CN108148469A - A kind of preparation method of aqueous UV electrically conductive inks - Google Patents
A kind of preparation method of aqueous UV electrically conductive inks Download PDFInfo
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- CN108148469A CN108148469A CN201810128796.7A CN201810128796A CN108148469A CN 108148469 A CN108148469 A CN 108148469A CN 201810128796 A CN201810128796 A CN 201810128796A CN 108148469 A CN108148469 A CN 108148469A
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- Prior art keywords
- electrically conductive
- aqueous
- pedot
- ink
- antifoaming agent
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- 239000000976 ink Substances 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 38
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 239000007800 oxidant agent Substances 0.000 claims abstract description 22
- 230000001590 oxidative effect Effects 0.000 claims abstract description 22
- 229920001940 conductive polymer Polymers 0.000 claims abstract description 21
- 239000002322 conducting polymer Substances 0.000 claims abstract description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052802 copper Inorganic materials 0.000 claims abstract description 17
- 239000010949 copper Substances 0.000 claims abstract description 17
- 239000000853 adhesive Substances 0.000 claims abstract description 16
- 230000001070 adhesive effect Effects 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003112 inhibitor Substances 0.000 claims abstract description 14
- 239000002105 nanoparticle Substances 0.000 claims abstract description 14
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 239000003381 stabilizer Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 8
- 229920000642 polymer Polymers 0.000 claims description 24
- 239000007864 aqueous solution Substances 0.000 claims description 21
- 239000000758 substrate Substances 0.000 claims description 17
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical class O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 claims description 15
- 238000013019 agitation Methods 0.000 claims description 14
- 238000007641 inkjet printing Methods 0.000 claims description 14
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 239000011152 fibreglass Substances 0.000 claims description 12
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000011575 calcium Substances 0.000 claims description 8
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 claims description 8
- 229920002401 polyacrylamide Polymers 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N 1,4-Benzenediol Natural products OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- 239000000178 monomer Substances 0.000 claims description 6
- 239000002383 tung oil Substances 0.000 claims description 6
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 5
- BBCLXYJRPRRZQW-UHFFFAOYSA-N 2-phenylnaphthalen-1-amine Chemical class C1=CC2=CC=CC=C2C(N)=C1C1=CC=CC=C1 BBCLXYJRPRRZQW-UHFFFAOYSA-N 0.000 claims description 5
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 5
- 239000011231 conductive filler Substances 0.000 claims description 5
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 5
- 235000019260 propionic acid Nutrition 0.000 claims description 5
- 229930192474 thiophene Natural products 0.000 claims description 5
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 4
- YZQBYALVHAANGI-UHFFFAOYSA-N magnesium;dihypochlorite Chemical compound [Mg+2].Cl[O-].Cl[O-] YZQBYALVHAANGI-UHFFFAOYSA-N 0.000 claims description 4
- ZJTLZYDQJHKRMQ-UHFFFAOYSA-N menadiol Chemical compound C1=CC=CC2=C(O)C(C)=CC(O)=C21 ZJTLZYDQJHKRMQ-UHFFFAOYSA-N 0.000 claims description 4
- 229950000688 phenothiazine Drugs 0.000 claims description 4
- 150000004672 propanoic acids Chemical class 0.000 claims description 4
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 4
- WJFKNYWRSNBZNX-UHFFFAOYSA-N 10H-phenothiazine Chemical compound C1=CC=C2NC3=CC=CC=C3SC2=C1 WJFKNYWRSNBZNX-UHFFFAOYSA-N 0.000 claims description 3
- -1 2- hydroxyl -4- n-octyloxy hexichol Chemical compound 0.000 claims description 3
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 2
- 125000000687 hydroquinonyl group Chemical group C1(O)=C(C=C(O)C=C1)* 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 claims 1
- 238000007639 printing Methods 0.000 abstract description 14
- 238000005245 sintering Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 abstract 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 9
- 239000012752 auxiliary agent Substances 0.000 description 9
- 239000010408 film Substances 0.000 description 9
- 239000000049 pigment Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- UMHFSEWKWORSLP-UHFFFAOYSA-N thiophene 1,1-dioxide Chemical compound O=S1(=O)C=CC=C1 UMHFSEWKWORSLP-UHFFFAOYSA-N 0.000 description 6
- LWRYDHOHXNQTSK-UHFFFAOYSA-N thiophene oxide Chemical compound O=S1C=CC=C1 LWRYDHOHXNQTSK-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000009472 formulation Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- CHXZRHMQQRUVHF-UHFFFAOYSA-N 2-hex-5-en-1,3-diynyl-5-prop-1-ynylthiophene Chemical compound CC#CC1=CC=C(C#CC#CC=C)S1 CHXZRHMQQRUVHF-UHFFFAOYSA-N 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- 244000309464 bull Species 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000012965 benzophenone Substances 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000012860 organic pigment Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000007806 chemical reaction intermediate Substances 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000001023 inorganic pigment Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 241000675108 Citrus tangerina Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- SXMUSCUQMMSSKP-UHFFFAOYSA-N [O].C=1C=CSC=1 Chemical compound [O].C=1C=CSC=1 SXMUSCUQMMSSKP-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- SGDMQXAOPGGMAH-UHFFFAOYSA-N phenol;thiophene Chemical compound C=1C=CSC=1.OC1=CC=CC=C1 SGDMQXAOPGGMAH-UHFFFAOYSA-N 0.000 description 1
- 125000001484 phenothiazinyl group Chemical group C1(=CC=CC=2SC3=CC=CC=C3NC12)* 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Landscapes
- Inks, Pencil-Leads, Or Crayons (AREA)
- Conductive Materials (AREA)
Abstract
The invention discloses a kind of preparation methods of aqueous UV electrically conductive inks, on the basis of the total weight of the electrically conductive ink, are made of the component of following mass percentage：40~60% conducting polymer PEDOT, 10~30% deionized water, 1~8% oxidant, 10~20% copper nanoparticle, 0.2~1.2% stabilizer, 2~5% adhesive, 1~6% levelling agent, 0.2~1.2% antifoaming agent, 0.2~2% polymerization inhibitor and 10~30% solvent.Technical solution using the present invention due to preparing electrically conductive ink using the conducting polymer PEDOT and Nanometer Copper of relative low price, greatly reduces cost and easy to operate, it is easy to accomplish industrialized production；The stability and consistency that technical scheme of the present invention not only simplifies technique and improve electrically conductive ink simultaneously in printing process without carrying out high temperature sintering to ink simultaneously.
