CN105304164B - A kind of water base nano silver wire ink and its method for manufacturing thin film easily post-processed - Google Patents

A kind of water base nano silver wire ink and its method for manufacturing thin film easily post-processed Download PDF

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Publication number
CN105304164B
CN105304164B CN201510646270.4A CN201510646270A CN105304164B CN 105304164 B CN105304164 B CN 105304164B CN 201510646270 A CN201510646270 A CN 201510646270A CN 105304164 B CN105304164 B CN 105304164B
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ink
zonyl
film
small molecule
minutes
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CN105304164A (en
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杨鑫
陈善勇
刘碧桃
李璐
闫恒庆
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Chongqing University of Arts and Sciences
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Chongqing University of Arts and Sciences
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Abstract

The invention discloses a kind of water base nano silver wire ink easily post-processed and its film preparation, its ink composition is:Nano silver wire, 0.2 1.5%;Fluorocarbon surfactant, 0.005 0.05%;Small molecule dispersant, 0.1 2%;Small molecule levelling agent, 1 3%;Small molecule defoamer, 1 2%;Water, 91.45 97.695%.Its membrane-film preparation process is:A layer binder solution is coated on substrate, tack coat is obtained after drying;Then will(1)The ink of preparation is coated on tack coat, dries to obtain silver-colored conductive network;Finally coat layer protective layer, dry conductive film finally.Simple heat treatment is only needed to can obtain high performance nano silver wire film after ink coating.The superior performance of the film, can be widely used in the electronics fields such as touch-screen.

