CN105118546A - Novel transparent silver nanowire conductive film with oxide protection - Google Patents
Novel transparent silver nanowire conductive film with oxide protection Download PDFInfo
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- CN105118546A CN105118546A CN201510648860.0A CN201510648860A CN105118546A CN 105118546 A CN105118546 A CN 105118546A CN 201510648860 A CN201510648860 A CN 201510648860A CN 105118546 A CN105118546 A CN 105118546A
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Abstract
The invention discloses a novel transparent silver nanowire conductive film with oxide protection and a preparation method of the novel transparent silver nanowire conductive film. The preparation method comprises the following steps: a substrate is cleaned and subjected to plasma treatment; the substrate is coated with a binder and dried by an infrared lamp; the substrate is coated with silver nanowire conductive ink and dried, and a silver conductive network is obtained; the silver conductive network is coated with a conductive oxide solution and dried, and the silver nanowire conductive film is obtained. The transparent silver nanowire conductive film has good bonding performance with the substrate, high conductivity and high light transmittance and can be applied to various aspects of the electronic information industry.
Description
Technical field
The invention belongs to transparent conductive film technical field, be specifically related to nano silver wire transparent conductive film and preparation method thereof.
Background technology
ITO (IndiumTinOxide) is widely used in the fields such as flat panel display, illumination and solar cell because of reasons such as its conduction light transmission are high.But there is following major defect in ITO: (1) natural indium content is few, so its output is restricted, price is also higher; (2) ito thin film is many is obtained by vacuum sputtering, and its equipment requirement is high, and high temperature sputtering also easily hurts substrate; (3) ITO fragility is comparatively large, and bending is easily broken, and causes it not to be suitable in flexible device.So along with wearable device market expanding day, people start to develop gradually can the transparent conductive film of flexible bending, as the transparent conductive film based on materials such as Graphene, carbon nano-tube, nano metal lines.Relative to Graphene and carbon nano-tube, nano metal line is the transparent conductive material of most possible breakthrough recently.Nano metal line comprises the metal such as gold, silver, copper.Wherein, silver-colored line, oxidation resistance best with its conductivity better and moderate and become the emphasis of people's research.In former nano silver wire conductive film preparation, people generally have employed following preparation process: (1) applies a layer binder on substrate, and infrared lamp is dried; (2) nano silver wire conductive ink is coated on substrate, after drying, obtains silver-colored conductive network; (3) top painting is coated on silver-colored conductive network, after drying, obtains nano silver wire conductive film.First two steps difference is less, and the top that the 3rd step adopts is coated with and then distinguishes to some extent.As patent CN104658700A, UV glue is adopted to be coated with as top; Patent CN103903817A, adopts graphene solution to be coated with as top; Patent CN102522145A, adopts the resins such as polyester, polyurethane, epoxy resin to be coated with as top; Patent CN102522145B, adopts conducting polymer PEDOT:PSS solution to be coated with as top; And other are as top painting materials such as optical cements.But UV glue, polyester, polyurethane, epoxy resin, optical cement etc. are as macromolecular material, it adds inherently can hinder the contact between silver-colored line thus the conductivity reducing film, also can reduce the light transmission of film simultaneously.And Graphene cost is higher, the price of the conductive film prepared with it is higher.The acidity of PEDOT:PSS can corrode silver-colored line, is unfavorable for permanent use.The silver-colored conductive film that these factors make these patents prepare above effectively can not embody the excellent properties of nano silver wire.
Therefore, selecting what top to be coated with material is the problem that photoelectric field needs solution badly with the close-burning high conductivity of silver nanoparticle conductive film and the high transmission rate of keeping of the excellence realizing nano silver wire conductive film and substrate simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of new top applying soln and membrane-film preparation process, thus solve top at present and be coated with the variety of problems that material exists.This film have conduction light transmission high, with the advantage such as substrate associativity is good, can prepare by large-scale low-cost, thus can be used for a lot of aspects of electronic information industry.Its specific embodiments is:
(1) substrate that the present invention uses is the one in PETG (PET), dimethyl silicone polymer (PDMS), Merlon, polyimides (PI) or glass.Diaphragm on the substrate newly bought is torn off, to put it in ethanol ultrasonic 10 minutes.Then film is put into vacuum drying oven 50 DEG C of vacuumizes 10 minutes.Take out substrate, put it in plasma cleaner, vacuum cleaned 5 minutes.Wherein, the frequency/power of the plasma cleaner of use is 13.56MHz/300W;
(2) with adhesive coated one deck tack coat of 5% concentration on the substrate processed in (1), thickness is at about 300nm.Binding agent comprises 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, toast 5 minutes with infrared baking lamp.The power of the infrared baking lamp used is 800W, drying area is 1000cm
2;
(3) on (2) basis, apply one deck nano silver wire coating fluid, 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;
(4) on (3) basis, one deck conductive oxide solution is applied.Then substrate is put into vacuum drying oven, 110 DEG C of heated bakings 10 minutes, conductive oxide thickness is 150nm.The oxide used comprises zinc oxide, molybdenum oxide, vanadium oxide etc., and its solution is homemade.Burnett's solution is that the presoma decomposing zinc obtains.The solution hydrogen peroxide such as the molybdenum oxide of Lacking oxygen, vanadium oxide and the metal normal temperature such as molybdenum, vanadium stirring reaction is had to obtain.By above these, obtain final Novel silver nano wire conductive film.
