KR20160020842A - Transparent conductive film and method for manufacturing the same - Google Patents
Transparent conductive film and method for manufacturing the same Download PDFInfo
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- KR20160020842A KR20160020842A KR1020140106081A KR20140106081A KR20160020842A KR 20160020842 A KR20160020842 A KR 20160020842A KR 1020140106081 A KR1020140106081 A KR 1020140106081A KR 20140106081 A KR20140106081 A KR 20140106081A KR 20160020842 A KR20160020842 A KR 20160020842A
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
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- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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Abstract
Description
The present invention relates to a transparent conductive film and a method of manufacturing the same.
The transparent conductive film means a thin film having high transparency to light and electricity, and can be used for a liquid crystal display, an electrochromic display (ECD), an organic electroluminescence device, a solar cell, a plasma Are widely used as voltage-applying common electrodes and pixel electrodes such as a plasma display panel, a flexible display, an electronic paper, and a touch panel.
ITO (Indium Tin Oxide) can be exemplified as a typical example of the transparent conductive film, but it is difficult to increase the size due to limitations of the manufacturing method, and low yield and high price are formed. In addition, since it is difficult to apply ITO as a flexible film, it is necessary to develop a transparent conductive film which can replace ITO.
It is an object of the present invention to provide a transparent conductive film applicable to an electronic device and a method of manufacturing the transparent conductive film.
An embodiment of the present disclosure includes a transparent substrate and an electrically conductive layer provided on the transparent substrate, wherein the electrically conductive layer comprises a poly vinyl alcohol (PVA) based polymer and an electrically conductive material constituting a three dimensional network , The light transmittance of the electrically conductive layer has a light transmittance of 85% or more in light of 550 nm wavelength, and the surface hardness of the electrically conductive layer is pencil hardness H or higher.
One embodiment of the present disclosure relates to a method of manufacturing a transparent substrate, Forming a composition comprising a solvent, a PVA-based polymer, and an electrically conductive material; And forming an electrically conductive layer using the composition. The present invention also provides a method for producing the transparent conductive film.
One embodiment of the present invention provides a transparent electrode comprising the transparent conductive film.
One embodiment of the present invention provides an electronic device including the transparent electrode.
The transparent conductive film according to one embodiment of the present invention has a low surface roughness value, and thus has a high bonding strength with an adjacent layer when included in an electronic device.
Since the transparent conductive film according to one embodiment of the present invention has excellent light transmittance and low haze value, it can be applied to various applications such as transparent electrodes and light scattering layers of electronic devices.
The transparent conductive film according to one embodiment of the present invention has an advantage that it can be manufactured through a simple manufacturing process.
The transparent conductive film according to one embodiment of the present invention does not cause a moiré phenomenon and can realize excellent tactility when it is included in an electronic device.
The transparent conductive film according to one embodiment of the present invention is advantageous in that it can be easily made larger and can be manufactured by a simple process. Specifically, the transparent conductive film according to one embodiment of the present invention has an advantage of securing excellent electrical conductivity and scratch resistance through a single coating solution process.
The transparent conductive film according to one embodiment of the present invention has an excellent adhesion to a substrate and a strong scratch resistance, thereby preventing the function from being lost due to external stress.
The transparent conductive film according to one embodiment of the present invention can minimize damage due to the external environment even if it does not have a separate protective layer.
Fig. 1 shows an image of a transparent conductive film produced according to Example 1. Fig.
Fig. 2 shows an image after forming a surface scratch in order to measure the surface hardness of the transparent conductive film produced according to Example 1. Fig.
Fig. 3 shows an image of a transparent conductive film produced according to Example 2. Fig.
Fig. 4 shows an image after forming a surface scratch to measure the surface hardness of the transparent conductive film produced according to Example 2. Fig.
Fig. 5 shows an image of a transparent conductive film produced according to Example 3. Fig.
Fig. 6 shows an image after forming a surface scratch to measure the surface hardness of the transparent conductive film produced according to Example 3. Fig.
Fig. 7 shows an image of a transparent conductive film produced according to Comparative Example 1. Fig.
FIG. 8 shows an image after forming a surface scratch to measure the surface hardness of the transparent conductive film produced according to Comparative Example 1. FIG.
Fig. 9 shows an image of a transparent conductive film produced according to Comparative Example 2. Fig.