Description

A kind of water base nano silver wire ink and its method for manufacturing thin film easily post-processed
Technical field
The invention belongs to transparent conductive film field, and in particular to a kind of water base nano silver wire ink easily post-processed and its Film preparation.
Background technology
In a large amount of materials that flexible conducting substrate can be achieved, nano silver wire is fitted with its technology maturation, excellent performance, price In and as most possible commercialized material recently.And the utilization of nano silver wire is realized, first have to be prepared into adding The silver-colored conductive ink of work.According to the difference using solvent, these inks can be divided into organic group and water base two major class.Wherein, meeting The organic group ink of generation environment pollution accounts for the overwhelming majority, and the water-based ink of environmental protection is then few.To change this situation, people The exploitation dynamics of water-based ink is increased, has carried out some primary works.
United States Patent (USP) US8018568B2, US8632700B2, US8723216B2 and US8049333B2 hydroxypropyl methyl Cellulose, fluorocarbon surfactant and water have prepared water based silver ink.But the high decomposition temperature of hydroxypropyl methyl cellulose and water In slower dissolution velocity cause it to be difficult to remove in last handling process, thus this kind of film electric conductivity and translucency not It is good.To solve this problem, patent CN104064282A and CN103965674A use the water for soaking and removing easily by pure water The new water-based ink of based adhesive and resin formulations, has lifted ink performance.But auxiliary agent causes the painting of the ink very little Cover that performance is bad, and then cause the uneven of the Thin film conductive.To improve ink paintability, people add a variety of auxiliary agent exploitations The excellent ink of paintability, such as patent CN103996455A.But the auxiliary agent that these patents are used is macromolecule material substantially Material, it, which post-processes the difficult macromolecule residual brought, is greatly affected the electric conductivity and translucency of film.To sum up, letter at present Single processing can obtain high conductivity, uniformity, the conductive film of translucency water-based ink it is also seldom, performance is much met not Demand.
Therefore, exploitation simple process is that to can obtain the water-based ink of excellent conductive film be that transparent conductive film field is needed badly The problem of solution.
The content of the invention
It is an object of the invention to provide a kind of water base nano silver wire ink easily post-processed and its film preparation, mesh is solved Preceding water-based ink paintability is not good and coats the problem of rear film performance is not good.The silver wire ink coating that the present invention is developed Can good, post processing it is simple, the electric conductivity for the film being made, light transmittance are high and uniform, can largely be used in electronic information field.This Invention is characterised by:
(1) the ink specific formula is as follows:
Nano silver wire, 0.2-1.5%;
Fluorocarbon surfactant, 0.005-0.05%;
Small molecule dispersant, 0.1-2%;
Small molecule levelling agent, 1-3%;
Small molecule defoamer, 1-2%;
Water, 91.45-97.695%.
(2) preparation process of film is:A layer binder solution is coated on substrate, tack coat is obtained after drying.Then The ink that (1) is prepared is coated on tack coat, dries to obtain silver-colored conductive network.Layer protective layer is finally coated, it is finally dry Conductive film;
A diameter of 30-50nm of nano silver wire used of the invention, length is at 10-20 μm;
(1) surfactant used is Zonyl@FSO, Zonyl@FSP, Zonyl@FSA, Zonyl@8867L, Zonyl@in The series fluorine carbon such as 8857A, Zonyl@FSN, Zonyl@FS, Zonyl@FSK, Zonyl@FSD, Zonyl@TBS, Capstone@FS One or more of mixing in surfactant;
(1) small molecule dispersant used is the high boiling liquids such as monoethanolamine, -2 methyl isophthalic acids of 2- amino-propyl alcohol in;
(1) in small molecule levelling agent used be butyl cellosolve, isopropoxide ethanol, propylene glycol monomethyl ether, isophorone, One or more of mixing in the high boiling solvents such as DAA, DBE;
Small molecule levelling agent used of the invention is butyl cellosolve, isopropoxide ethanol, propylene glycol monomethyl ether, different Fo Er One or more of mixing in the high boiling solvents such as ketone, DAA, DBE;
(1) small molecule defoamer used is 2- hexyl ethanol in;
(1) preparation steps of ink inside are:Determine that ink set is constituted, calculate the quality needed for every kind of material.Then claim Take all substances to be added in a flask, stir 30 minutes.Finally, by membrane filtration of the slurry with 20 μm of apertures, obtain final Ink;
(2) substrate used is polyethylene terephthalate (PET), dimethyl silicone polymer (PDMS), poly- carbonic acid in One kind in ester, polyimides (PI) or glass;
