according to the volume ratio of 1/1 to obtain the solution for copper chemical deposition. The reaction time of copper chemical deposition is 15min, and the copper grid structure of the flexible electrode middle layer is obtained.
(4) Ionic liquid gel protective layer for preparing flexible electrode outer layer
Tributylvinylammonium (trifluoromethanesulfonyl) imide salt, ammonium persulfate, N-methylenebisacrylamide dissolved in water (weight ratio tributylvinylammonium (trifluoromethanesulfonyl) imide salt/ammonium persulfate/N, N-methylenebisacrylamide/water 1000/10/20/1000), was spin-coated on the sample surface. Heating at 70 ℃ for 1h to obtain the ionic liquid gel protective layer on the outer layer of the flexible electrode.
(5) Application of copper grid composite ionic liquid gel flexible transparent electrode
The prepared copper grid composite ionic liquid gel flexible transparent electrode has the light transmittance of more than 85 percent and the square resistance of 5-20 omega/sq, and can be used for preparing wearable electronic equipment, flexible display screens, solar cells, electrochromic displays and OLED displays.
Example 9
(1) Preparation of silver nanoparticle dispersion
Silver nitrate and polyvinylpyrrolidone were dissolved in ethylene glycol at a weight ratio of 1/5 (the weight ratio of silver nitrate/ethylene glycol was 1/50), and stirred to a uniform state. The silver nitrate is uniformly dispersed in a heating state at 60 ℃, and then the temperature is raised to 120 ℃ and kept for 1 hour to ensure that the silver nanoparticles completely react. And washing the silver nanoparticles obtained by the reaction with acetone, ethanol and water for three times, and drying the silver nanoparticles in a vacuum drying oven at 60 ℃ for 0.5h to obtain silver nanoparticle powder. Silver nanoparticles were dispersed in a mixed solvent of ethylene glycol and water (the volume ratio of ethylene glycol/water was 1/1) (the weight ratio of silver nanoparticles/mixed solvent was 5/100) to form a silver nanoparticle dispersion liquid. The prepared silver nanoparticle dispersion liquid is used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate in the next step.
(2) Preparation of silver nanoparticle grid on surface of flexible transparent substrate
Selecting acrylonitrile-butadiene-styrene copolymer as flexible transparent substrate, filtering silver nanoparticle dispersion liquid with 1 μm filter membrane, filling into ink box, placing the ink box into printer, and inputting predesigned design in computerThe distance between two adjacent printing points is set to be 35 mu m, the corresponding acrylonitrile-butadiene-styrene copolymer substrate is placed for printing, and the size of the printed silver nanoparticle grid is 0.4 multiplied by 0.4mm2。
(3) Copper grid for preparing flexible electrode interlayer
Preparing a solution for copper chemical deposition: the solution A comprises copper chloride dihydrate (48g/L), sodium hydroxide (56g/L), ethylene diamine tetraacetic acid dihydrate (100g/L) and sodium potassium tartrate (56 g/L); the solution B is formaldehyde solution (60 g/L). And mixing the solution A and the solution B according to the volume ratio of 1/1 to obtain the solution for copper chemical deposition. The reaction time of copper chemical deposition is 15min, and the copper grid structure of the flexible electrode middle layer is obtained.
(4) Ionic liquid gel protective layer for preparing flexible electrode outer layer
Tributylvinylammonium (trifluoromethanesulfonyl) imide salt, ammonium persulfate, N-methylenebisacrylamide dissolved in water (weight ratio tributylvinylammonium (trifluoromethanesulfonyl) imide salt/ammonium persulfate/N, N-methylenebisacrylamide/water 1000/10/20/1000), was spin-coated on the sample surface. Heating at 70 ℃ for 1h to obtain the ionic liquid gel protective layer on the outer layer of the flexible electrode.
(5) Application of copper grid composite ionic liquid gel flexible transparent electrode
The prepared copper grid composite ionic liquid gel flexible transparent electrode has the light transmittance of more than 85 percent and the square resistance of 5-20 omega/sq, and can be used for preparing wearable electronic equipment, flexible display screens, solar cells, electrochromic displays and OLED displays.
Example 10
(1) Preparation of silver nanoparticle dispersion
Silver nitrate and polyvinylpyrrolidone were dissolved in ethylene glycol at a weight ratio of 1/5 (the weight ratio of silver nitrate/ethylene glycol was 1/50), and stirred to a uniform state. The silver nitrate is uniformly dispersed in a heating state at 60 ℃, and then the temperature is raised to 120 ℃ and kept for 1 hour to ensure that the silver nanoparticles completely react. And washing the silver nanoparticles obtained by the reaction with acetone, ethanol and water for three times, and drying the silver nanoparticles in a vacuum drying oven at 60 ℃ for 0.5h to obtain silver nanoparticle powder. Silver nanoparticles were dispersed in a mixed solvent of ethylene glycol and water (the volume ratio of ethylene glycol/water was 1/1) (the weight ratio of silver nanoparticles/mixed solvent was 5/100) to form a silver nanoparticle dispersion liquid. The prepared silver nanoparticle dispersion liquid is used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate in the next step.