Description
The application is the divisional application of the patent application application No. is 2015107903117, and the applying date of female case is 2015
It is on November 16, in, entitled：A kind of aqueous UV electrically conductive inks and preparation method thereof.
Technical field
The invention belongs to macromolecule conducting material field more particularly to a kind of preparation methods of aqueous UV electrically conductive inks.
Background technology
Aqueous UV (ultraviolet light curing) electrically conductive ink is a kind of novel ink developed in recent years, aqueous UV ink settings speed
Degree is fast, and environmental pollution is low, and energy consumption is few, becomes the universally recognized novel ink kind of current ink industry, is mainly used in
Radio frequency identification (RFID), printed wiring board (PCB), electronics panel type display, sensor, Electronic Paper, solar cell and thin
The fields such as membrane switch, aqueous UV electrically conductive inks represent the development of film printing electronic material, even entire printed electronic industry
Direction is expected to become the following cutting edge technology for changing human life style.It is applied to the electrically conductive ink of printed electronics industry at present
Mainly filled-type electrically conductive ink, conductive filler used are mostly inorganic filler, as gold, silver, copper, nickel, carbon black, graphite, carbon are fine
Dimension etc., wherein, metallic silver is most widely used with good electric conductivity, stability.Aqueous UV electrically conductive inks are consolidated with aqueous light
Change resin is binder, and addition nano-silver powder is filler, and is aided with other compositions and is prepared.Its print principle is to be with by silver
Electrically conductive ink is printed on the base materials such as above-mentioned printed wiring board, is first positioned over drying in baking oven, is cured after through uv curing machine,
It at about 150 DEG C~350 DEG C is sintered, is cooled to room temperature.After sintering the conductivity of silver conductive layer can reach 2.4 ×
10-5 Ω cm, up to 0.1 Ω/, (is square resistance printing technology to sheet resistance, refers to a square Thin film conductive material
Expect the resistance between edge to edge, the characteristic of square resistance is the same for the resistance of the square edge to edge of arbitrary size, only
With the factors such as the thickness of conductive film in relation to) hereinafter, can meet RFID antenna and PCB circuit board etc. completely applies need
It asks.
But following reason constrains the industrial applications of aqueous UV electrically conductive inks：(1) can occur in printing process chemical anti-
Should, and the temperature being sintered is high.The Shlomo Magdassi of such as American Chemical Society are in paper " Triggering the
It is pointed out in sintering of silver nanoparticles at room temperature ", when nano-Ag particles and instead
After charging polyeletrolyte contact, metal combination can be spontaneously formed, is sintered, but tests so as to fulfill the room temperature of electrically conductive ink
It equips complex.(2) silver is the metal that electric conductivity is best under room temperature, but it is to restrict aqueous UV conductions that nano-silver powder is expensive
The main reason for ink industry extensive use.The novel aqueous UV electrically conductive inks that can be solved the above problems are studied, are domestic and international
The research hotspot of ink industry is printed, therefore has critically important realistic meaning to the research and development of aqueous UV electrically conductive inks.
Therefore for drawbacks described above present in currently available technology, it is really necessary to be studied, to provide a kind of scheme,
Solve defect in the prior art.
Invention content
In view of this, it is necessory to provide a kind of preparation method of aqueous UV electrically conductive inks, technique can be simplified simultaneously
Improve the stability and consistency of electrically conductive ink.