10 shows an image after forming a surface scratch in order to measure the surface hardness of the transparent conductive film produced according to Comparative Example 2. Fig.
Fig. 11 shows an image of a transparent conductive film produced according to Comparative Example 3. Fig.
Fig. 12 shows an image after forming a surface scratch to measure the surface hardness of the transparent conductive film produced according to Comparative Example 3. Fig.
Fig. 13 shows an image of a transparent conductive film produced according to Comparative Example 4. Fig.
14 shows an image after forming a surface scratch in order to measure the surface hardness of the transparent conductive film produced according to Comparative Example 4. Fig.
Fig. 15 shows an image of a transparent conductive film produced according to Comparative Example 5. Fig.
16 shows an image after forming a surface scratch to measure the surface hardness of the transparent conductive film produced according to Comparative Example 5. Fig.
17 shows an image of a transparent conductive film produced according to Comparative Example 6. Fig.
18 shows an image after forming a surface scratch in order to measure the surface hardness of the transparent conductive film produced according to Comparative Example 6. Fig.
When a member is referred to herein as being "on " another member, it includes not only a member in contact with another member but also another member between the two members.
Whenever a component is referred to as "comprising ", it is to be understood that the component may include other components as well, without departing from the scope of the present invention.
Hereinafter, the present invention will be described in more detail.
An embodiment of the present disclosure includes a transparent substrate and an electrically conductive layer provided on the transparent substrate, wherein the electrically conductive layer comprises a poly vinyl alcohol (PVA) based polymer and an electrically conductive material constituting a three dimensional network , The light transmittance of the electrically conductive layer has a light transmittance of 85% or more in light of 550 nm wavelength, and the surface hardness of the electrically conductive layer is pencil hardness H or higher.
The transparent conductive layer according to one embodiment of the present invention has an elasticity, so that it is advantageous in that the function is not lost even when the substrate is bent on the flexible substrate.
In this specification, "conductive" means electrical conductivity.
According to one embodiment of the present disclosure, the electrically conductive material constitutes a three-dimensional network and may mean a three-dimensional electrically conductive line.
According to one embodiment of the present invention, the light transmittance of the electrically conductive layer may have a light transmittance of not less than 85% and not more than 100% in a light having a wavelength of 550 nm.
In the present specification, "light transmittance" is a value measured by a V-7100 UV-Vis spectrophotometer of JASCO Co., Ltd., in which light transmittance in a 550 nm wavelength light is measured.
The surface hardness value in the present specification is a pencil hardness value, and the pencil hardness is measured using ASTM D7027 which is a standard specification, and the load used here is 500 g.
The surface hardness of the electrically conductive layer in this specification means to maintain electrical conductivity without loss of electrical conductivity when forming a surface scratch with an intensity of pencil hardness H or higher. Specifically, since the electrically conductive material forms a three-dimensional network, the inside of the electrically conductive layer can maintain electrical conductivity even by a surface scratch.
According to one embodiment of the present disclosure, the sheet resistance of the electrically conductive layer when a surface scratch of not less than pencil hardness H is generated can be 80% or more of the electrical conductivity without surface scratches. Specifically, according to one embodiment of the present invention, the surface resistance in the case where a surface scratch of a pencil hardness H or higher is generated in the electrically conductive layer may be 90% or more of the electrical conductivity in the case where there is no surface scratch.
According to one embodiment of the present invention, the surface hardness of the electrically conductive layer may be not less than 5H and not less than H pencil hardness.
According to one embodiment of the present invention, the PVA-based polymer is a polymer containing vinyl alcohol. According to one embodiment of the present invention, the PVA-based polymer is a poly (vinyl alcohol-co-methyl methacrylate) (poly (vinyl alcohol-co-methyl methacrylate) Or a PVA-based copolymer such as poly (vinyl butyral-co-vinylalcohol-co-vinylacetate).
According to one embodiment of the present invention, the saponification degree of the PVA-based polymer may be 80% or more and 90% or less. Specifically, according to one embodiment of the present invention, the saponification degree of the PVA-based polymer may be 85% or more and 90% or less.
The saponification degree may refer to a weight ratio of vinyl alcohol in the PVA-based polymer.