(2) Preparation of silver nanoparticle grid on surface of flexible transparent substrate
Selecting polyimide as a flexible transparent substrate, filtering silver nanoparticle dispersion liquid through a filter membrane of 1 mu m, filling the silver nanoparticle dispersion liquid into an ink box, putting the ink box into a printer, inputting a pre-designed printing pattern into a computer, setting the distance between two adjacent printing points to be 35 mu m, placing the corresponding polyimide substrate for printing, and setting the size of a printed silver nanoparticle grid to be 0.4 multiplied by 0.4mm2。
(3) Copper grid for preparing flexible electrode interlayer
Preparing a solution for copper chemical deposition: the solution A comprises copper chloride dihydrate (96g/L), sodium hydroxide (112g/L), ethylene diamine tetraacetic acid dihydrate (200g/L) and sodium potassium tartrate (112 g/L); the solution B is formaldehyde solution (120 g/L). And mixing the solution A and the solution B according to the volume ratio of 1/1 to obtain the solution for copper chemical deposition. The reaction time of copper chemical deposition is 15min, and the copper grid structure of the flexible electrode middle layer is obtained.
(4) Ionic liquid gel protective layer for preparing flexible electrode outer layer
Tributylvinylammonium (trifluoromethanesulfonyl) imide salt, ammonium persulfate, N-methylenebisacrylamide dissolved in water (weight ratio tributylvinylammonium (trifluoromethanesulfonyl) imide salt/ammonium persulfate/N, N-methylenebisacrylamide/water 1000/10/20/1000), was spin-coated on the sample surface. Heating at 70 ℃ for 1h to obtain the ionic liquid gel protective layer on the outer layer of the flexible electrode.
(5) Application of copper grid composite ionic liquid gel flexible transparent electrode
The prepared copper grid composite ionic liquid gel flexible transparent electrode has the light transmittance of more than 85 percent and the square resistance of 5-10 omega/sq, and can be used for preparing wearable electronic equipment, flexible display screens, solar cells, electrochromic displays and OLED displays.
Example 11
(1) Preparation of silver nanoparticle dispersion
Silver nitrate and polyvinylpyrrolidone were dissolved in ethylene glycol at a weight ratio of 1/5 (the weight ratio of silver nitrate/ethylene glycol was 1/50), and stirred to a uniform state. The silver nitrate is uniformly dispersed in a heating state at 60 ℃, and then the temperature is raised to 120 ℃ and kept for 1 hour to ensure that the silver nanoparticles completely react. And washing the silver nanoparticles obtained by the reaction with acetone, ethanol and water for three times, and drying the silver nanoparticles in a vacuum drying oven at 60 ℃ for 0.5h to obtain silver nanoparticle powder. Silver nanoparticles were dispersed in a mixed solvent of ethylene glycol and water (the volume ratio of ethylene glycol/water was 1/1) (the weight ratio of silver nanoparticles/mixed solvent was 5/100) to form a silver nanoparticle dispersion liquid. The prepared silver nanoparticle dispersion liquid is used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate in the next step.
(2) Preparation of silver nanoparticle grid on surface of flexible transparent substrate
Selecting polydimethylsiloxane as a flexible transparent substrate, filtering silver nanoparticle dispersion liquid through a filter membrane of 1 mu m, filling the silver nanoparticle dispersion liquid into an ink box, putting the ink box into a printer, inputting a pre-designed printing pattern into a computer, setting the distance between two adjacent printing points to be 30 mu m, placing the corresponding polydimethylsiloxane substrate for printing, wherein the size of a printed silver nanoparticle grid is 0.4 multiplied by 0.4mm2。
(3) Copper grid for preparing flexible electrode interlayer
Preparing a solution for copper chemical deposition: the solution A comprises copper chloride dihydrate (96g/L), sodium hydroxide (112g/L), ethylene diamine tetraacetic acid dihydrate (200g/L) and sodium potassium tartrate (112 g/L); the solution B is formaldehyde solution (120 g/L). And mixing the solution A and the solution B according to the volume ratio of 1/1 to obtain the solution for copper chemical deposition. The reaction time of copper chemical deposition is 15min, and the copper grid structure of the flexible electrode middle layer is obtained.