In order to overcome the shortcomings of the prior art, the present invention provides following technical scheme：
A kind of preparation method of aqueous UV electrically conductive inks, includes the following steps：
Step S1：On the basis of the total weight of the electrically conductive ink, mass percentage is uniformly mixed for following component
Form mixed solution：
Conducting polymer PEDOT (poly- 3,4- ethylenedioxy thiophenes)：40~60%；The PEDOT is EDOT (3,4- ethylenes
Dioxythiophene monomers) polymer；
Deionized water：10~30%；
Oxidant：1~8%；The oxidant is one in calcium hypochlorite, magnesium hypochlorite, sodium hypochlorite or postassium hypochlorite
Kind is a variety of；
Solvent, 10~30%；The solvent is one or more in butyl, tung oil or normal propyl alcohol；
Copper nanoparticle conductive filler, 10~20%；
Stabilizer：0.2~1.2%；The stabilizer is cetyl trimethylammonium bromide, 2- hydroxyl -4- n-octyloxies
It is one or more in benzophenone, dodecyl trimethyl ammonium bromide or polyvinylpyrrolidone；
Adhesive：2~5%；Described adhesive is in 2,2- dihydromethyl propionic acids, dimethylolpropionic acid or polyacrylamide
It is one or more；
Levelling agent：1~6%；The levelling agent is TEGO Glide100, pure acrylic acid levelling agent, ethylene oxide or epoxy
It is one or more in propane；
Antifoaming agent：0.2~1.2%；The antifoaming agent is antifoaming agent 6800, antifoaming agent 810, antifoaming agent D105, antifoaming agent
It is one or more in T-20GA or antifoaming agent DF-100；
Polymerization inhibitor：0.2~2%；The polymerization inhibitor for hydroquinone, phenothiazine, beta-phenyl naphthylamines, methylnaphthohydroquinone THQ or
It is one or more in methylene blue；
Step S2：Above-mentioned mixed solution is heated to 65~80 DEG C persistently to stir 1 hour, then cooling 2 is small at normal temperatures
When, obtain ink mixture；
Step S3：The ink mixture obtained in step S2 in a manner of inkjet printing is printed upon and is pre-heated to 60~95
DEG C substrate on form ink pattern after the substrate is put into 30 minutes drying and mouldings in hot air drier；
Step S4：Ultraviolet light curing is carried out to the ink pattern on substrate.
As preferred technical solution, the step S1 further comprises the steps：
Mixed solution is re-formed after first preparing conducting polymer PEDOT aqueous solutions, wherein, prepare conducting polymer PEDOT
The step of aqueous solution, is as follows：
The PEDOT that mass percent is 40~60% is placed in round-bottomed flask, it is 10~30% to add in mass percent
Deionized water, mechanical agitation is carried out 10 minutes with the speed of 400r/min, then pour into mass percent as 1~8% oxidant；
Between round-bottomed flask is heated and kept 50~80 DEG C, mechanical agitation is carried out 50 minutes with the speed of 800r/min,
Then it is cooled down 1 hour under room temperature again, forms conducting polymer PEDOT aqueous solutions.
As preferred technical solution, the oxidant is calcium hypochlorite (Ca (ClO)2) when, in the step S1, institute
The oxidation reaction process for stating PEDOT and the calcium hypochlorite is as follows：
As preferred technical solution, in the step S3, the substrate selects the PET sheet after fiberglass reinforced.
As preferred technical solution, the particle diameter of the copper nanoparticle is less than 50nm, and purity is more than 99.9%.
Compared with prior art, due to technical scheme of the present invention, using the high conduction of relative low price, specific capacity
Polymer P EDOT and Nanometer Copper prepare electrically conductive ink, middle using nano-Ag particles compared with prior art, greatly reduce cost and
It is easy to operate, it is easy to accomplish industrialized production；Technical scheme of the present invention is in printing process without carrying out high temperature burning to ink
The substrate that prepare printing need to be only preheated to 60~95 DEG C by knot, then by the way of inkjet printing be prepared the present invention aqueous
UV electrically conductive inks are printed upon by the way of inkjet printing in preheated substrate, and preheated substrate can accelerate ink in substrate
Printing shaping finally cures substrate drying molding and ultraviolet light.Therefore it improves and leads simultaneously invention not only simplifies technique
The stability and consistency of electric ink.
Description of the drawings
Fig. 1 is a kind of flow diagram of the preparation method of aqueous UV electrically conductive inks of the present invention.
Fig. 2 is the SEM photograph of the aqueous UV electrically conductive inks of the embodiment of the present invention 1.
Fig. 3 is the SEM photograph of the aqueous UV electrically conductive inks of the embodiment of the present invention 2.
Fig. 4 is the SEM photograph of the aqueous UV electrically conductive inks of the embodiment of the present invention 3.
Fig. 5 is the SEM photograph of the aqueous UV electrically conductive inks of the embodiment of the present invention 4.
Specific examples below will be further illustrated the present invention with reference to above-mentioned attached drawing.
Specific embodiment
Below with reference to attached drawing, the invention will be further described.
Its print principle is printed on the base materials such as printed wiring board with by silver system electrically conductive ink in the prior art, is first placed
It is dry in baking oven, cure after through uv curing machine, it at about 150 DEG C~350 DEG C is sintered, is cooled to room temperature.
The expensive industrial applications for greatly constraining electrically conductive ink of nano-silver powder；High temperature sintering can introduce uncertain chemistry simultaneously
Reaction so as to ensure the stability and consistency of electrically conductive ink, makes it increase uncertainty in practical applications.
