CN104650652A - Nano-silver conductive ink and preparation method thereof - Google Patents
Nano-silver conductive ink and preparation method thereof Download PDFInfo
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Abstract
Belonging to the technical field of high polymer materials, the invention relates to a nano-silver conductive ink and a preparation method thereof. The nano-silver conductive ink is characterized by being prepared from the following components by weight: 0.05-2 parts of nano-silver; 0.01-2 parts of a nano-additive; 0.05-10 parts of a high polymer binder; 0.001-2 parts of a surface additive; 0.001-2 parts of an anti-settling agent; 0.001-2 parts of a leveling agent; 0.001-2 parts of a dispersion agent; 0.001-5 parts of a curing agent; and 73-95 parts of an organic solvent. The product prepared by the invention not only can be applied to touch screen cover glass, but also can be further popularized to display panels, LED display, thin-film solar cells, electromagnetic shielding and other fields.
Description
Technical field
the invention belongs to electrically conductive ink field, particularly relate to a kind of Nano silver conductive ink and preparation method thereof.background technology
At present; the ITO conducting wire for having etched of the visible area of touch-screen; existing printed form conductive silver paste is essentially opaque silver grey property or canescence; silver powder is micron particles or flap-type; in this oleaginous system silver slurry, the content of argent is 40-75%; the consumption of noble silver is more, cost is high, does not also have silver powder content to account for the transparent wire reticulated printing conductive silver paste of total ink less than 5% at present.
Mainly there is following problem in traditional transparent conductive film based on tin indium oxide (ITO): the key element indium in (1) ITO faces comparatively serious shortage of resources problem, and price is more and more higher; (2) ito thin film is processed in magnetron sputtering mode usually, and apparatus expensive, complete processing are complicated, and energy consumption is high; (3) needed for ITO, processing temperature is higher, and the temperature that flexible parent metal can bear usually will, lower than 200 ° of C, cause the ito thin film obtained easily to occur defect for meeting base material temperature ability to bear; (4) ITO is a kind of oxide material, and fragility is comparatively large comparatively speaking, easily breaks, be difficult to the snappiness of satisfied touch-control product of new generation to transparent conductive film, the demand of portability after bending; (5) be difficult to be prepared into conducting wire by silk-screen printing technique.
According to investigation, the transparent wire printing ink that OGS touching technique obtains greatly reduces the development cost of technology, and manufacturer can be made effectively to utilize existing equipment, reduces device upgrade and to regenerate the cost produced.
Summary of the invention
The object of the invention is to for solving the problem, provide a kind of transparent silk-screen Nano silver conductive ink that can be used for touch-screen cover-plate glass, by regulating resin types and light transmission, mist degree, the sheet resistance of the realization of composition content parameter to conducting wire of silver nanoparticle and the polymer binder used in Nano silver conductive ink, surface hardness, chemical solvent resistance can wait adjustment.The product of prepared electrically conducting transparent circuit finally not only can be applied to Touch Screen cover-plate glass, and can further genralrlization to fields such as display pannel, LED display, thin-film solar cells, electromagnetic shieldings.
Another object of the present invention is to provide a kind of preparation method of above-mentioned conductive nano silver slurry.
Object of the present invention can be realized by following technical proposals:
A kind of Nano silver conductive ink, is characterized in that, be made up of the component comprising following weight part:
Nanometer silver 0.05 ~ 2 part;
Nano assistant 0.01 ~ 2 part;
Polymer binder 0.05 ~ 10 part;
Surface modifier 0.001 ~ 2 part;
Anti-settling agent 0.001 ~ 2 part;
Flow agent 0.001 ~ 2 part;
Dispersion agent 0.001 ~ 2 part;
0.001 ~ 5 part, solidifying agent;
Organic solvent 73 ~ 95 parts.
Described nanometer silver be selected from nanometer silver rod, nano-silver thread, nanometer ping-pong ball or nano silver slice one or more.
Described nano assistant be selected from titania nanoparticles, graphene nanometer sheet, Nano carbon balls, carbon nanotube, aluminum oxide nanoparticle, Zinc oxide nanoparticle or ferric oxide nanometer particle one or more.
