CN105161220A - Preparation method of high-temperature-resistant silver conductive film - Google Patents

Preparation method of high-temperature-resistant silver conductive film Download PDF

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Publication number
CN105161220A
CN105161220A CN201510646221.0A CN201510646221A CN105161220A CN 105161220 A CN105161220 A CN 105161220A CN 201510646221 A CN201510646221 A CN 201510646221A CN 105161220 A CN105161220 A CN 105161220A
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substrate
preparation
binding agent
minutes
conductive film
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CN201510646221.0A
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CN105161220B (en
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程江
陈善勇
李璐
刘碧桃
金容�
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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 preparation method of a high-temperature-resistant silver conductive film. The preparation method comprises: carrying out cleaning, drying and plasma processing on a substrate; coating a heterocyclic-ring high-molecular binder on the substrate and carrying out drying; coating silver-nanowire conductive ink on a bonding layer and carrying out drying to obtain a silver conductive network; ad coating the heterocyclic-ring high-molecular binder on the conductive network and carrying out drying to obtain a novel conductive film. According to the conductive film, with the novel heterocyclic-ring high-molecular binder, performances including the high-temperature resistance, conductivity, light transmittance, and haze degree are optimized; and thus the conductive film is suitable for an electronic information field.

Description

A kind of preparation method of high temperature resistant silver-colored conductive film
Technical field
The invention belongs to transparent conductive film technical field, be specifically related to a kind of preparation of high temperature resistant silver-colored conductive film.
Background technology
Nano silver wire conductive film relies on the electrical and thermal conductivity, light transmission etc. of its excellence and becomes the desirable conductive film of the electronic information field such as touch-screen, display.At present, the conventional preparation process of nano silver wire conductive film is: (1) applies one deck primary coat binding agent on substrate, dries; (2) nano silver wire conductive ink is coated on substrate, after drying, obtains silver-colored conductive network; (3) top stopping off is coated on silver-colored conductive network, after drying, obtains nano silver wire conductive film.Conventional primary coat binding agent has the materials such as epoxy resin, acrylate, acrylic resin, mylar, polyamide, polyurethane resin, polyimide resin, polyvinyl alcohol resin, polyketone resin, phenolic resins, silane coupler, titanate coupling agent.Push up stopping off then varied, as patent CN104658700A, CN102522145A, CN102522145B adopt UV glue, resin (polyester, polyurethane, epoxy resin etc.), conducting polymer PEDOT:PSS solution to be coated with material as top respectively.
But these primary coats and top are coated with material a common drawback: resistance to elevated temperatures is bad.When ambient temperature is higher, these materials may melt or be out of shape, thus conductive film performance is sharply declined.So, be not suitable for using in the environment that some temperature are higher with silver-colored conductive film prepared by these materials, then cause the blank of high temperature resistant silver-colored conductive film.But the environment that some temperature are higher needs again can resistant to elevated temperatures conductive film.
Therefore, exploitation can resistant to elevated temperatures silver-colored transparent conductive film be 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 high temperature resistant silver-colored conductive film, solve the problem of current thin film resin non-refractory used.This film has that resistance to elevated temperatures is 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 one deck heterocyclic polymer binding agent, dry;
(3) nano silver wire conductive ink is coated on tack coat, after drying, obtains silver-colored conductive network;
(4) by heterocyclic polymer adhesive coated on conductive network, obtain a kind of resistant to elevated temperatures silver-colored conductive film after oven dry.
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 1000cm 2; Frequency/the power of the plasma cleaner used is 13.56MHz/300W;
With heterocyclic polymer adhesive coated one deck tack coat of 5% concentration on the substrate that (1) processed, thickness is at about 300nm.Heterocyclic polymer binding agent used is the mixing of one or more in the high temperature resistant binders such as polybenzimidazoles adhesive (polybenzimidazoles pyrrolidones), poly-oxazoline binding agent, polyarylsulfone (PAS) binding agent, poly-time diphenyl sulfide binding 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 150 DEG C, vacuum dry 10 minutes;
(2) basis applies one deck 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) heterocyclic polymer binding agent used is the mixing of one or more in the high temperature resistant binders such as polybenzimidazoles adhesive (polybenzimidazoles pyrrolidones), poly-oxazoline binding agent, polyarylsulfone (PAS) binding agent, poly-time diphenyl sulfide binding agent.Control the amount of coating, make final top coat thickness be about 150nm;
After heterocyclic polymer adhesive coated, first toast 3 minutes with infrared baking lamp, then with baking under vacuum drying oven 150 DEG C of vacuum 10 minutes, obtain final high temperature resistant silver-colored conductive film;
The binding agent that the present invention uses is some special high temperature-resistant binding agents, the problem conventional binding agent being avoided to melt when temperature is higher or be out of shape with them.Thus, can use in the environment of some higher temperatures with the film that they are prepared;
The present invention has the following advantages: the silver-colored transparent conductive film that the use of (1) high temperature resistant binder makes us prepare has excellent resistance to elevated temperatures, can be used for some special occasions and high-end electronic product; (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; (3) filling between dargyrome network decreases the scattering of light, and thus product mist degree is low; (4) film conductivity and light transmittance good, have broad application prospects.
Accompanying drawing explanation
Fig. 1: structural representation of the present invention;
1-substrate; 2-high temperature resistant bonding layer; 3-silver conductive network; 4-high temperature resistant bonding layer; 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 polybenzimidazole adhesive 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 150 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.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 a small amount of dispersant, surfactant, levelling agent, NMF and binding agents;
Polybenzimidazole adhesive solution is coated on silver-colored conductive network.First toast 3 minutes with infrared baking lamp, then with baking under vacuum drying oven 150 DEG C of vacuum 10 minutes, obtain the protective layer that 150nm is thick.Comprehensive above each step obtains final high temperature resistant silver-colored 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 high temperature resistant silver-colored conductive film, is characterized in that, concrete preparation process is:
(1) substrate is carried out clean, dry and plasma treatment;
(2) on substrate, apply one deck heterocyclic polymer binding agent, dry;
(3) nano silver wire conductive ink is coated on tack coat, after drying, obtains silver-colored conductive network;
(4) by heterocyclic polymer adhesive coated on conductive network, obtain a kind of resistant to elevated temperatures conductive film after oven dry.
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: the heterocyclic polymer binding agent in step (2) is the mixing of one or more in the high temperature resistant binders such as polybenzimidazoles adhesive (polybenzimidazoles pyrrolidones), poly-oxazoline binding agent, polyarylsulfone (PAS) binding agent, poly-time diphenyl sulfide binding 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 150 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%, and 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, is characterized in that: it is the mixing of one or more in the high temperature resistant binders such as polybenzimidazoles adhesive (polybenzimidazoles pyrrolidones), poly-oxazoline binding agent, polyarylsulfone (PAS) binding agent, poly-time diphenyl sulfide binding agent that step (4) top used is coated with heterocyclic polymer binding agent.
9. preparation method according to claim 1, it is characterized in that: after top is coated with heterocyclic polymer adhesive coated by step (4), first toast 3 minutes with infrared baking lamp, then with baking under vacuum drying oven 150 DEG C of vacuum 10 minutes, obtain final high temperature resistant silver-colored conductive film.
CN201510646221.0A 2015-10-09 2015-10-09 A kind of preparation method of the silver-colored conductive film of high temperature resistant Active CN105161220B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105895196A (en) * 2016-04-07 2016-08-24 江苏三月光电科技有限公司 Novel transparent conductive thin film and preparation method thereof
CN110942843A (en) * 2019-10-23 2020-03-31 清远高新华园科技协同创新研究院有限公司 Polymer conductive film for electric automobile, production equipment and preparation method