According to one embodiment of the present invention, when the saponification degree of the PVA polymer is within the above range, the electroconductive material can smoothly form a three-dimensional network, and the light transmittance and surface hardness of the electroconductive layer It can be excellent. Specifically, when the degree of saponification of the PVA polymer is less than the above range, the electroconductive material may form a three-dimensional network at a low density, resulting in a problem of deterioration of electrical conductivity. In addition, when the degree of saponification of the PVA polymer is in excess of the above range, the content of the electroconductive material becomes excessively high, thereby lowering the light transmittance and lowering the surface hardness of the electroconductive layer.
According to one embodiment of the present invention, the weight average molecular weight of the PVA-based polymer may be 50,000 or more and 500,000 or less. Specifically, according to one embodiment of the present invention, the weight average molecular weight of the PVA-based polymer may be 70,000 or more and 150,000 or less.
When the weight average molecular weight of the PVA polymer is within the above range, the solubility of the PVA polymer in a solvent is excellent during the formation of the composition for preparing the electroconductive layer, thereby easily forming the electroconductive layer, It is possible to form a three-dimensional network of density.
When the weight average molecular weight of the PVA polymer is less than the above range, the three-dimensional network formed by the electroconductive material may be formed at a low density, thereby increasing the sheet resistance. If the weight average molecular weight of the PVA polymer exceeds the above range, the solubility of the PVA polymer in the solvent may be decreased during the formation of the composition for preparing the electroconductive layer.
According to one embodiment of the present invention, the PVA-based polymer may be cross-linked with an acrylate-based monomer.
The acrylate-based polymer may enhance the adhesion between the electrically conductive layer and the transparent substrate.
Specifically, according to one embodiment of the present invention, the acrylate compound may be an acrylate compound having three or more reactors. Specifically, according to one embodiment of the present invention, the acrylate-based compound may include at least one selected from the group consisting of pentaerythritol triacrylate (PETA), trimethylolpropane triacrylate (TMPTA), and dipentaerythritol hexaacrylate (DPHA).
According to one embodiment of the present invention, the content of the PVA polymer may be 0.5 wt% or more and 15 wt% or less with respect to the electroconductive layer. Specifically, according to one embodiment of the present invention, the content of the PVA polymer may be 5 wt% or more and 15 wt% or less with respect to the electroconductive layer.
When the content of the PVA polymer is within the above range, the formation of the three-dimensional network of the electroconductive material is smoothly performed. Further, when the content of the PVA polymer is 5 wt% or more with respect to the electroconductive layer, The three-dimensional network formation of the material may be easier. When the content of the PVA polymer is more than 15 wt% with respect to the electroconductive layer, the electrical conductivity of the electroconductive layer may significantly decrease.
According to one embodiment of the present invention, when the content of the PVA polymer is within the above range, the scratch resistance of the electroconductive layer is improved and the electroconductive material can smoothly form a three-dimensional network.
According to one embodiment of the present disclosure, the PVA-based polymer may form a polymer network of the electrically conductive layer.
According to one embodiment of the present disclosure, the electrically conductive layer comprises a polymer matrix comprising a PVA-based polymer; And an electrically conductive material provided at an interface of the PVA polymer to constitute a three-dimensional network.
According to one embodiment of the present invention, the surface roughness value Ra of the electrically conductive layer may be 3 占 퐉 or less.
In the present specification, "surface roughness value (Ra)" is a value measured using 3D Optical Profiler NV-2000.
The transparent conductive film according to one embodiment of the present invention has a low surface roughness value. Therefore, when the present invention is applied to an electronic device, when another member or layer is formed on the transparent conductive film, the bonding strength is high and the defective ratio .
According to one embodiment of the present disclosure, the haze value of the electrically conductive layer may be 3 or less. Specifically, according to one embodiment of the present disclosure, the haze value of the electrically conductive layer may be 1 or less.
In the present specification, "haze value" is a value measured using a color research laboratory HM-150 hazemeter of Murakami.
The transparent conductive film according to one embodiment of the present invention has excellent light transmittance and low haze value, and thus can be used for a transparent electrode and a light scattering layer of an electronic device. Further, since the transparent conductive film has a high light transmittance, the light loss rate is low and the efficiency of the electronic device can be increased.