Described polymer binder be selected from cellulose acetate, soluble cotton, Vltra tears, cellulose acetate butyrate, epoxy resin, acrylate resin, vibrin, polyamide resin, polyimide resin, acrylate, fluorocarbon resin, Polyglycolic acid fibre (PEDOT) or polyaniline one or more; Preferably, polymer binder is selected from one or more in acrylate resin, cellulose acetate, Polyglycolic acid fibre (PEDOT) or polyketone resin.
Described surface modifier be selected from cetyl trimethylammonium bromide, halogenated phosphates, palmityl trimethyl ammonium chloride, diallyl dimethyl ammoniumchloride, polyacrylamide or non-ionic type fluorocarbon surfactant one or more.
Described anti-settling agent to be selected from Mitsui chemical industry anti-settling auxiliary agent FDSS-5, Mitsui chemical industry anti-settling auxiliary agent FD380, organobentonite 881-A, organobentonite 881-B, organobentonite P-1, this ST auxiliary rheological agents of extra large name, polyimide wax MT 6650, polyimide wax BYK 420, polyimide wax BYK-425 or polyimide wax BYK-410 one or more; Preferably, anti-settling agent is selected from one or more in polyimide wax BYK 420, polyimide wax BYK-425, Mitsui chemical industry anti-settling auxiliary agent FD380 or Mitsui chemical industry anti-settling auxiliary agent FDSS-5.
Described flow agent be selected from Bick BYK-300, Bick BYK-333, Bick BYK-310, Bick BYK-371, Bick BYK358, enlightening height Tego900, enlightening height Tego410, enlightening height Tego432 or enlightening height Tego450 one or more.
Described dispersion agent to be selected from enlightening height Dispers610, enlightening height Dispers610S, enlightening height Dispers655, enlightening height Dispers700, enlightening height Dispers710, enlightening height Dispers740W, enlightening height Dispers750W, enlightening height Dispers760W, enlightening height Dispers 750w or enlightening height Dispers 760w one or more.
Described solidifying agent is selected from Bayer Desmodur 3390BA/SN, Bayer Desmodur N3300, Bayer Bayhydur XP2451, Bayer Bayhydur 2570, Bayer Desmodur RC, Japan Asahi Chemical Industry NPU solidifying agent CORONATE HXR, Japan Asahi Chemical Industry NPU solidifying agent HX, Japan Asahi Chemical Industry NPU solidifying agent HK, Japan Asahi Chemical Industry NPU solidifying agent, Japan Asahi Chemical Industry NPU solidifying agent, Japan Asahi Chemical Industry CORONATE 2604, Japan Asahi Chemical Industry CORONATE MF-K60X, Japan Asahi Chemical Industry CORONATE MF-B60X, Degussa BI1358A, Japanese fuji Fujicure FXR1081, or one or more in Fujicure FXR 1020, preferably, solidifying agent is selected from one or more in Bayer Desmodur 3390BA/SN, Japanese Asahi Chemical Industry CORONATE MF-B60X or Degussa BI1358A.
Described organic solvent is selected from methyl alcohol, ethanol, Virahol, dimethyl formamide, ethylene glycol, propylene glycol, glycerol, propylene glycol monomethyl ether, propylene-glycol ethyl ether, propandiol butyl ether, dipropylene glycol methyl ether, dipropylene, dipropylene glycol hexyl ether, toluene, dimethylbenzene, ethyl acetate, propyl acetate, isopropyl acetate, methyl-formiate, ethyl formate, ethyl lactate, Valeric acid ethylester, acetone, methylethylketone, butanone, isophorone, diacetone alcohol, pimelinketone, nylon acid dimethyl ester (DBE), Terpineol 350, turps, diethylene glycol ether, acetic acid glycol ether monoethyl ether ester, or one or more in propylene glycol phenylate.