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CN101186128A (en) * 2007-10-29 2008-05-28 福建师范大学 High temperature resistant high photics reflexive conductive film and preparation method thereof
CN101239518A (en) * 2007-12-26 2008-08-13 苏州纳米技术与纳米仿生研究所 Composite coating material and preparation thereof
US20090104440A1 (en) * 2007-10-22 2009-04-23 Nitto Denko Corporation Transparent conductive film, method for production thereof and touch panel therewith
CN101697288A (en) * 2009-10-13 2010-04-21 福建师范大学 Transparent conductive film of metal silver/metal oxide and preparation method thereof
CN101709029A (en) * 2009-11-16 2010-05-19 清华大学 Polybenzimidazole material and midbody organic diacid thereof as well as preparation methods 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
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

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090104440A1 (en) * 2007-10-22 2009-04-23 Nitto Denko Corporation Transparent conductive film, method for production thereof and touch panel therewith
CN101186128A (en) * 2007-10-29 2008-05-28 福建师范大学 High temperature resistant high photics reflexive conductive film and preparation method thereof
CN101239518A (en) * 2007-12-26 2008-08-13 苏州纳米技术与纳米仿生研究所 Composite coating material and preparation thereof
CN101697288A (en) * 2009-10-13 2010-04-21 福建师范大学 Transparent conductive film of metal silver/metal oxide and preparation method thereof
CN101709029A (en) * 2009-11-16 2010-05-19 清华大学 Polybenzimidazole material and midbody organic diacid thereof as well as preparation methods 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
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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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105895196A (en) * 2016-04-07 2016-08-24 江苏三月光电科技有限公司 Novel transparent conductive thin film and preparation method thereof
CN110942843A (en) * 2019-10-23 2020-03-31 清远高新华园科技协同创新研究院有限公司 Polymer conductive film for electric automobile, production equipment and preparation method

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Address after: 200100 Building C, No. 888, Huanhu West Second Road, Lingang New Area, Pudong New Area Free Trade Pilot Zone, Shanghai

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