The defects of in order to overcome the prior art, the present invention propose a kind of preparation method of aqueous UV electrically conductive inks, referring to
Shown in Fig. 1, include the following steps：
Step S1：On the basis of the total weight of the electrically conductive ink, mass percentage is uniformly mixed for following component
Form mixed solution：
Conducting polymer PEDOT (poly- 3,4- ethylenedioxy thiophenes)：40~60%；The PEDOT is EDOT (3,4- ethylenes
Dioxythiophene monomers) polymer；
Deionized water：10~30%；
Oxidant：1~8%；The oxidant is one in calcium hypochlorite, magnesium hypochlorite, sodium hypochlorite or postassium hypochlorite
Kind is a variety of；
Solvent, 10~30%；The solvent is one or more in butyl, tung oil or normal propyl alcohol；
Copper nanoparticle conductive filler, 10~20%；
Stabilizer：0.2~1.2%；The stabilizer is cetyl trimethylammonium bromide, 2- hydroxyl -4- n-octyloxies
It is one or more in benzophenone, dodecyl trimethyl ammonium bromide or polyvinylpyrrolidone；
Adhesive：2~5%；Described adhesive is in 2,2- dihydromethyl propionic acids, dimethylolpropionic acid or polyacrylamide
It is one or more；
Levelling agent：1~6%；The levelling agent is TEGO Glide100, pure acrylic acid levelling agent, ethylene oxide or epoxy
It is one or more in propane；
Antifoaming agent：0.2~1.2%；The antifoaming agent is antifoaming agent 6800, antifoaming agent 810, antifoaming agent D105, antifoaming agent
It is one or more in T-20GA or antifoaming agent DF-100；
Polymerization inhibitor：0.2~2%；The polymerization inhibitor for hydroquinone, phenothiazine, beta-phenyl naphthylamines, methylnaphthohydroquinone THQ or
It is one or more in methylene blue；
Wherein, further comprise the steps in step S1：
Mixed solution is re-formed after first preparing conducting polymer PEDOT aqueous solutions, wherein, prepare conducting polymer PEDOT
The step of aqueous solution, is as follows：
The PEDOT that mass percent is 40~60% is placed in round-bottomed flask, it is 10~30% to add in mass percent
Deionized water, mechanical agitation is carried out 10 minutes with the speed of 400r/min, then pour into mass percent as 1~8% oxidant；
Between round-bottomed flask is heated and kept 50~80 DEG C, mechanical agitation is carried out 50 minutes with the speed of 800r/min,
Then it is cooled down 1 hour under room temperature again, forms conducting polymer PEDOT aqueous solutions.
When oxidant is calcium hypochlorite (Ca (ClO) 2), in the step S1, the PEDOT and the calcium hypochlorite
Oxidation reaction process is as follows：
PEDOT is the polymer of EDOT (3,4-ethylene dioxythiophene monomer), and (3,4-ethylene dioxythiophene polymerize PEDOT
Object) in calcium hypochlorite Ca (ClO) 2 times oxidation reaction mechanisms：Wherein OCl- (hypochlorous acid) is oxidant, it is by PEDOT (3,4- second
Support dioxy thiophene polymer) in thiophene (a) be oxidized to its corresponding thiophene -1- oxide (b).Similarly, thiophene -1- oxides
(b) it is oxidized to its corresponding thiophene -1,1- dioxide (c).In this reaction, thiophene -1- oxides (b) are assumed thiophene
A reaction intermediate in fen -1,1- dioxide (c).Finally, thiophene -1,1- dioxide (c) further aoxidizes
The SO2 in compound is eliminated, and by the necleophilic reaction of water, hydroxyl is allowed to be attached to thiophene -1,1- dioxide (c), thus
Form the aqueous solutions of polymers with high conductivity.
Step S2：Above-mentioned mixed solution is heated to 65~80 DEG C persistently to stir 1 hour, then cooling 2 is small at normal temperatures
When, obtain ink mixture；
Step S3：The ink mixture obtained in step S2 in a manner of inkjet printing is printed upon and is pre-heated to 60~95
DEG C substrate on form ink pattern after the substrate is put into 30 minutes drying and mouldings in hot air drier；
Step S4：Ultraviolet light curing is carried out to the ink pattern on substrate.
Preferably, in above-mentioned technical proposal, naturally it is also possible to according to the actual demand of aqueous UV electrically conductive inks, be not added with pigment
Aqueous UV electrically conductive inks be gloss oil；The type for needing pigment to be added is any color for thinking addition, can be organic pigment
Or one or both of inorganic pigment, it is 5~10% to need pigment mass percentage to be added.
Preferably, substrate selects the PET sheet after fiberglass reinforced, because the heat resistance of pure PET is not high, thermal deformation temperature
Degree is only 90 DEG C or so, but the PET mechanical properties after fiberglass reinforced can similar to engineering plastics, heat distortion temperatures such as PC, PA
Reach 225 DEG C.
