CN105206350A - Preparing method for silver conductive thin film resisting water and oil - Google Patents

Preparing method for silver conductive thin film resisting water and oil Download PDF

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Publication number
CN105206350A
CN105206350A CN201510646940.2A CN201510646940A CN105206350A CN 105206350 A CN105206350 A CN 105206350A CN 201510646940 A CN201510646940 A CN 201510646940A CN 105206350 A CN105206350 A CN 105206350A
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substrate
minutes
preparation
silver
thin film
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CN105206350B (en
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阮海波
李璐
刘碧桃
周海霞
陈善勇
关有为
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Shanghai Juerxi Electronic Technology Co ltd
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Chongqing University of Arts and Sciences
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Abstract

The invention discloses a preparing method for a silver conductive thin film resisting water and oil. The preparing method comprises the steps that a substrate is cleaned, dried and treated in a plasma mode; the substrate is coated with a binding agent and dried; a binding layer is coated with silver nanometer wire conductive ink and dried to obtain a silver conductive network; the conductive network is coated with a polyfluoroacrylate protecting agent and dried to obtain the conductive thin film resisting the water and the oil. As the polyfluoroacrylate protecting agent resisting the water and the oil is used in the conductive thin film, the prepared conductive thin film has good water and oil resistance; meanwhile, the thin film has excellent electrical conductivity, light transparency and small fog scale, and is suitable for the field of electronic information.