(4) Ionic liquid gel protective layer for preparing flexible electrode outer layer
Tributylvinylammonium (trifluoromethanesulfonyl) imide salt, ammonium persulfate, N-methylenebisacrylamide dissolved in water (weight ratio tributylvinylammonium (trifluoromethanesulfonyl) imide salt/ammonium persulfate/N, N-methylenebisacrylamide/water 1000/10/20/1000), was spin-coated on the sample surface. Heating at 70 ℃ for 1h to obtain the ionic liquid gel protective layer on the outer layer of the flexible electrode.
(5) Application of copper grid composite ionic liquid gel flexible transparent electrode
The prepared copper grid composite ionic liquid gel flexible transparent electrode has the light transmittance of more than 85 percent and the square resistance of 5-20 omega/sq, and can be used for preparing wearable electronic equipment, flexible display screens, solar cells, electrochromic displays and OLED displays.
Example 12
(1) Preparation of silver nanoparticle dispersion
Silver nitrate and polyvinylpyrrolidone were dissolved in ethylene glycol at a weight ratio of 1/5 (the weight ratio of silver nitrate/ethylene glycol was 1/50), and stirred to a uniform state. The silver nitrate is uniformly dispersed in a heating state at 60 ℃, and then the temperature is raised to 120 ℃ and kept for 1 hour to ensure that the silver nanoparticles completely react. And washing the silver nanoparticles obtained by the reaction with acetone, ethanol and water for three times, and drying the silver nanoparticles in a vacuum drying oven at 60 ℃ for 0.5h to obtain silver nanoparticle powder. Silver nanoparticles were dispersed in a mixed solvent of ethylene glycol and water (the volume ratio of ethylene glycol/water was 1/1) (the weight ratio of silver nanoparticles/mixed solvent was 5/100) to form a silver nanoparticle dispersion liquid. The prepared silver nanoparticle dispersion liquid is used for preparing silver nanoparticle grids on the surface of the flexible transparent substrate in the next step.
(2) Preparation of silver nanoparticle grid on surface of flexible transparent substrate
Selecting polycarbonate as a flexible transparent substrate, filtering silver nanoparticle dispersion liquid through a filter membrane of 1 mu m, filling the silver nanoparticle dispersion liquid into an ink box, putting the ink box into a printer, inputting a pre-designed printing pattern into a computer, setting the distance between two adjacent printing points to be 30 mu m, placing the corresponding polycarbonate substrate for printing, wherein the size of a printed silver nanoparticle grid is 0.4 multiplied by 0.4mm2。
(3) Copper grid for preparing flexible electrode interlayer
Preparing a solution for copper chemical deposition: the solution A comprises copper chloride dihydrate (48g/L), sodium hydroxide (56g/L), ethylene diamine tetraacetic acid dihydrate (100g/L) and sodium potassium tartrate (56 g/L); the solution B is formaldehyde solution (60 g/L). And mixing the solution A and the solution B according to the volume ratio of 1/1 to obtain the solution for copper chemical deposition. The reaction time of copper chemical deposition is 15min, and the copper grid structure of the flexible electrode middle layer is obtained.
(4) Ionic liquid gel protective layer for preparing flexible electrode outer layer
Tributylvinylammonium (trifluoromethanesulfonyl) imide salt, ammonium persulfate, N-methylenebisacrylamide dissolved in water (weight ratio tributylvinylammonium (trifluoromethanesulfonyl) imide salt/ammonium persulfate/N, N-methylenebisacrylamide/water 1000/10/20/1000), was spin-coated on the sample surface. Heating at 70 ℃ for 1h to obtain the ionic liquid gel protective layer on the outer layer of the flexible electrode.
(5) Application of copper grid composite ionic liquid gel flexible transparent electrode
The prepared copper grid composite ionic liquid gel flexible transparent electrode has the light transmittance of more than 85 percent and the square resistance of 5-20 omega/sq, and can be used for preparing wearable electronic equipment, flexible display screens, solar cells, electrochromic displays and OLED displays.