(2) binding agent used is epoxy resin, acrylate, acrylic resin, polyester resin, polyamide resin in Fat, polyurethane resin, polyimide resin, polyvinyl alcohol resin, polyketone resin, phenolic resin, silane coupler, titanate esters are even Join one or more of mixing in agent.Coated with Gardco Automatic Drawdown Machine DP8301 sheet types After machine or other coating machines coated with adhesive solution, toasted 5 minutes with infrared baking lamp, then 100 DEG C in vacuum drying oven Lower vacuum drying 5 minutes, obtains tack coat.Infrared baking lamp used is that the power of the infrared baking lamp used is 800W, drying Area is 1000cm2
(2) coat after ink, toasted 5 minutes with infrared baking lamp, then 110 DEG C in vacuum drying oven on tack coat in Lower vacuum drying 10 minutes, removes solvent and other auxiliary materials, obtains silver-colored conductive network;
(2) top coat protective layer used is UV glue, some common resins, PEDOT in:PSS, graphene, CNT, metal One or more in the materials such as oxide, optical cement, PUR.The concentration and amount of top coat are controlled, makes top coat after coating Thickness is less than the thickness of silver-colored conductive network.Then top coat is toasted 5 minutes with infrared baking lamp, then 110 in vacuum drying oven It is dried in vacuo 10 minutes at DEG C.If using UV glue, solidified with ultraviolet curing lamp.So obtain final conductive film;
The reason for ink convenient post-treatment of the present invention is that the auxiliary agent that ink is used is essentially easily heat organic small Molecule.Under 110 DEG C of vacuum, these organic molecules are changed into steam and left from silver-colored conductive network.And the fluorine carbon table only remained The content of face activating agent is very low, and the performance impact to nano silver wire conductive network is smaller.
The present invention has the following advantages:(1) contain the auxiliary agent of a variety of not same-actions in ink, ink performance can be allocated to each The physical parameter needed for substrate coating is planted, therefore, the coating effect of ink of the present invention on various substrates is fine;(2) silver wire is removed Outer most auxiliary agents are easy to remove by heating, and heating in vacuum avoids the oxidation of silver wire, thus the film prepared Electric conductivity and light transmittance are fine;(3) primary coat and top coat ensure that silver nanoparticle network and substrate have good adhesion, while slowing down ring Erosion of the border to silver wire, thus the conductive film can use persistently;(4) top coat filling reduces the unfavorable factors such as light scattering, because And the mist degree of the film is smaller;(5) ink and the raw material of film are cheap, and film-forming process is simple, is not required to complex instrument, thus film Cost is low, facilitates use of large-scale production.
Brief description of the drawings
Fig. 1:The silver wire network formed after ink coating of the present invention.
Specific embodiment
Embodiment:
Using a diameter of 30-50nm, length 10-20 μm nano silver wire be conductive materials.From Zonyl@FSO-100 It is that scattered anti-settling agent, propylene glycol monomethyl ether are that levelling agent, 2- hexyl ethanol are for surfactant, -2 methyl isophthalic acids of 2- amino-propyl alcohol Defoamer, water are solvent to prepare slurry;
Determine that ink set is constituted, calculate the quality needed for every kind of material.Then all substances are weighed and are added to a flask In, stir 30 minutes.Finally, by membrane filtration of the slurry with 20 μm of apertures, final ink is obtained;
It is substrate from PET, acrylic resin is binding agent.With Gardco Automatic Drawdown Machine Acrylic resin soln is coated in PET film by DP8301 sheet type coating machines.Then toasted 5 minutes with infrared baking lamp, Then it is dried in vacuo 5 minutes at 100 DEG C in vacuum drying oven, obtains tack coat;Ink is coated on tack coat with coating machine, Then toasted 5 minutes, be then dried in vacuo 10 minutes at 110 DEG C in vacuum drying oven with infrared baking lamp, remove solvent and its His auxiliary material, obtains silver-colored conductive network;
Top coat uses PEDOT:PSS solution.It is coated onto on silver nanoparticle network.Usage amount is controlled, makes final protective layer Thickness be less than silver nanoparticle network thickness.After the completion of coating, toasted 5 minutes with infrared baking lamp, then in vacuum drying oven Vacuum drying obtains final conductive film in 10 minutes at 110 DEG C.
Presently preferred embodiments of the present invention described in detail above.It should be appreciated that one of ordinary skill in the art is without wound The property made work just can make many modifications and variations according to the design of the present invention.All technical staff Yi Benfa in the art Bright design passes through the available experiment of logical analysis, reasoning, or a limited experiment and technology on the basis of existing technology Scheme, all should be in the protection domain being defined in the patent claims.