According to one embodiment of the present disclosure, the sheet resistance of the electrically conductive layer may be less than 300? / ?. According to one embodiment of the present invention, the sheet resistance of the transparent conductive film may be 1 Ω / □ or more, or 10 Ω / □ or more.
According to an embodiment of the present invention, the electrically conductive material may include at least one selected from the group consisting of a metal nanowire, a conductive metal oxide, and a conductive polymer material.
According to an embodiment of the present invention, the metal nanowire may include at least one metal selected from the group consisting of Cu, Zn, Cr, Ag, Au, and Pt. Specifically, according to one embodiment of the present disclosure, the metal nanowire may be an AgNW (Ag nanowire) including Ag.
According to one embodiment of the present disclosure, the aspect ratio of the diameter and length of the metal nanowires may be 100: 1 to 1000: 1. According to an embodiment of the present invention, the diameter of the metal nanowire may be 20 nm or more and 50 nm or less.
According to an embodiment of the present invention, the conductive metal oxide may include at least one material selected from the group consisting of an In-based oxide, an Nb-based oxide, a Ti-based oxide and a Zn-based oxide.
According to one embodiment of the present invention, the In-based oxide may be indium tin oxide (ITO), indium zinc oxide (IZO).
According to one embodiment of the present disclosure, the Nb-based oxide may be NbO 2 .
According to one embodiment of the present disclosure, the Ti-based oxide may be TiO 2 .
According to one embodiment of the present invention, the Zn-based oxide may be Ga-doped ZnO, Al-doped ZnO, or Ga-doped ZnO.
According to one embodiment of the present invention, the conductive polymer material may be PEDOT: PSS (poly (3,4-ethylenedioxythiophene): polystyrenesulfonic acid).
According to one embodiment of the present disclosure, the electrically conductive material comprises a metal nanowire and a conductive metal oxide, wherein the metal nanowire forms a three-dimensional network, and the conductive metal oxide comprises at least two of the metal nanowires Can be electrically connected.
According to one embodiment of the present disclosure, the electrically conductive layer may be a single layer structure.
According to one embodiment of the present disclosure, the thickness of the electrically conductive layer may be 300 nm or more and 2 占 퐉 or less.
According to one embodiment of the present invention, when the thickness of the electrically conductive layer is within the above range, excellent electrical conductivity can be realized. Specifically, when the thickness is less than the above-mentioned range, a problem that the electrically conductive material can not smoothly form a three-dimensional network may occur. If the thickness exceeds the above-mentioned range, the thickness of the electrically conductive layer becomes excessively thick and the light transmittance may become low.
According to one embodiment of the present disclosure, the transparent substrate may be a glass substrate or a plastic substrate.
According to one embodiment of the present invention, the adhesion of the electrically conductive layer to a PET (polyethylene terephthalate) substrate is 4B or more and 5B or less, and the adhesion value may be according to ASTM D3359-02, which is an adhesive force test.
Specifically, the adhesion test is one of the methods of cross cut test by tape, and when the adhesive force is 4B, the electrically conductive layer is hardly separated from the PET substrate by the tape. In the case of 5B, And the layer is not separated from the PET substrate at all by the tape.
According to one embodiment of the present disclosure, the transparent conductive film may be flexible.
According to one embodiment of the present invention, the substrate can use a substrate having excellent transparency, surface smoothness, ease of handling, and waterproofness. Specifically, a glass substrate, a thin film glass substrate, or a transparent plastic substrate can be used. The plastic substrate may include films such as PET (polyethylene terephthalate), TAC (triacetyl cellulose), PEN (polyethylene naphthalate), PEEK (polyether ether ketone) and PI (polyimide) in a single layer or a multilayer.
One embodiment of the present disclosure relates to a method of manufacturing a transparent substrate, Forming a composition comprising a solvent, a PVA-based polymer, and an electrically conductive material; And forming an electrically conductive layer using the composition. The present invention also provides a method for producing the transparent conductive film.
According to one embodiment of the present invention, the composition may further comprise an acrylate-based compound.
According to one embodiment of the present invention, the acrylate-based compound may act to polymerize the PVA-based polymer. Also, according to one embodiment of the present invention, the acrylate-based compound may participate in polymerization of the PVA-based polymer through a photoinitiator or a thermal initiator.