A preparation method for Nano silver conductive ink, comprises the steps:
(1) first 0.05 ~ 10 part of polymer binder is joined in organic solvent, be uniformly dissolved under dispersion machine dispersed with stirring and obtain cream liquid A;
(2) 0.05 ~ 2 part of nanometer silver is scattered in organic solvent, obtains homodisperse nano silver dispersion B;
(3) cream liquid A obtained above to be mixed with nano silver dispersion B and after stirring, add 0.001 ~ 5 part of solidifying agent, 0.001 ~ 2 part of dispersion agent, 0.001 ~ 2 part of surface modifier, 0.001 ~ 2 part of anti-settling agent, 0.001 ~ 2 part of flow agent and 0.01 ~ 2 part of nano assistant again, be dispersed to and mix, and can Nano silver conductive ink be obtained 3 ~ 10 times with three-roller grinding.
Described organic solvent total amount is 73 ~ 95 parts;
Consumption of organic solvent in described step (1) is the half of organic solvent total amount;
Consumption of organic solvent in described step (2) is remaining organic solvent.
beneficial effect:
(1) Nano silver conductive ink of the present invention realizes the high transparent of printed wiring, be specially adapted to the high transparent requirement of visible area circuit on Touch Screen, display pannel, the requirement of patterning can be realized by silk screen printing, and the equipment of existing producer can be relied on, not need significantly to adjust.
(2) after silk screen printing, the thickness of line layer dry film is between 400 ~ 800nm, and this thickness is easy to laser radium carving, wet-etching technology, makes wire sizes can obtain precision and the fineness of manufacturer's needs;
(3) adopt argent content in this Nano silver conductive ink low, reduce precious metal waste, 1/20 ~ 1/50 of normally common touch screen silver slurry.
(4) electrically conductive ink can according to different substrate materials adjustment formula, and can meet at different material sticking power, snappiness, the performance index such as hardness, preparation method of the present invention is simple, solves transmittance, line pattern, adhesion problem simultaneously.
(5) electrically conductive ink be alternative ITO be widely used in the fields such as Touch Screen, display pannel, electromagnetic shielding, light-emitting diode display, electroluminescent device and thin-film solar cells.
Embodiment
Nano silver conductive ink of the present invention can be used for the transparent silk-screen of touch-screen cover-plate glass, and base material is one or more in toughened glass, polyethylene terephthalate, polycarbonate, polyvinyl alcohol, polyethylene, polyvinyl chloride, polymethylmethacrylate, polydimethylsiloxane, urethane, polypropylene, polystyrene, polyvinylidene difluoride (PVDF) or tetrafluoroethylene.The transmittance of the material after the coating obtained is greater than 80%, film surface resistance 10 ~ 500 Ω/, surface hardness >=1H.
The testing process of electrically conductive ink: with polyethylene terephthalate (PET) for transparent flexible base material, himself transmittance is 92%, and thickness is 188 microns.By the above-mentioned nano conductive printing ink prepared with the half tone of 350 order PET, be coated on PET base material on the surface in the mode of silk screen printing, in the convection oven of 140-150 DEG C, heat 30-60min.Finally adopt four-point probe to measure the sheet resistance of gained film, the transmittance of the prepared film of photoelectricity haze meter test and mist degree, and test the impact of different bending angle on sheet resistance.Below in conjunction with embodiment, the specific embodiment of the present invention is further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
The percentage ratio of the following stated, except particularly pointing out, is mass percent.
Embodiment
A preparation method for Nano silver conductive ink, comprises the steps:
(1) prepare each component raw material by the proportioning in table 1, polymer binder is joined in organic solvent, be uniformly dissolved under dispersion machine dispersed with stirring and obtain cream liquid A;
(2) nanometer silver is scattered in organic solvent, obtains homodisperse nano silver dispersion B;
(3) cream liquid A obtained above to be mixed with nano silver dispersion B and after stirring, add solidifying agent, dispersion agent, surface modifier, anti-settling agent, flow agent and nano assistant again, be dispersed to and mix, and can Nano silver conductive ink be obtained 3 ~ 10 times with three-roller grinding.
Consumption of organic solvent in described step (1) is the half of organic solvent total amount;
Consumption of organic solvent in described step (2) is remaining organic solvent.