The present invention has the following advantages: the macromolecules such as the resin that (1) replaces some common with conductive oxide, optical cement, make the film of preparation at the close-burning high conductivity of nano silver wire network and the light transmittance of maintaining of the excellence realizing nano silver wire conductive network and substrate simultaneously; (2) avoid PEDOT:PSS etc. has corrosiveness material to nano silver wire, this network is not corroded while being coated in protection silver nanoparticle network in new top, makes silver-colored conductive film durable in use; (3) filling of conductive materials improves the conductivity of silver nanoparticle network, reduces the scattering of light and reduces mist degree, and thus product mist degree is low; (4) wet process film, step is simple, does not need the complex steps needed for ITO masking and equipment, low price, has a good application prospect.
Accompanying drawing explanation
Fig. 1: structural representation of the present invention;
1-substrate; 2-primary coat tack coat; 3-silver conductive network; 4-oxide electroconductive film; Wherein, 3 and 4 layers overlap.
Specific embodiment
Embodiment:
Employing PET is substrate.Diaphragm on substrate is torn off, puts into ethanol ultrasonic 10 minutes.Then by its vacuumize 10 minutes (50 DEG C) in vacuum drying oven.Take out substrate, put it in plasma cleaner, vacuum cleaned 5 minutes;
The substrate processed applies with GardcoAutomaticDrawdownMachineDP8301 sheet type coating machine the acrylic resin of one deck 5% concentration.Then, toast 5 minutes with infrared baking lamp, obtain the tack coat of thickness in about 300nm left and right;
Tack coat applies one deck nano silver wire solution, and then vacuumize 10 minutes at vacuum drying oven 110 DEG C, obtains 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;
After the hydrochloric acid solution that molybdenum powder concentration is extremely low is washed 5 minutes, desalt acid solution.Suction filtration, wash three times, ethanol washes three times.Then vacuumize 10 minutes.The molybdenum powder processed is added in a bottle with two necks, under nitrogen, in bottle, add a certain amount of ethanol, stir 10 minutes.Then, the hydrogen peroxide of 30% concentration is slowly added wherein.Stir after 18 hours, with Rotary Evaporators except desolventizing, obtain oxide powder.According to desired concn, it is deployed stand-by to add ethanol;
Nano silver wire network applies the molybdenum oxide solution that one deck has Lacking oxygen.Then substrate is put into vacuum drying oven, toast 10 minutes at 110 DEG C, Electrochromic Molybdenum Oxide Coatings thickness is at about 150nm.Finally obtain novel 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 (7)
1. a nano silver wire transparent conductive film for new oxide protection, it is characterized in that, concrete preparation process is:
(1) substrate cleaned and carry out plasma treatment;
(2) on substrate, apply a layer binder, infrared lamp is dried;
(3) nano silver wire conductive ink is coated on substrate, after drying, obtains silver-colored conductive network;
(4) conductive oxide solution is coated on silver-colored conductive network, after drying, obtains nano silver wire conductive film.
2. nano silver wire transparent conductive film 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. nano silver wire transparent conductive film 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; Its cleaning process is for carry out ultrasonic cleaning with ethanol.
4. nano silver wire transparent conductive film according to claim 1, is characterized in that: the binding agent in step (2) 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.
5. nano silver wire transparent conductive film according to claim 1, is characterized in that: the infrared lamp Dryly use of step (2) be the infrared baking lamp of 500W, dry about 5 minutes.
6. nano silver wire transparent conductive film 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, substrate is put into vacuum drying oven, 110 DEG C of heated bakings 10 minutes.
7. nano silver wire transparent conductive film according to claim 1, it is characterized in that: the conductive oxide that step (4) uses is homemade, to be decomposed by presoma or the mode such as metal and hydrogen peroxide reaction obtains, comprise the solution such as zinc oxide, molybdenum trioxide, vanadic oxide; After the coating of conductive oxide solution, substrate is put into vacuum drying oven, and 110 DEG C of heated bakings obtain final nano silver wire transparent conductive film for 10 minutes.
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| CN106098134A (en) * | 2016-07-04 | 2016-11-09 | 陕西煤业化工技术研究院有限责任公司 | A kind of nano silver wire transparent conductive film and preparation method |
| CN106739597A (en) * | 2016-12-31 | 2017-05-31 | 武汉理工大学 | A kind of all print multifunctional transparent film and preparation method thereof |
| CN108668517A (en) * | 2017-04-01 | 2018-10-16 | 中国科学院化学研究所 | Electromagnetic shielding film and preparation method thereof |
| CN112349449A (en) * | 2020-10-30 | 2021-02-09 | 中国建筑材料科学研究总院有限公司 | Transparent conductive coating and preparation method and application thereof |
| CN113152754A (en) * | 2021-05-31 | 2021-07-23 | 天津包钢稀土研究院有限责任公司 | Heat preservation type heating doubling glass curtain wall |
| CN113963844A (en) * | 2021-10-12 | 2022-01-21 | 浙江大学 | Flexible silver nanowire-based composite transparent film heater and preparation method thereof |
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| CN108668517A (en) * | 2017-04-01 | 2018-10-16 | 中国科学院化学研究所 | Electromagnetic shielding film and preparation method thereof |
| CN112349449A (en) * | 2020-10-30 | 2021-02-09 | 中国建筑材料科学研究总院有限公司 | Transparent conductive coating and preparation method and application thereof |
| CN112349449B (en) * | 2020-10-30 | 2022-04-08 | 中国建筑材料科学研究总院有限公司 | Transparent conductive coating and preparation method and application thereof |
| CN113152754A (en) * | 2021-05-31 | 2021-07-23 | 天津包钢稀土研究院有限责任公司 | Heat preservation type heating doubling glass curtain wall |
| CN113963844A (en) * | 2021-10-12 | 2022-01-21 | 浙江大学 | Flexible silver nanowire-based composite transparent film heater and preparation method thereof |
| CN113963844B (en) * | 2021-10-12 | 2022-08-23 | 浙江大学 | Flexible silver nanowire-based composite transparent film heater and preparation method thereof |
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Effective date of registration: 20221201 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 |