Description

A kind of preparation method of silver-colored conductive film of Waterproofing/oilproofing
Technical field
The invention belongs to transparent conductive film technical field, be specifically related to a kind of preparation of silver-colored conductive film of Waterproofing/oilproofing.
Background technology
At current consumer electronic message area, what can be used as electrode material has Graphene, carbon nano-tube, metal oxide, nano metal line, conducting polymer etc.Wherein, the tin indium oxide (ITO) in metal oxide is electrode material the most frequently used at present.But the fragility of complexity prepared by the rareness of indium content, ito thin film and ITO itself makes it be not suitable for for building low cost flexible electrode.In above-mentioned material, nano silver wire is best with its electric conductivity, technology is the most ripe and become the flexible conducting material of current most possible breakthrough.When preparing silver-colored conductive film, people often cover one deck top stopping off to increase the protective of silver-colored conductive film on silver-colored conductive network.As patent CN104658700A, have employed the protection of UV glue; Patent CN102522145A, adopts the resin protections such as polyester, polyurethane, epoxy resin; Patent CN102522145B, adopts conducting polymer PEDOT:PSS protection; And other are as material protections such as optical cements.But these tops are coated with material a common drawback: only have certain repellence to the one in water or oil.This in water or organic solvent, has certain dissolubility because these tops are coated with material.This is disadvantageous for film application because water or organic solvent enter the sharply decline that can cause film performance and life-span.Therefore, the transparent conductive film of exploitation energy Waterproofing/oilproofing is needed.But it's a pity, this respect work is also considerably less.
Therefore, the high-performance silver conductive film developing Waterproofing/oilproofing is the problem that solution is needed in transparent conductive film field badly.
Summary of the invention
The object of the present invention is to provide a kind of preparation of silver-colored conductive film of Waterproofing/oilproofing, solve the problem that current thin film water-oil resistance is poor.This film have water-oil resistance can good, conductivity is high, light transmittance is high, with the advantage such as substrate associativity is good, preparation simply, can be widely used in electronic information field.Its specific embodiments is:
(1) substrate is carried out clean, dry and plasma treatment;
(2) on substrate, apply a layer binder, dry;
(3) nano silver wire conductive ink is coated on tack coat, after drying, obtains silver-colored conductive network;
(4) polyfluoroacrylate class protective agent is coated on conductive network, after oven dry, obtains a kind of silver-colored conductive film of Waterproofing/oilproofing.
The substrate that the present invention uses is the one in PETG (PET), dimethyl silicone polymer (PDMS), Merlon, polyimides (PI) or glass;
(1) in substrate cleaning, dry with plasma treatment process be: the diaphragm newly bought on substrate is torn off, puts it in acetone, ethanol and distinguish ultrasonic 5 minutes.Then substrate infrared baking lamp is toasted 5 minutes.Take out substrate, put it in plasma cleaner, vacuum cleaned 5 minutes.Wherein, the power of the infrared baking lamp of use is 800W, drying area is 1000cm2; Frequency/the power of the plasma cleaner used is 13.56MHz/300W;
With adhesive coated one deck tack coat of 5% concentration on the substrate that (1) processed, thickness is at about 300nm.Binding agent used is the mixing of one or more in epoxy resin, acrylate, acrylic resin, mylar, polyamide, polyurethane resin, polyimide resin, polyvinyl alcohol resin, polyketone resin, phenolic resins, silane coupler, titanate coupling agent.Coating uses GardcoAutomaticDrawdownMachineDP8301 sheet type coating machine, also comprises other coating machines.After having applied, first toast 5 minutes with infrared baking lamp, then in vacuum drying oven at 100 DEG C, vacuum dry 10 minutes;
(2) basis applies last layer nano silver wire coating fluid.Then, first 3 minutes are toasted with infrared baking lamp.Then to use at vacuum drying oven 110 DEG C vacuumize 10 minutes, obtain the nano silver wire network that thickness is about 200nm.Nano silver wire ink is homemade.Nano silver wire diameter is between 30-50nm, and length is between 10-20 μm.Ink silver line content is about 0.5%.Except silver-colored line, ink is also containing auxiliary agents such as dispersant, surfactant, levelling agent, NMF and binding agents;
Step (4) polyfluoroacrylate class protective agent used is the mixing of one or more in the fluoropropenes acid polymers such as poly-fluoro (trifluoromethyl) acrylate, (methyl) perfluoroalkyl acrylate polymer, (methyl) perfluoroethyl alkylamide ester polymer, (methyl) perfluoroethyl alkyl sulfonamide ester polymer.Due to dissolubility reason, apply the emulsion using polyfluoroacrylate class protective agent to make.Control coated weight, make final top coat thickness be 150nm;
After being applied by polyfluoroacrylate class protective agent, first toast 3 minutes with infrared baking lamp, then with baking under vacuum drying oven 100 DEG C of vacuum 10 minutes, obtain final Waterproofing/oilproofing silver conductive film;
The polyfluoroacrylate class protective agent that the present invention uses is the binding agent of a class hydrophobic and oil repellent, is coated on dargyrome network, can effectively anti-sealing and organic substance to the permeating corrosion of film, greatly extend film useful life;
The present invention has the following advantages: the protectant use of polyfluoroacrylate class of (1) hydrophobic and oil repellent makes film can allow water thereon and organic substance not stop erosion, remains the high-performance of film; (2) top is coated with and makes the adhesion of conductive film and substrate good with primary coat, and its defencive function makes membrane life time long; (2) filling between dargyrome network decreases the scattering of light, and thus product mist degree is low; (4) film conductivity and light transmittance high, have broad application prospects.
Accompanying drawing explanation
Fig. 1: structural representation of the present invention;
1-substrate; 2-tack coat; 3-silver conductive network; 4 polyfluoroacrylate class protective layers; Wherein, 3 and 4 layers overlap.
Specific embodiment
Embodiment:
Adopt PET as substrate.Diaphragm on new substrate is torn off, puts it in acetone, ethanol and distinguish ultrasonic 5 minutes.Then dry with infrared baking lamp.Then put it in plasma cleaner, vacuum cleaned 5 minutes;
With the polyacrylic resin of GardcoAutomaticDrawdownMachineDP8301 sheet type coating machine coating last layer 5% concentration on the substrate processed.Then, first toast 5 minutes with infrared baking lamp, then in vacuum drying oven at 100 DEG C, vacuum dry 10 minutes.Obtain the tack coat of a layer thickness in about 300nm left and right;
Tack coat applies one deck nano silver wire solution, first toasts 3 minutes with infrared baking lamp, then to use at vacuum drying oven 110 DEG C vacuumize 10 minutes, obtain the nano silver wire network of thickness at about 200nm;
(methyl) Perfluoroalkyl acrylate polymer emulsion is coated on silver-colored conductive network.First toast 3 minutes with infrared baking lamp, then with baking under vacuum drying oven 100 DEG C of vacuum 10 minutes, obtain the protective layer that 150nm is thick.Comprehensive above each step obtains final Waterproofing/oilproofing silver transparent conductive film.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just design according to the present invention can make many modifications and variations without the need to creative work.All technical staff in the art, all should by the determined protection range of claims under this invention's idea on the basis of existing technology by the available experiment of logical analysis, reasoning, or a limited experiment and technical scheme.

Claims (9)