Table 1
In embodiment 1, the mean diameter of nanometer silver rod is 40 nanometers, and mean length is 5-10 micron, and length-to-diameter ratio exceedes and is about 100 ~ 300.
Table 2
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Nanometer silver concentration | 2.3% | 0.05% | 0.9% | 1.6% |
| Electrically conductive ink viscosity | 8000-10000 mPa·s | 7000-9000 mPa·s | 6000-8000 mPa·s | 9000-12000 mPa·s |
| Sheet resistance | 40-200 Ω/□ | 100-300 Ω/□ | 150-300 Ω/□ | 80-250 Ω/□ |
| The transmittance of opaque line | 82% | 84% | 83.5% | 85% |
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a Nano silver conductive ink, is characterized in that, is made up of the component comprising following weight part:
Nanometer silver 0.05 ~ 2 part;
Nano assistant 0.01 ~ 2 part;
Polymer binder 0.05 ~ 10 part;
Surface modifier 0.001 ~ 2 part;
Anti-settling agent 0.001 ~ 2 part;
Flow agent 0.001 ~ 2 part;
Dispersion agent 0.001 ~ 2 part;
0.001 ~ 5 part, solidifying agent;
Organic solvent 73 ~ 95 parts.
2. a kind of Nano silver conductive ink according to claim 1, is characterized in that, described nanometer silver be selected from nanometer silver rod, nano-silver thread, nanometer ping-pong ball or nano silver slice one or more; Described nano assistant be selected from titania nanoparticles, graphene nanometer sheet, Nano carbon balls, carbon nanotube, aluminum oxide nanoparticle, Zinc oxide nanoparticle or ferric oxide nanometer particle one or more.
3. a kind of Nano silver conductive ink according to claim 1, it is characterized in that, described surface modifier be selected from cetyl trimethylammonium bromide, halogenated phosphates, palmityl trimethyl ammonium chloride, diallyl dimethyl ammoniumchloride, polyacrylamide or non-ionic type fluorocarbon surfactant one or more.
4. a kind of Nano silver conductive ink according to claim 1, it is characterized in that, described flow agent be selected from Bick BYK-300, Bick BYK-333, Bick BYK-310, Bick BYK-371, Bick BYK358, enlightening height Tego900, enlightening height Tego410, enlightening height Tego432 or enlightening height Tego450 one or more.
5. a kind of Nano silver conductive ink according to claim 1, it is characterized in that, described dispersion agent to be selected from enlightening height Dispers610, enlightening height Dispers610S, enlightening height Dispers655, enlightening height Dispers700, enlightening height Dispers710, enlightening height Dispers740W, enlightening height Dispers750W, enlightening height Dispers760W, enlightening height Dispers 750w or enlightening height Dispers 760w one or more.
6. a kind of Nano silver conductive ink according to claim 1, it is characterized in that, described organic solvent is selected from methyl alcohol, ethanol, Virahol, dimethyl formamide, ethylene glycol, propylene glycol, glycerol, propylene glycol monomethyl ether, propylene-glycol ethyl ether, propandiol butyl ether, dipropylene glycol methyl ether, dipropylene, dipropylene glycol hexyl ether, toluene, dimethylbenzene, ethyl acetate, propyl acetate, isopropyl acetate, methyl-formiate, ethyl formate, ethyl lactate, Valeric acid ethylester, acetone, methylethylketone, butanone, isophorone, diacetone alcohol, pimelinketone, nylon acid dimethyl ester, Terpineol 350, turps, diethylene glycol ether, acetic acid glycol ether monoethyl ether ester, or one or more in propylene glycol phenylate.
7. a kind of Nano silver conductive ink according to claim 1, it is characterized in that, described polymer binder be selected from cellulose acetate, soluble cotton, Vltra tears, cellulose acetate butyrate, epoxy resin, acrylate resin, vibrin, polyamide resin, polyimide resin, acrylate, fluorocarbon resin, Polyglycolic acid fibre or polyaniline one or more; Preferably, polymer binder is selected from one or more in acrylate resin, cellulose acetate, Polyglycolic acid fibre PEDOT or polyketone resin.
