KR20160037298A - Silver nanowire using reduction for ultraviolet irradating, preparing method of the same and transparent conductive film including the same - Google Patents
Silver nanowire using reduction for ultraviolet irradating, preparing method of the same and transparent conductive film including the same Download PDFInfo
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- KR20160037298A KR20160037298A KR1020140129088A KR20140129088A KR20160037298A KR 20160037298 A KR20160037298 A KR 20160037298A KR 1020140129088 A KR1020140129088 A KR 1020140129088A KR 20140129088 A KR20140129088 A KR 20140129088A KR 20160037298 A KR20160037298 A KR 20160037298A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
Abstract
The present invention relates to a silver nanowire, a method of manufacturing the same, and a transparent conductive film comprising the silver nanowire. More particularly, the present invention relates to a silver nanowire using a silver- And a transparent conductive film comprising the silver nanowire thus produced.
Description
The present invention relates to a silver nanowire, a method of manufacturing the same, and a transparent conductive film comprising the silver nanowire. More particularly, the present invention relates to a silver nanowire using a silver- And a transparent conductive film comprising the silver nanowire thus produced.
In general, ITO (Indium Tin Oxide) refers to ITO having improved conductivity by adding tin oxide (SnO 2 ) to conductive indium oxide (In 2 O 3 ). ITO is used as a sputtering target A transparent electrode film can be obtained by sputtering on a glass plate by processing and a transparent electrode film can be obtained by dissolving ITO and spraying on a glass plate or immersing a glass plate in a solution.
Here, when ITO is coated on a film such as polyethylene, a transparent conductive film can be produced. Such a transparent conductive film is applied to a light emitting surface electrode of a display EL panel, a liquid crystal panel, a transparent switch, a surface heating element and the like.
However, in the case of a film using ITO or the like as a conductive thin film, since the thin film is made of an inorganic material, its bending property is weak and it is disadvantageous to implement flexibility of the final product.
As a result, many researches and developments have been made on various conductive materials capable of realizing low resistance as a substitute material of ITO, among which metal nano wires are attracting attention due to their excellent electric conductivity, flexibility and optical characteristics.
Basically, in order to apply the metal nanowire as a conductive material of a display, a thin, long and high aspect ratio characteristic is required because the optical characteristic should be excellent.
These metal nanowires are generally made by a polyol reduction method through a heating reaction of a reducing solvent. In order to control diameter and length, various factors (reaction temperature, precursor and catalyst concentration, ratio, etc.) .
Korean Patent No. 1,089,299 relates to a method for producing metal nanowires using an ionic liquid, wherein a metal element generated through a polyol reduction reaction is formed by mixing a metal salt and a reducing solvent in the presence of an ionic liquid, Discloses a method of manufacturing a metal nanowire that is manufactured in the form of nanowires through interaction with the metal nanowires.
However, when the metal nanowires are manufactured through the above-described method, the metal nanowires having a small diameter and a long length and having a high aspect ratio depend on the ratio of the halogen-containing catalyst to the metal salt. There is a disadvantage in that the yield is reduced and a large amount of by-products are produced due to the reaction.
It is an object of the present invention to provide a method for producing silver nanowires capable of controlling diameter and length by controlling silver nanowires by a reduction method by ultraviolet irradiation and controlling a reduction rate according to ultraviolet irradiation amount and irradiation time.
It is also an object of the present invention to provide a transparent conductive film containing silver nanowires.
According to an aspect of the present invention, there is provided a method for producing a silver halide photographic light-sensitive material, comprising: preparing a solution containing silver salt and a capping agent; And a step of irradiating the solution with ultraviolet light to produce silver nanowires. The silver nanowires are produced by a reduction method using ultraviolet irradiation.
At this time, the ultraviolet wavelength is 280 to 400 nm, the intensity is 1 to 10 W / cm 2 , and the irradiation time is 5 to 60 minutes.
The capping agent is preferably at least one selected from the group consisting of polyvinylpyrrolidone, polyvinyl acetate, polyvinyl alcohol, cetyltrimethylammonium bromide, cetyltrimethylammonium chloride, polyacrylamide and polyacrylic acid, The molecular weight of the ping agent is preferably 30,000 to 100,000.
The present invention also provides a coating composition comprising silver nanowires, a binder and a surfactant and a solvent prepared by the above-described method.
In addition, the present invention provides a transparent conductive film wherein the coating composition is applied to one side or both sides of a film.