The present invention may be embodied in many different forms and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. A preparation method of a copper grid composite ionic liquid gel flexible transparent electrode comprises the following steps:
(1) preparing silver nano particles and preparing a silver nano particle dispersion liquid, comprising the following steps of:
1.1 the step of preparing silver nanoparticles comprises:
dissolving silver nitrate and polyvinylpyrrolidone in ethylene glycol, uniformly stirring, heating to react the silver nanoparticles, washing and drying to obtain silver nanoparticles; the weight ratio of the silver nitrate to the polyvinylpyrrolidone is 1: 5-1: 50, the weight ratio of the total amount of the silver nitrate and the polyvinylpyrrolidone to the ethylene glycol is 1: 5-1: 20;
1.2 the step of preparing the silver nanoparticle dispersion liquid comprises:
dispersing silver nanoparticles in a mixed solvent of ethylene glycol and water to prepare a silver nanoparticle dispersion liquid, wherein the weight ratio of the silver nanoparticles to the mixed solvent of the silver nanoparticle dispersion liquid is 1: 10-1: 100, respectively;
(2) preparing a silver nanoparticle grid on the surface of a flexible transparent substrate:
preparing silver nanoparticle grids on the surface of a flexible transparent substrate by using the silver nanoparticle dispersion liquid prepared in the step (1);
(3) preparing a copper grid of the flexible electrode interlayer:
catalyzing chemical deposition of copper by the silver nanoparticle grid prepared in the step (2) to form a copper network structure;
the solution preparation of the copper chemical deposition comprises a solution A and a solution B; the solution A comprises copper chloride dihydrate, sodium hydroxide, ethylene diamine tetraacetic acid dihydrate and sodium potassium tartrate; the solution B is formaldehyde solution; the A solution and the B solution are mixed in a ratio of 10: 1-1: 1 to obtain a copper chemical deposition solution; the reaction time of the copper chemical deposition is 5-30 min;
(4) preparing an ionic liquid gel protective layer of the outer layer of the flexible electrode:
covering a layer of ionic liquid pre-polymerization liquid on the surface of the copper grid in the step (3), and preparing a transparent ionic liquid gel protective layer by adopting photo-initiation or thermal initiation to prepare the flexible transparent electrode.
2. The method according to claim 1, wherein the heating temperature in step 1.1 is 60 to 120 ℃.
3. The method of claim 1, wherein the silver nanoparticle dispersion liquid of step (2) is used for preparing a silver nanoparticle grid on the surface of the flexible transparent substrate by an ink-jet printer.
4. The method of claim 1, wherein the flexible transparent substrate is one or more of polyethylene terephthalate, polyvinyl chloride, polyethylene, polypropylene, polystyrene, polymethyl methacrylate, acrylonitrile-butadiene-styrene copolymer, polyimide, polydimethylsiloxane, and polycarbonate.
5. The preparation method according to claim 1, wherein the ionic liquid pre-polymerization solution of step (4) comprises an ionic liquid pre-polymerization solution prepared by dissolving an ionic liquid monomer containing a double bond, an initiator and a cross-linking agent in a solvent, and/or an ionic liquid pre-polymerization solution prepared by dissolving a functional polyionic liquid and a cross-linking agent in a solvent; wherein the ionic liquid monomer containing double bonds is one or more of pyridine, quaternary ammonium salt, quaternary phosphonium salt, pyrrolidine and piperidine ionic liquid; the functional polyion liquid is one or more of ionic liquid macromolecules containing carboxyl, hydroxyl and amino.
6. The method according to claim 5, wherein the pyridine is N-vinylpyridine tetrafluoroborate, the quaternary ammonium salt is tributylvinylammonium (trifluoromethanesulfonyl) imide, the quaternary phosphonium salt is tributylvinylphosphine bromide, the pyrrolidine is N-vinyl-N-methylpyrrolidine bromide, and the piperidine is N-vinyl-N-methylpiperidine bromide; the functional polyion liquid is one or more of poly (1-vinyl-3-carboxyethylimidazole nitrate), poly (1-vinyl-3-hydroxyethyl imidazole tetrafluoroborate) and poly (1-vinyl-3-aminopropylimidazole nitrate); the initiator is one or more of benzoin ethyl ether, diphenylethanone, benzophenone, potassium persulfate, ammonium persulfate, benzoyl peroxide, di-tert-butyl peroxide and azobisisobutyronitrile; the cross-linking agent is one or more of N, N-methylene bisacrylamide, polyethylene glycol dimethacrylate, glutaraldehyde, calcium chloride aqueous solution and diisocyanate.
7. The preparation method according to claim 1, 5 or 6, wherein the ionic liquid pre-polymerization solution in the step (4) is coated on the surface of the copper grid by a spin coating method.
8. The copper grid composite ionic liquid gel flexible transparent electrode is characterized by being prepared by the preparation method of any one of claims 1 to 7.
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| CN101292362A (en) * | 2005-08-12 | 2008-10-22 | 凯博瑞奥斯技术公司 | Nanowires-based transparent conductors |
| CN104681645A (en) * | 2015-01-23 | 2015-06-03 | 华南师范大学 | Method for preparing composite transparent conductive electrode based on metal grid and metal nano-wire |
| CN105140408A (en) * | 2015-08-02 | 2015-12-09 | 北京天恒盛通科技发展有限公司 | Preparation method for flexible and transparent composite ionic liquid gel conductive electrode |
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| CN104681645A (en) * | 2015-01-23 | 2015-06-03 | 华南师范大学 | Method for preparing composite transparent conductive electrode based on metal grid and metal nano-wire |
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