The defects of in order to overcome the prior art, the present invention propose a kind of water at low cost, simple for process and function admirable
Property UV electrically conductive inks, on the basis of the total weight of the ink, are mainly made of the component of following percentage composition：
40~60% conducting polymer, 10~30% deionized water, 1~8% oxidant, 10~20% conduction
Filler, 0.2~1.2% stabilizer, 2~5% adhesive, 1~6% levelling agent, 0.2~1.2% antifoaming agent, 0.2
~2% polymerization inhibitor and 10~30% solvent, wherein, conducting polymer is 40~60% PEDOT (poly- 3,4- ethylenes two
Oxygen thiophene), relative low price, the characteristics of specific capacity is high.Conducting polymer is the key that determine aqueous UV electrically conductive inks performance.
Conducting polymer PEDOT is the polymer of EDOT (3,4-ethylene dioxythiophene monomer), has special electricity, optical property,
The features such as its molecular structure is simple, energy gap is small, conductivity high (600S/cm).
Since PEDOT sheets are as insoluble polymer, it is impossible to directly utilize its special electric conductivity.But it sends out in test
Existing, adding in after oxidant carries out oxidation reaction can make PEDOT form water-soluble polymer, and with high conductivity.Oxidant is
One or more of calcium hypochlorite, magnesium hypochlorite, sodium hypochlorite or postassium hypochlorite, for being chemically reacted with PEDOT
Aqueous solutions of polymers of the generation with high conductivity.
In test of many times, calcium hypochlorite (Ca (ClO) is found2) with PEDOT occur oxidation reaction after, aqueous solutions of polymers
Electric conductivity be greatly improved, specific reaction process is as follows：
PEDOT is the polymer of EDOT (3,4-ethylene dioxythiophene monomer), and (3,4-ethylene dioxythiophene polymerize PEDOT
Object) at calcium hypochlorite Ca (ClO)2Lower oxidation reaction mechanism：Wherein OCl- (hypochlorous acid) is oxidant, it is by PEDOT (3,4- second
Support dioxy thiophene polymer) in thiophene (a) be oxidized to its corresponding thiophene -1- oxide (b).Similarly, thiophene -1- oxides
(b) it is oxidized to its corresponding thiophene -1,1- dioxide (c).In this reaction, thiophene -1- oxides (b) are assumed thiophene
A reaction intermediate in fen -1,1- dioxide (c).Finally, thiophene -1,1- dioxide (c) further aoxidizes
Eliminate the SO in compound2, and by the necleophilic reaction of water, hydroxyl is allowed to be attached to thiophene -1,1- dioxide (c), thus
Form the aqueous solutions of polymers with high conductivity.
Although the conductive polymer polymer of above-mentioned formation is pretty good in water-soluble state electric conductivity, after its curing, lead
Electrical property can substantially reduce.In order to promote the electric conductivity of the aqueous UV electrically conductive inks of the present invention, add in above-mentioned conducting polymer
Enter copper nanoparticle conductive filler, so as to the electric conductivity of significant increase ink.
Preferably, the particle diameter of copper nanoparticle is less than 50nm, and purity is more than 99.9%, so as to enable copper nanoparticle equal
It is even to be blended in ink.
Copper nanoparticle easily aoxidizes at normal temperatures, and the electric conductivity of the copper nanoparticle after oxidation substantially reduces.Therefore this hair
Stabilizer is added in bright formula prevents the oxidation of copper nanoparticle, and further, stabilizer is cetyl trimethylammonium bromide, 2-
It is one or more in hydroxyl -4- oxy-octyl benzophenones, dodecyl trimethyl ammonium bromide or polyvinylpyrrolidone.
The printing viscosity of ink is to ensure the key factor of print quality, and the adhesive in inventive formulation can control ink
Viscosity.Further, adhesive 2, one kind or more in 2- dihydromethyl propionic acids, dimethylolpropionic acid or polyacrylamide
Kind；Particularly preferably using the polyacrylamide (PAM) with good flocculability.Adhesive has flocculability and thickening power,
Segregation phenomenon can be occurred by being avoided that between ink and mixed solvent.
Solvent in inventive formulation is the auxiliary agent for diluting ink, and above-mentioned PEDOT chemical reaction generation tools occur
The aqueous solutions of polymers and other auxiliary agents for having high conductivity are diluted.Further, solvent for butyl, tung oil or
It is one or more in normal propyl alcohol.
Levelling agent in inventive formulation is mainly used to improve the mobility of UV curable ink, enables ink in base
Levelling on material.If levelability is bad, printed matter can be caused the phenomenon that tangerine peel, sagging, shrinkage cavity etc. are bad occur, do not had not only
Good conductive effect, but also other performances can be reduced.Further, levelling agent is TEGO Glide100, pure acrylic acid stream
It is one or more in flat agent, ethylene oxide or propylene oxide；
Antifoaming agent in inventive formulation is to eliminate ultraviolet light curing electrically conductive ink occurs in stirring the one of bubble
Kind auxiliary agent.Because some auxiliary agents such as table in ink and activating agent, levelling agent can generate during ink stirring, grinding
Bubble.Further, antifoaming agent is antifoaming agent 6800, antifoaming agent 810, antifoaming agent D105, antifoaming agent T-20GA or antifoaming agent DF-
It is one or more in 100；
Polymerization inhibitor in inventive formulation is a kind of a kind of auxiliary agent hindered or retardation of curing reacts, can inhibit unsaturated
The thermal polymerization of object, while it is avoided that equipment gum deposit and blocking in printing process.Further, polymerization inhibitor is hydroquinone, phenol thiophene
It is one or more in piperazine, beta-phenyl naphthylamines, methylnaphthohydroquinone THQ or methylene blue.