The present invention can control the diameter and length of silver nanowires by controlling the reduction rate according to the amount of ultraviolet irradiation and the irradiation time by preparing silver nanowires using a reduction method by ultraviolet irradiation, and it is easy to control compared to existing polyol reduction method , And since a halogen catalyst is not used, it is possible to suppress the addition reaction and thereby to improve the production and reduction of a large amount of by-products.
In addition, when the transparent conductive film is produced on the basis of the silver nanowire of the present invention, it is possible to improve the conductivity of the silver nanowire by reducing the contact resistance between the nanowires, thereby reducing the overall sheet resistance of the transparent conductive film, It is possible to improve the unevenness.
Figure 1 schematically illustrates a silver nanowire according to one embodiment of the present invention.
Hereinafter, the present invention will be described in detail so that those skilled in the art can readily understand the present invention and can carry out the present invention without undue experimentation.
In describing the present invention, the terms first, second, etc. may be used to describe various components, but the components should not be limited by the terms.
The present invention relates to a method for producing a silver halide photographic light-sensitive material, And irradiating the solution with ultraviolet light to produce silver nanowires.
Meanwhile, the method for producing silver nanowires according to the present invention proceeds based on a reduction method by ultraviolet irradiation.
The method for manufacturing silver nanowires according to the present invention will be described in detail as follows.
First, a silver salt and a capping agent are added to a solvent to prepare a solution.
Here, the solvent is preferably deionized water, but is not limited thereto.
The silver salt is not particularly limited, but silver nitrate (AgNO 3 ), perchloric acid (AgClO 4 ), silver chloride (AgClO 3 ), silver acetate, silver carbonate, Is preferably used.
The capping agent is added to a solvent to induce wire formation. When the reduction for silver nanowire formation is performed too fast, it is difficult for the metals to aggregate and form a wire shape so that the materials in the solvent are appropriately dispersed So as to prevent aggregation.
The capping agent may be at least one selected from the group consisting of polyvinylpyrrolidone, polyvinyl acetate, polyvinyl alcohol, cetyltrimethylammonium bromide, cetyltrimethylammonium chloride, polyacrylamide and polyacrylic acid. It does not.
The molecular weight of the capping agent is preferably 40,000 to 100,000, and when the molecular weight of the water-soluble polymer is within the above range, one-dimensional nanowires can be grown.
Silver nanowires can be prepared by irradiating ultraviolet rays to a solution containing silver salts, a capping agent and a solvent as described above to reduce the solvent and solvated elecron in the solution to metal cations.
At this time, the ultraviolet wavelength is preferably 280 to 400 nm, and the intensity is preferably 1 to 10 W / cm 2 , but is not limited thereto. When the intensity of ultraviolet rays is less than 1 W / cm 2 , the reaction does not start. When the intensity exceeds 10 W / cm 2, nanowires having a large diameter are formed rapidly or amorphous nanoparticles are formed.
The ultraviolet ray irradiation time is preferably 5 to 60 minutes, but is not limited thereto. When the irradiation time is less than 5 minutes, the length of the nanowire is shortened. When the irradiation time exceeds 60 minutes, the growth in the nanowire length direction no longer occurs.
The diameter of the silver nanowires produced by this method is 15 to 50 nm, the length is 15 μm or more, and the aspect ratio is 500 to 1200.
Hereinafter, the coating composition containing silver nanowires and the transparent conductive film according to the present invention will be described in detail.
The coating compositions of the present invention may comprise the silver nanowires, binders, surfactants and solvents.
Here, the coating composition includes silver nanowires, so that the contact resistance between the nanowires is reduced to improve the conductivity of the silver nanowires, thereby reducing the overall sheet resistance of the film and improving non-uniformity.
On the other hand, the content of the silver nanowires is preferably 0.1 to 0.5 wt%, the binder is 0.02 to 0.05 wt%, and the surfactant is 0.005 to 0.05 wt% based on the total weight of the coating composition, but is not limited thereto.
The binder may be one or more polymers, copolymers or oligomers such as acrylic polymers, vinyl polymers, polyesters, polycarbonates, styrene polymers, polyurethanes, polyolefins, epoxy polymers, cellulosic polymers, silicone polymers, But are not limited to, polymers, rubbers, conducting polymers, reversed conducting polymers, nonconductive polymers and the like.
The solvent is not particularly limited as long as it can improve workability such as coatability, but organic solvents such as water, alcohols, glycols, ketones, esters, amides and hydrocarbons are preferably used .