Claims (1)

1. a kind of water base nano silver wire ink and its method for manufacturing thin film easily post-processed, it is characterised in that
(1)Ink set is:
A diameter of 30-50 nm, nano silver wire 0.2-1.5% of the length at 10-20 μm;
Fluorocarbon surfactant 0.005-0.05%, the surfactant be Zonyl@FSO, Zonyl@FSP, Zonyl@FSA, Zonyl@8867L、Zonyl@8857A、Zonyl@ FSN、Zonyl@FS、Zonyl@ FSK、Zonyl@ FSD、Zonyl@ TBS、 One or more of mixing in Capstone@FS series fluorocarbon surfactants;
Small molecule dispersant 0.1-2%, the small molecule dispersant is monoethanolamine, -2 methyl isophthalic acids of 2- amino-propyl alcohol higher boiling liquid Body;
Small molecule levelling agent 1-3%, small molecule levelling agent used be butyl cellosolve, isopropoxide ethanol, propylene glycol monomethyl ether, One or more of mixing in isophorone, DAA, DBE high boiling solvents;
Small molecule defoamer 2- hexyl ethanol 1-2%;
Water, 91.45-97.695%;
Weigh all substances to be added in a flask, stir 30 minutes, finally, membrane filtration of the slurry with 20 μm of apertures is obtained To final ink;
(2)The preparation process of film is:A layer binder solution is coated on substrate, after binder solution coating, infrared baking is used Heat lamp is toasted 5 minutes, is then dried in vacuo 5 minutes at 100 DEG C in vacuum drying oven, obtains being bonded after tack coat is dried Layer;Then will(1)The ink of preparation is coated on tack coat, after being toasted 5 minutes with infrared baking lamp after ink coating, in vacuum It is dried in vacuo 10 minutes at 110 DEG C in baking oven, obtains silver-colored conductive network and dry to obtain silver-colored conductive network;One layer of top coat is finally coated to protect Sheath, after the coating of top coat protective layer, is toasted 5 minutes with infrared baking lamp, is then dried in vacuo 10 at 110 DEG C in vacuum drying oven Minute, obtain final conductive film;Substrate used is polyethylene terephthalate (PET), dimethyl silicone polymer (PDMS), one kind in makrolon, polyimides (PI) or glass;Binding agent used be epoxy resin, acrylate, Acrylic resin, polyester resin, polyamide, polyurethane resin, polyimide resin, polyvinyl alcohol resin, polyketone resin, One or more of mixing in phenolic resin, silane coupler, titanate coupling agent;Top coat Protective substances used be UV glue, Some common resins, PEDOT:One kind in the materials such as PSS, graphene, CNT, metal oxide, optical cement, PUR Or it is several.
CN201510646270.4A 2015-10-09 2015-10-09 A kind of water base nano silver wire ink and its method for manufacturing thin film easily post-processed Active CN105304164B (en)

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CN106229036B (en) * 2016-07-26 2017-09-29 珠海纳金科技有限公司 A kind of transparent conductive film and preparation method thereof
CN106847512A (en) * 2016-12-27 2017-06-13 江汉大学 Conductive film and used by dye sensitization solar battery polyaniline/metal nanometer line combined counter electrode
CN108250469B (en) * 2016-12-29 2021-04-30 乐凯华光印刷科技有限公司 Production process of nano silver wire transparent conductive film
CN106502020B (en) * 2017-01-13 2019-06-21 合肥微晶材料科技有限公司 A kind of controllable conductivity light modulation structure and preparation method thereof
CN108231246B (en) * 2018-03-01 2020-01-03 合肥微晶材料科技有限公司 Ultraviolet-resistant nano silver wire conductive film and manufacturing method thereof
CN108519703A (en) * 2018-04-17 2018-09-11 苏州顾氏新材料有限公司 A kind of flexible single substrate nano silver wire electrode liquid crystal light modulation film and preparation method thereof
CN108995103A (en) * 2018-08-20 2018-12-14 中国科学院工程热物理研究所 Low radiation film and preparation method thereof
CN110070965A (en) * 2019-03-26 2019-07-30 天津大学 A kind of multi-layer-structure transparent conductive film and preparation method thereof
CN111847898A (en) * 2020-07-28 2020-10-30 虞晖 High-infrared-reflection coated glass and preparation process thereof

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JP2010113912A (en) * 2008-11-05 2010-05-20 Sumitomo Rubber Ind Ltd High-temperature calcination type silver paste, and electromagnetic wave shield using the same
CN103160165B (en) * 2013-03-01 2015-07-15 溧阳市新力机械铸造有限公司 Photo-hardening nanometer silver-copper alloy conductive ink
CN103198884B (en) * 2013-03-04 2016-03-02 中国科学院长春光学精密机械与物理研究所 Full-solution-procesmultilayered-structutransparent multilayered-structutransparent transparent conductive thin film and preparation method thereof
CN103627255B (en) * 2013-05-06 2015-05-20 苏州冷石纳米材料科技有限公司 Nano-silver conductive ink and conductive film prepared by employing same

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