In the preferred embodiment of the present invention, ink further includes mass percentage as 5~10% pigment, passes through
Different types of pigment is added so as to allow ink that there is multiple color, meets the application demand for being unable to occasion.Whether pigment
The aqueous UV electrically conductive inks that addition according to the actual demand of aqueous UV electrically conductive inks, can be not added with pigment are gloss oil；Need can be
One or both of organic pigment or inorganic pigment.
Below again by the embodiment during specific experiment to further instruction of the present invention.
Embodiment 1
The first step, the synthesis of PEDOT：The PEDOT of mass percent 40% is placed in the round-bottomed flask of 1000ml, is added in
The deionized water of weight 28% carries out mechanical agitation 10 minutes, then pour into 1% hypochlorous acid of oxidant with the speed of 400r/min
Between round-bottomed flask is heated and kept 80 DEG C, mechanical agitation is carried out 50 minutes with the speed of 800r/min for calcium, then room temperature again
Lower cooling 1 hour, has thus generated the aqueous solutions of polymers with high conductivity.
Second step, by the mass percent of above-mentioned generation for 40%PEDOT high conductivities aqueous solutions of polymers and other
Auxiliary agent mixes according to a certain percentage, is fitted into vessel and is placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus, 65 DEG C of heating
Stirring 1 hour, then cools down 2 hours to get ink to be prepared again under room temperature.Wherein by mass percentage, selection of auxiliary：
(copper nanoparticle 10% of 50nm 99.9%, stabilizer：Cetyl trimethylammonium bromide 1%；Adhesive 2,2- dihydroxymethyls
Propionic acid, 2%, levelling agent is TEGO Glide100,1%；Antifoaming agent be antifoaming agent 6800,0.2%；Polymerization inhibitor is to benzene two
Phenol, 1%；Solvent is butyl 15.8%.), it is not added with any pigment and intends generating aqueous UV electrically conductive inks gloss oil.
Third walks, and the PET sheet after fiberglass reinforced for preparing printing is preheated to 60 DEG C, then using the side of inkjet printing
On the PET battens that the aqueous UV electrically conductive inks of above-mentioned preparation are printed upon after fiberglass reinforced by the way of the inkjet printing by formula,
Then printed batten is put into 30 minutes drying and mouldings in hot air drier, finally carries out ultraviolet light curing.
Embodiment 2
The first step, the synthesis of PEDOT：The PEDOT of mass percent 45% is placed in the round-bottomed flask of 1000ml, is added in
The deionized water of weight 10% carries out mechanical agitation 10 minutes, then pour into 2% hypochlorous acid of oxidant with the speed of 400r/min
Between round-bottomed flask is heated and kept 60 DEG C, mechanical agitation is carried out 50 minutes with the speed of 800r/min for magnesium, then room temperature again
Lower cooling 1 hour, has thus generated the aqueous solutions of polymers with high conductivity.
Second step, by the aqueous solutions of polymers of the PEDOT high conductivities of above-mentioned generation and other auxiliary agents according to certain ratio
Example mixing, is fitted into vessel and is placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus, 75 DEG C of heating stirrings 1 hour, Ran Houzai
It is cooled down 2 hours under room temperature, up to ink to be prepared.Wherein by mass percentage, selection of auxiliary：(50nm's 99.9% receives
Rice copper powder 16%, stabilizer：Dodecyl trimethyl ammonium bromide 0.2%；Adhesive is dimethylolpropionic acid, 1%, levelling agent is
Pure acrylic acid levelling agent, 1.8%；Antifoaming agent is to defoam Antifoam Agent 810,0.5%；Polymerization inhibitor is phenothiazine, 0.8%；Solvent
For tung oil 16%.), while add 6.7% organic pigment red 146.
Third walks, and the PET sheet after fiberglass reinforced for preparing printing is preheated to 85 DEG C, then using the side of inkjet printing
On the PET battens that the aqueous UV electrically conductive inks of above-mentioned preparation are printed upon after fiberglass reinforced by the way of the inkjet printing by formula,
Then printed batten is put into 30 minutes drying and mouldings in hot air drier, finally carries out ultraviolet light curing.
Embodiment 3
The first step, the synthesis of PEDOT：The PEDOT of mass percent 45.2% is placed in the round-bottomed flask of 1000ml, is added
Enter the deionized water of weight 10%, mechanical agitation is carried out 10 minutes, then pour into 5% hypochlorous acid of oxidant with the speed of 400r/min
Between round-bottomed flask is heated and kept 70 DEG C, mechanical agitation is carried out 50 minutes with the speed of 800r/min for sodium, then room temperature again
Lower cooling 1 hour, has thus generated the aqueous solutions of polymers with high conductivity.