8. a kind of Nano silver conductive ink according to claim 1, it is characterized in that, described anti-settling agent to be selected from Mitsui chemical industry anti-settling auxiliary agent FDSS-5, Mitsui chemical industry anti-settling auxiliary agent FD380, organobentonite 881-A, organobentonite 881-B, organobentonite P-1, this ST auxiliary rheological agents of extra large name, polyimide wax MT 6650, polyimide wax BYK 420, polyimide wax BYK-425 or polyimide wax BYK-410 one or more; Preferably, anti-settling agent is selected from one or more in polyimide wax BYK 420, polyimide wax BYK-425, Mitsui chemical industry anti-settling auxiliary agent FD380 or Mitsui chemical industry anti-settling auxiliary agent FDSS-5.
9. a kind of Nano silver conductive ink according to claim 1, it is characterized in that, described solidifying agent is selected from Bayer Desmodur 3390BA/SN, Bayer Desmodur N3300, Bayer Bayhydur XP2451, Bayer Bayhydur 2570, Bayer Desmodur RC, Japan Asahi Chemical Industry NPU solidifying agent CORONATE HXR, Japan Asahi Chemical Industry NPU solidifying agent HX, Japan Asahi Chemical Industry NPU solidifying agent HK, Japan Asahi Chemical Industry NPU solidifying agent, Japan Asahi Chemical Industry NPU solidifying agent, Japan Asahi Chemical Industry CORONATE 2604, Japan Asahi Chemical Industry CORONATE MF-K60X, Japan Asahi Chemical Industry CORONATE MF-B60X, Degussa BI1358A, Japanese fuji Fujicure FXR1081, or one or more in Fujicure FXR 1020, preferably, solidifying agent is selected from one or more in Bayer Desmodur 3390BA/SN, Japanese Asahi Chemical Industry CORONATE MF-B60X or Degussa BI1358A.
10. the preparation method of a kind of Nano silver conductive ink according to claim 1, is characterized in that, comprise the steps:
(1) first 0.05 ~ 10 part of polymer binder is joined in organic solvent, be uniformly dissolved under dispersion machine dispersed with stirring and obtain cream liquid A;
(2) 0.05 ~ 2 part of nanometer silver is scattered in organic solvent, obtains homodisperse nano silver dispersion B;
(3) cream liquid A obtained above to be mixed with nano silver dispersion B and after stirring, add 0.001 ~ 5 part of solidifying agent, 0.001 ~ 2 part of dispersion agent, 0.001 ~ 2 part of surface modifier, 0.001 ~ 2 part of anti-settling agent, 0.001 ~ 2 part of flow agent and 0.01 ~ 2 part of nano assistant again, be dispersed to and mix, carry out grinding with three-roller and can obtain Nano silver conductive ink 3 ~ 10 times;
Described organic solvent total amount is 73 ~ 95 parts;
Consumption of organic solvent in described step (1) is the half of organic solvent total amount;
Consumption of organic solvent in described step (2) is remaining organic solvent.
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| CN104830158A (en) * | 2015-06-03 | 2015-08-12 | 苏州靖羽新材料有限公司 | Nano-silver electrically conductive printing ink and preparation method thereof |
| CN105086620A (en) * | 2015-10-08 | 2015-11-25 | 苏州市永津彩印包装有限公司 | High-performance durable printing ink |
| CN105400459A (en) * | 2015-12-23 | 2016-03-16 | 东莞市纳利光学材料有限公司 | Anti-electromagnetic wave high-viscosity adhesive for OCA optics films and preparation method thereof |
| CN105936769A (en) * | 2016-05-25 | 2016-09-14 | 青岛瑞利特新材料科技有限公司 | Graphene modified nano-silver aqueous conductive ink and preparation method thereof |
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| CN105086620A (en) * | 2015-10-08 | 2015-11-25 | 苏州市永津彩印包装有限公司 | High-performance durable printing ink |
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