According to one embodiment of the present invention, the content of the acrylate-based compound may be 10 wt% or more and 50 wt% or less based on the PVA-based polymer. Specifically, according to one embodiment of the present invention, the content of the acrylate compound may be 30 wt% or more and 50 wt% or less with respect to the PVA-based polymer.
When the content of the acrylate compound is within the above range, the adhesion between the electrically conductive layer and the transparent substrate can be increased.
The acrylate compound contained in the composition is the same as the acrylate compound described above.
According to one embodiment of the present invention, the composition may further include at least one member selected from the group consisting of a thermal initiator, a photoinitiator, a dispersant, and an antioxidant.
According to one embodiment of the present disclosure, the photoinitiator or thermal initiator may be hydrophilic. In addition, the thermal initiator and the photoinitiator can be used without limitation as long as they are used in the art.
According to one embodiment of the present invention, the content of the photoinitiator or the thermal initiator may be 1 wt% or more and 15 wt% or less based on the acrylate compound.
The dispersant of the present invention can prevent the aggregation of the electroconductive materials in the solvent.
According to one embodiment of the present invention, the dispersing agent is selected from the group consisting of polyvinyl pyrrolidone (PVP), polyoxyethylene glycol alkyl ether (Brij), polyoxyethylene glycol octyl nonionic dispersants such as phenol ether and glycerol alkyl ester; And ionic dispersants such as CTAB (cetyl trimethyl ammonium bromide), sodium stearate, and SDS (sodium dodecyl sulfate).
According to one embodiment of the present invention, the antioxidant may include at least one selected from the group consisting of a phenol antioxidant, an amine antioxidant, and a phosphorus antioxidant. However, the antioxidant may be used without limitation as long as it is used in the art.
According to one embodiment of the present invention, the content of the antioxidant may be 0.1 wt% or more and 5 wt% or less based on the composition.
According to one embodiment of the present invention, the content of the electrically conductive material may be 0.05 wt% or more and 1 wt% or less with respect to the total composition.
According to one embodiment of the present disclosure, the step of forming the electrically conductive layer may include coating the composition on the transparent substrate, and then curing the composition.
One embodiment of the present invention provides a transparent electrode comprising the transparent conductive film.
Specifically, according to one embodiment of the present invention, the transparent electrode may be formed of the transparent conductive film. According to an embodiment of the present invention, the transparent electrode may further include an additional layer as needed.
The present specification provides an electronic device including the transparent electrode. Specifically, the electronic device may be a touch panel, a light emitting glass, a light emitting device, a solar cell, or a transistor.
The touch panel, the light emitting glass, the light emitting device, the solar cell, and the transistor may be commonly known in the art, and the electrode may be used as the transparent electrode of the present invention.
Hereinafter, the present invention will be described in detail by way of examples with reference to the drawings. However, the embodiments according to the present disclosure can be modified in various other forms, and the scope of the present specification is not construed as being limited to the embodiments described below. Embodiments of the present disclosure are provided to more fully describe the present disclosure to those of ordinary skill in the art.
[Example 1]
Ag nanowire (AgNW) with an aspect ratio of about 1000 nm and PVA with a degree of saponification of 87% to 89% (Sigma-aldrich catalog) with a diameter of about 30 nm and an aspect ratio of 1000: 1 were added to a 5: 5 mixture of water and IPA No. 333081) and PETA (pentaerythritol triacrylate) were added in a weight ratio of 9: 0.66: 0.33, and a composition was prepared by adding rgacure 2959 (BASF) as a photoinitiator to PETA in an amount of 10% by weight. At this time, the total weight of AgNW, PVA and PETA was 0.15 wt% with respect to the solvent.
After coated on a PET (polyethyleneterephthalate) the substrate the composition as a bar coating method, a transparent conductive film by screen 1 minutes 30 seconds 80 ℃ dried in UV having up to about 1000 mJ / cm 2 energy of 1 to 3 seconds sight from . At this time, the thickness of the electrically conductive layer formed on the PET substrate was 400 nm.
The sheet resistance of the transparent conductive film prepared according to Example 1 was 300 Ω / □ or less, the surface hardness was H or higher, the light transmittance was 89.56% at a wavelength of 550 nm, and the haze was 0.3.
Fig. 1 shows an image of a transparent conductive film produced according to Example 1. Fig. Specifically, in the bright solid line area in Fig. 1, AgNW forms a three-dimensional network.