Second step, by the aqueous solutions of polymers of the PEDOT high conductivities of above-mentioned generation and other auxiliary agents according to certain ratio
Example mixing, is fitted into vessel and is placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus, 80 DEG C of heating stirrings 1 hour, Ran Houzai
It is cooled down 2 hours under room temperature, up to ink to be prepared.Wherein by mass percentage, selection of auxiliary：(50nm's 99.9% receives
Rice copper powder 12%, stabilizer：Cetyl trimethylammonium bromide 0.5%；Adhesive is polyacrylamide, 1.5%, levelling agent is
Ethylene oxide, 1%；Antifoaming agent is antifoaming agent D105,0.8%；Polymerization inhibitor be beta-phenyl naphthylamines, 1%；Solvent is tung oil
18%.；), while add 5% phthalocyanine blue.
Third walks, and the PET sheet after fiberglass reinforced for preparing printing is preheated to 90 DEG C, then using the side of inkjet printing
On the PET battens that the aqueous UV electrically conductive inks of above-mentioned preparation are printed upon after fiberglass reinforced by the way of the inkjet printing by formula,
Then printed batten is put into 30 minutes drying and mouldings in hot air drier, finally carries out ultraviolet light curing.
Embodiment 4
The first step, the synthesis of PEDOT：The PEDOT of mass percent 50% is placed in the round-bottomed flask of 1000ml, is added in
The deionized water of weight 10% carries out mechanical agitation 10 minutes, then pour into 3% hypochlorous acid of oxidant with the speed of 400r/min
Between round-bottomed flask is heated and kept 65 DEG C, mechanical agitation is carried out 50 minutes with the speed of 800r/min for calcium, then room temperature again
Lower cooling 1 hour, has thus generated the aqueous solutions of polymers with high conductivity.
Second step, by the aqueous solutions of polymers of the PEDOT high conductivities of above-mentioned generation and other auxiliary agents according to certain ratio
Example mixing, is fitted into vessel and is placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus, 80 DEG C of heating stirrings 1 hour, Ran Houzai
It is cooled down 2 hours under room temperature, up to ink to be prepared.Wherein by mass percentage, selection of auxiliary：((50nm's 99.9%
Copper nanoparticle 18%, stabilizer：Polyvinylpyrrolidone 1%；Adhesive is polyacrylamide, 1%, levelling agent is pure acrylic acid
Levelling agent, 1%；Antifoaming agent is antifoaming agent DF-100,0.2%；Polymerization inhibitor is methylene blue, 0.2%；Solvent is normal propyl alcohol
10.6%.), while add 5% pigment orange 36 (Clariant HL).
Third walks, and the PET sheet after fiberglass reinforced for preparing printing is preheated to 95 DEG C, then using the side of inkjet printing
On the PET battens that the aqueous UV electrically conductive inks of above-mentioned preparation are printed upon after fiberglass reinforced by the way of the inkjet printing by formula,
Then printed batten is put into 30 minutes drying and mouldings in hot air drier, finally carries out ultraviolet light curing.
The performance of the aqueous UV electrically conductive inks of above-described embodiment is detected again below.
In order to measure the electric conductivity of the aqueous UV electrically conductive inks of technical solution of the present invention, will be prepared by above-described embodiment
The difference ink jet printing of aqueous UV electrically conductive inks on circuit board, being put into 30 minutes drying and mouldings in hot air drier, it is most laggard
Row ultraviolet light cures, and is cooled to room temperature.Above-described embodiment ink film layer is swept using with JSM-6460 types scanning electron microscope
SEM photograph after retouching, specifically as shown in Fig. 2, Fig. 3, Fig. 4 and Fig. 5, respectively embodiment 1, embodiment 2, embodiment 3, embodiment
4 SEM photograph.Simultaneously using the conductivity of U.S. sensION+EC5 portable electric conductance test ink film layers, while to more than
4 embodiments firmly tear ink film 30 times with 4M adhesive tapes respectively, then survey the ink film layer conductivity after tearing.
In embodiment 1, the particle granules in ink are larger and not close, there are larger gap, therefore the resistance of film
Larger, conductivity is only 0.15 × 10-5 Ω cm, square resistance be 203.1 Ω/ (is square resistance printing technology,
Refer to the resistance between a square thin film of conductive material edge to edge)；In embodiment 3, conducting polymer particle is equal in ink
Uniform close, the conductive path that can have been formed, therefore, laminated film conductivity at this time reach 5.62 × 10-5 Ω cm,
Resistance is relatively low, and square resistance is only 0.23 Ω/.Embodiment 2 and its conductivity of embodiment 4 between embodiment 1 and embodiment 3 it
Between, value please refer to table 1.The results are shown in Table 1 for its experiment, and square resistance, conductivity variations are little before and after ink film is torn, and show
Ink has good adhesive force.
Square resistance, conductivity test result before and after 1 aqueous UV electrically conductive inks of table are torn 30 times
The explanation of above example is only intended to facilitate the understanding of the method and its core concept of the invention.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvement and modification are also fallen within the protection scope of the claims of the present invention.
The foregoing description of the disclosed embodiments enables professional and technical personnel in the field to realize or use the present invention.
A variety of modifications of these embodiments will be apparent for those skilled in the art, it is as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and the principles and novel features disclosed herein phase one
The most wide range caused.