1. a preparation method for the silver-colored conductive film of Waterproofing/oilproofing, is characterized in that, concrete preparation process is:
(1) substrate is carried out clean, dry and plasma treatment;
(2) on substrate, apply a layer binder, dry;
(3) nano silver wire conductive ink is coated on tack coat, after drying, obtains silver-colored conductive network;
(4) polyfluoroacrylate class protective agent is coated on conductive network, after oven dry, obtains a kind of conductive film of Waterproofing/oilproofing.
2. preparation method according to claim 1, is characterized in that: substrate is the one in PETG (PET), dimethyl silicone polymer (PDMS), Merlon, polyimides (PI) or glass.
3. preparation method according to claim 1, is characterized in that: in (1), the cleaning of substrate is torn off by the diaphragm on substrate, then substrate is put into acetone, ethanol ultrasonic 5 minutes respectively; Drying is toasted 5 minutes under the substrate after cleaning being placed on infrared baking lamp.
4. preparation method according to claim 1, is characterized in that: the plasma treatment process of step (1) is: by lying substrate in plasma processor, opens machine to substrate processing 5 minutes.
5. preparation method according to claim 1, is characterized in that: in step (2), binding agent used is the mixing of one or more in epoxy resin, acrylate, acrylic resin, mylar, polyamide, polyurethane resin, polyimide resin, polyvinyl alcohol resin, polyketone resin, phenolic resins, silane coupler, titanate coupling agent.
6. preparation method according to claim 1, is characterized in that: the oven dry of step (2) for first to toast 5 minutes with infrared baking lamp, then in vacuum drying oven at 100 DEG C, vacuum dry 10 minutes.
7. preparation method according to claim 1, is characterized in that: step (3) nano silver wire used is homemade, and diameter is between 30-50nm, and length is between 10-20 μm; Ink silver line content is about 0.5%; Except silver-colored line, ink is also containing dispersant, surfactant, levelling agent, NMF and binding agent etc.; After ink coating, first toast 3 minutes with infrared baking lamp; Then substrate is put into vacuum drying oven, heated baking 10 minutes at 110 DEG C, vacuum.
8. preparation method according to claim 1; it is characterized in that: step (4) polyfluoroacrylate class protective agent used is the mixing of one or more in the fluoropropenes acid polymers such as poly-fluoro (trifluoromethyl) acrylate, (methyl) perfluoroalkyl acrylate polymer, (methyl) perfluoroethyl alkylamide ester polymer, (methyl) perfluoroethyl alkyl sulfonamide ester polymer, uses its emulsion.
9. preparation method according to claim 1; it is characterized in that: step (4) is by after polyfluoroacrylate class protective agent lotion applicator; 3 minutes are first toasted with infrared baking lamp; then with baking under vacuum drying oven 100 DEG C of vacuum 10 minutes, final Waterproofing/oilproofing silver conductive film is obtained.
CN201510646940.2A 2015-10-09 2015-10-09 A kind of preparation method of the silver-colored conductive film of Waterproofing/oilproofing Active CN105206350B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105618787A (en) * 2016-01-27 2016-06-01 东莞理工学院 Preparation method of hydrophobic silver nanoparticles
CN106927693A (en) * 2017-01-19 2017-07-07 广东南海启明光大科技有限公司 A kind of nano-silver thread transparent conducting glass and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102093774A (en) * 2010-12-31 2011-06-15 清华大学 Conductive ink and preparation method thereof
CN102290506A (en) * 2011-09-20 2011-12-21 苏州晶能科技有限公司 Manufacturing technology of LED (Light Emitting Diode) module with graphical transparent thin-film electrode
CN102522145A (en) * 2011-12-02 2012-06-27 浙江科创新材料科技有限公司 Nanometer silver transparent electrode material and preparation method thereof
CN102867917A (en) * 2012-09-24 2013-01-09 中国乐凯胶片集团公司 Flexible film used for flexible organic solar battery
CN103198884A (en) * 2013-03-04 2013-07-10 中国科学院长春光学精密机械与物理研究所 Full-solution-processed multilayered-structure transparent conductive thin film and preparation method thereof
CN103903817A (en) * 2014-03-18 2014-07-02 中科院广州化学有限公司南雄材料生产基地 Preparing method and application of transparent conducting thin film
CN104658700A (en) * 2015-01-23 2015-05-27 华南师范大学 Preparation method for transparent silver nanowire conducting electrode

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102093774A (en) * 2010-12-31 2011-06-15 清华大学 Conductive ink and preparation method thereof
CN102290506A (en) * 2011-09-20 2011-12-21 苏州晶能科技有限公司 Manufacturing technology of LED (Light Emitting Diode) module with graphical transparent thin-film electrode
CN102522145A (en) * 2011-12-02 2012-06-27 浙江科创新材料科技有限公司 Nanometer silver transparent electrode material and preparation method thereof
CN102867917A (en) * 2012-09-24 2013-01-09 中国乐凯胶片集团公司 Flexible film used for flexible organic solar battery
CN103198884A (en) * 2013-03-04 2013-07-10 中国科学院长春光学精密机械与物理研究所 Full-solution-processed multilayered-structure transparent conductive thin film and preparation method thereof
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CN104658700A (en) * 2015-01-23 2015-05-27 华南师范大学 Preparation method for transparent silver nanowire conducting electrode

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105618787A (en) * 2016-01-27 2016-06-01 东莞理工学院 Preparation method of hydrophobic silver nanoparticles
CN106927693A (en) * 2017-01-19 2017-07-07 广东南海启明光大科技有限公司 A kind of nano-silver thread transparent conducting glass and preparation method thereof

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Effective date of registration: 20221207

Address after: Building C, No. 888, Huanhu West 2nd Road, Lingang New District, Pudong New Area pilot Free Trade Zone, Shanghai

Patentee after: Shanghai Juerxi Electronic Technology Co.,Ltd.

Address before: 402168 Chongqing Yongchuan District double bamboo town

Patentee before: CHONGQING University OF ARTS AND SCIENCES