Fig. 2 shows an image after forming a surface scratch in order to measure the surface hardness of the transparent conductive film produced according to Example 1. Fig. Specifically, FIG. 2 shows scratches formed on the surface of the transparent conductive film according to Example 1 with an intensity of pencil hardness H. FIG. According to Example 1, as shown in Fig. 2, the electric conductivity in the region where the scratch was formed with the pencil hardness H had no significant influence.
[Example 2]
A transparent conductive film having a thickness of 600 nm was prepared in the same manner as in Example 1.
The sheet resistance of the transparent conductive film prepared in Example 2 was 200 Ω / □ or less, the surface hardness was H or more, the light transmittance was 88.99% in light with a wavelength of 550 nm, and the haze was 0.8.
Fig. 3 shows an image of a transparent conductive film produced according to Example 2. Fig. Specifically, in FIG. 3, the bright solid line indicates that the AgNW forms a three-dimensional network.
Fig. 4 shows an image after forming a surface scratch to measure the surface hardness of the transparent conductive film produced according to Example 2. Fig. Specifically, FIG. 2 shows scratches formed on the surface of the transparent conductive film according to Example 2 at an intensity of pencil hardness H. FIG. According to Example 2, as shown in Fig. 4, the electric conductivity in the region where the scratch was formed with the pencil hardness H had no significant influence.
[Example 3]
A transparent conductive film having a thickness of 850 nm was prepared in the same manner as in Example 1.
The sheet resistance of the transparent conductive film prepared in Example 3 was 150 Ω / □ or less, the surface hardness was H or higher, the light transmittance was 88.01% at a wavelength of 550 nm, and the haze was 1.6.
Fig. 5 shows an image of a transparent conductive film produced according to Example 3. Fig. Specifically, in the bright solid line area in Fig. 5, AgNW forms a three-dimensional network.
Fig. 6 shows an image after forming a surface scratch to measure the surface hardness of the transparent conductive film produced according to Example 3. Fig. Specifically, FIG. 6 shows scratches formed on the surface of the transparent conductive film according to Example 3 with an intensity of pencil hardness H. FIG. According to Example 3, as shown in Fig. 6, the electric conductivity in the region where the scratch was formed with the pencil hardness H had no significant influence.
[Comparative Example 1]
AgNW (Ag nanowire) having a diameter of about 30 nm and an aspect ratio of 1000: 1 was added to water in an amount of 0.15 weight% with respect to water, and PVP (Polyvinylpyrrolidone) as a dispersing agent was added in an amount of 2 weight% with respect to AgNW to disperse the binder. Acrylate was added in an amount of 10% by weight based on the weight of AgNW, applied on a PET (polyethyleneterephthalate) substrate by a bar coating method, and dried at 80 캜 for 1 minute and 30 seconds to prepare a transparent conductive film having a thickness of 200 nm.
The sheet resistance of the transparent conductive film produced according to Comparative Example 1 was 100 Ω / □ or less, the surface hardness was less than H, the light transmittance was 90.75% at a wavelength of 550 nm, and the haze was 0.1.
Fig. 7 shows an image of a transparent conductive film produced according to Comparative Example 1. Fig. Specifically, in FIG. 7, the bright solid line region forms a two-dimensional network on the substrate.
FIG. 8 shows an image after forming a surface scratch to measure the surface hardness of the transparent conductive film produced according to Comparative Example 1. FIG. Specifically, FIG. 8 shows scratches formed on the surface of the transparent conductive film of Comparative Example 1 with an intensity of pencil hardness H. FIG. According to Comparative Example 1, as shown in Fig. 8, most of the AgNW was lost in the region where the scratch was formed at the intensity of pencil hardness H, and the electrical conductivity was remarkably lowered.
[Comparative Example 2]
A transparent conductive film having a thickness of 200 nm was prepared in the same manner as in Example 1.
The sheet resistance of the transparent conductive film prepared in Comparative Example 2 was 6,000? / ?, the surface hardness was H, the light transmittance was 91.05% in light with a wavelength of 550 nm, and the haze was 0.