Claims (5)
1. a kind of preparation method of aqueous UV electrically conductive inks, which is characterized in that include the following steps：
Step S1：On the basis of the total weight of the electrically conductive ink, mass percentage is uniformly mixed to form for following component
Mixed solution：
Conducting polymer PEDOT (poly- 3,4- ethylenedioxy thiophenes)：40~60%；The PEDOT is EDOT (3,4- enedioxies
Thiophene monomer) polymer；
Deionized water：10~30%；
Oxidant：1~8%；The oxidant be calcium hypochlorite, magnesium hypochlorite, sodium hypochlorite or postassium hypochlorite in one kind or
Person is a variety of；
Solvent, 10~30%；The solvent is one or more in butyl, tung oil or normal propyl alcohol；
Copper nanoparticle conductive filler, 10~20%；
Stabilizer：0.2~1.2%；The stabilizer is cetyl trimethylammonium bromide, 2- hydroxyl -4- n-octyloxy hexichol
It is one or more in ketone, dodecyl trimethyl ammonium bromide or polyvinylpyrrolidone；
Adhesive：2~5%；Described adhesive is one in 2,2- dihydromethyl propionic acids, dimethylolpropionic acid or polyacrylamide
Kind is a variety of；
Levelling agent：1~6%；The levelling agent is TEGO Glide100, pure acrylic acid levelling agent, ethylene oxide or propylene oxide
In it is one or more；
Antifoaming agent：0.2~1.2%；The antifoaming agent is antifoaming agent 6800, antifoaming agent 810, antifoaming agent D105, antifoaming agent T-
It is one or more in 20GA or antifoaming agent DF-100；
Polymerization inhibitor：0.2~2%；The polymerization inhibitor is hydroquinone, phenothiazine, beta-phenyl naphthylamines, methylnaphthohydroquinone THQ or methylene
It is one or more in base basket；
Step S2：Above-mentioned mixed solution is heated to 65~80 DEG C persistently to stir 1 hour, then cools down 2 hours, obtains at normal temperatures
Ink mixture；
Step S3：The ink mixture obtained in step S2 in a manner of inkjet printing is printed upon and is pre-heated to 60~95 DEG C
It is formed on substrate after ink pattern and the substrate is put into 30 minutes drying and mouldings in hot air drier；
Step S4：Ultraviolet light curing is carried out to the ink pattern on substrate.
2. the preparation method of aqueous UV electrically conductive inks according to claim 1, which is characterized in that the step S1 is further
Include the following steps：
Mixed solution is re-formed after first preparing conducting polymer PEDOT aqueous solutions, wherein, it is water-soluble to prepare conducting polymer PEDOT
The step of liquid, is as follows：
The PEDOT that mass percent is 40~60% is placed in round-bottomed flask, it is 10~30% to go to add in mass percent
Ionized water carries out mechanical agitation 10 minutes with the speed of 400r/min, then pours into mass percent as 1~8% oxidant；
Between round-bottomed flask is heated and kept 50~80 DEG C, mechanical agitation is carried out 50 minutes with the speed of 800r/min, then
It is cooled down 1 hour under room temperature again, forms conducting polymer PEDOT aqueous solutions.
3. the preparation method of aqueous UV electrically conductive inks according to claim 1 or 2, which is characterized in that the oxidant is
Calcium hypochlorite (Ca (ClO)2) when, in the step S1, the oxidation reaction process of the PEDOT and the calcium hypochlorite is such as
Under：
4. the preparation method of aqueous UV electrically conductive inks according to claim 1 or 2, which is characterized in that in the step S3
In, the substrate selects the PET sheet after fiberglass reinforced.
5. the preparation method of aqueous UV electrically conductive inks according to claim 1 or 2, which is characterized in that the copper nanoparticle
Particle diameter be less than 50nm, purity be more than 99.9%.
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| CN110527358A (en) * | 2019-08-19 | 2019-12-03 | 上海佳利笔业文具有限公司 | A kind of composite material pen core and preparation method thereof |
| CN111469573A (en) * | 2020-05-28 | 2020-07-31 | 安庆盛华纸质包装有限公司 | Printing ink processing technology of high-performance coated paper sheet |
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| CN109935469A (en) * | 2017-12-15 | 2019-06-25 | 钰邦科技股份有限公司 | Printed form conduction composite mortar, capacitor and its manufacturing method |
| CN108219577A (en) * | 2017-12-29 | 2018-06-29 | 杭州卡丽佛装饰材料科技有限公司 | A kind of printing water-based ink of pvc coloured silk films and water-based ink printing technology |
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| CN103804995A (en) * | 2012-11-09 | 2014-05-21 | 财团法人工业技术研究院 | Conductive ink composition and transparent conductive film |
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| CN110527358A (en) * | 2019-08-19 | 2019-12-03 | 上海佳利笔业文具有限公司 | A kind of composite material pen core and preparation method thereof |
| CN111469573A (en) * | 2020-05-28 | 2020-07-31 | 安庆盛华纸质包装有限公司 | Printing ink processing technology of high-performance coated paper sheet |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105400281A (en) | 2016-03-16 |
| CN105400281B (en) | 2018-03-23 |
| CN108148469B (en) | 2021-01-08 |
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