The transparent conductive film of the present invention can be formed by applying the coating composition to one side or both sides of the film.
Here, the coating composition may be coated by a suitable method depending on the material to be used. For example, the coating composition may be coated on a hard-coated film and then dried.
Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries are to be interpreted as having a meaning consistent with the contextual meaning of the related art and are to be interpreted as either ideal or overly formal in the sense of the present application Do not.
Hereinafter, the present invention will be described in detail with reference to examples. However, these examples are for illustrating the present invention specifically, and the scope of the present invention is not limited to these examples.
Examples 1 to 9
50 mmol of AgNO 3 and 250 mmol of polyvinylpyrrolidone (molecular weight = 55,000) were dissolved in deionized water and stirred at room temperature for 15 minutes. UV light having a wavelength of 280 nm was irradiated to the mixed solution for the intensity of the irradiation amount shown in the following Table 1 and irradiation time to synthesize silver nanowires, respectively.
Comparative Example 1
50 mmol of AgNO 3 and 250 mmol of polyvinylpyrrolidone (molecular weight = 55,000) were dissolved in deionized water and stirred at room temperature for 15 minutes. The silver nanowires were synthesized by irradiating the mixed solution with visible light having a wavelength of 550 nm for 20 minutes at an intensity of 5 W / cm 2 .
Evaluation example
Diameters and lengths of the silver nanowires prepared in Examples and Comparative Examples were measured by scanning electron microscope (SEM), and the results are shown in Table 1 below.
As can be seen in Table 1, the silver nanowires prepared in Examples 1 to 9 of the present invention can control the diameter and length of silver nanowires by adjusting the amount of ultraviolet irradiation and the irradiation time to control the reduction rate Respectively.
Claims (6)
And irradiating the solution with ultraviolet light to produce silver nanowires. 2. The silver nanowire manufacturing method according to claim 1,
Wherein the ultraviolet wavelength is from 280 to 400 nm, the intensity is from 1 to 10 W / cm 2 , and the irradiation time is from 5 to 60 minutes.
Wherein the capping agent is at least one selected from the group consisting of polyvinylpyrrolidone, polyvinyl acetate, polyvinyl alcohol, cetyltrimethylammonium bromide, cetyltrimethylammonium chloride, polyacrylamide and polyacrylic acid. A method for producing silver nanowires using a reduction method.
Wherein the capping agent has a molecular weight of 30,000 to 100,000.
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| KR1020140129088A KR20160037298A (en) | 2014-09-26 | 2014-09-26 | Silver nanowire using reduction for ultraviolet irradating, preparing method of the same and transparent conductive film including the same |
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| KR1020140129088A KR20160037298A (en) | 2014-09-26 | 2014-09-26 | Silver nanowire using reduction for ultraviolet irradating, preparing method of the same and transparent conductive film including the same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180053490A (en) * | 2016-11-11 | 2018-05-23 | 한국생산기술연구원 | Preparing method of metal nanotube for transparent electrode using electrospinning |
| CN108468209A (en) * | 2018-03-16 | 2018-08-31 | 三元控股集团有限公司 | A kind of preparation method of the antibiotic fabric based on UV-curing technology |
| CN109014242A (en) * | 2018-09-11 | 2018-12-18 | 昆明理工大学 | A kind of preparation method of nano silver wires with high length-diameter ratio |
| WO2019141260A1 (en) * | 2018-01-22 | 2019-07-25 | 深圳市希诺威光电科技有限公司 | Method for manufacturing surface-roughened silver nanowire |
-
2014
- 2014-09-26 KR KR1020140129088A patent/KR20160037298A/en not_active Application Discontinuation
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180053490A (en) * | 2016-11-11 | 2018-05-23 | 한국생산기술연구원 | Preparing method of metal nanotube for transparent electrode using electrospinning |
| WO2019141260A1 (en) * | 2018-01-22 | 2019-07-25 | 深圳市希诺威光电科技有限公司 | Method for manufacturing surface-roughened silver nanowire |
| CN108468209A (en) * | 2018-03-16 | 2018-08-31 | 三元控股集团有限公司 | A kind of preparation method of the antibiotic fabric based on UV-curing technology |
| CN109014242A (en) * | 2018-09-11 | 2018-12-18 | 昆明理工大学 | A kind of preparation method of nano silver wires with high length-diameter ratio |
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