The transparent conductive film produced according to Comparative Example 2 was excellent in surface hardness and haze value, but had a too high sheet resistance value and could not serve as a conductive film. Specifically, at a thickness of 200 nm, it can be seen that AgNW can not form a three-dimensional network smoothly in the PVA, resulting in a high sheet resistance.
Fig. 9 shows an image of a transparent conductive film produced according to Comparative Example 2. Fig. Specifically, the bright solid line in FIG. 9 shows AgNW, but the sheet resistance is too high because AgNW does not form a network.
10 shows an image after forming a surface scratch in order to measure the surface hardness of the transparent conductive film produced according to Comparative Example 2. Fig. Specifically, FIG. 10 shows that scratches were formed on the surface of the transparent conductive film according to Comparative Example 2 with the pencil hardness H. According to Comparative Example 2, although the surface hardness maintained a high value as H, it had an excessively high sheet resistance value and thus was not applicable to electronic devices.
[Comparative Example 3]
Ag nanowire (AgNW) with an aspect ratio of about 1000 nm and PVA with a degree of saponification of 87% to 89% (Sigma-aldrich catalog) with a diameter of about 30 nm and an aspect ratio of 1000: 1 were added to a 5: 5 mixture of water and IPA no.363081), and PETA (pentaerythritol triacrylate) were added in a weight ratio of 9.5: 0.33: 0.16, a transparent conductive film having a thickness of 200 nm was prepared.
The sheet resistance of the transparent conductive film prepared in Comparative Example 3 was 100 to 150 Ω / □, the surface hardness was less than H, the light transmittance was 90.18% at a wavelength of 550 nm, and the haze was 0.3.
Fig. 11 shows an image of a transparent conductive film produced according to Comparative Example 3. Fig. Specifically, in the bright solid line area in FIG. 11, AgNW forms a two-dimensional network on the substrate.
Fig. 12 shows an image after forming a surface scratch to measure the surface hardness of the transparent conductive film produced according to Comparative Example 3. Fig. Specifically, FIG. 12 shows scratches formed on the surface of the transparent conductive film according to Comparative Example 3 at an intensity of pencil hardness H. FIG. According to Comparative Example 3, most of the AgNW was lost in the region where the scratch was formed at the intensity of pencil hardness H as shown in Fig. 12, and the electrical conductivity was remarkably lowered.
[Comparative Example 4]
Ag nanowire (AgNW) with an aspect ratio of about 1000 nm and PVA with a degree of saponification of 87% to 89% (Sigma-aldrich catalog) with a diameter of about 30 nm and an aspect ratio of 1000: 1 were added to a 5: 5 mixture of water and IPA no.363081), and PETA (pentaerythritol triacrylate) were added in a weight ratio of 9.5: 0.33: 0.16, a transparent conductive film having a thickness of 400 nm was prepared.
The sheet resistance of the transparent conductive film prepared in Comparative Example 4 was 100 Ω / □ or less, the surface hardness was less than H, the light transmittance was 88.69% in light with a wavelength of 550 nm, and the haze was 0.9.
Fig. 13 shows an image of a transparent conductive film produced according to Comparative Example 4. Fig. Specifically, in the bright solid line area in Fig. 13, AgNW forms a two-dimensional network on the substrate.
14 shows an image after forming a surface scratch in order to measure the surface hardness of the transparent conductive film produced according to Comparative Example 4. Fig. Specifically, FIG. 14 shows that scratches were formed on the surface of the transparent conductive film of Comparative Example 4 with the pencil hardness H. According to Comparative Example 4, as shown in Fig. 14, most of the AgNW was lost in the region where the scratch was formed at the intensity of pencil hardness H, and the electrical conductivity was remarkably lowered.
[Comparative Example 5]
Ag nanowire (AgNW) with an aspect ratio of about 1000 nm and PVA with a degree of saponification of 87% to 89% (Sigma-aldrich catalog) with a diameter of about 30 nm and an aspect ratio of 1000: 1 were added to a 5: 5 mixture of water and IPA no.363081), and PETA (pentaerythritol triacrylate) were added in a weight ratio of 9.9: 0.06: 0.03, a transparent conductive film having a thickness of 200 nm was prepared.
The sheet resistance of the transparent conductive film prepared in Comparative Example 5 was 100 to 150 Ω / □, the surface hardness was H or less, the light transmittance was 89.8% in light of 550 nm wavelength, and the haze was 0.2.
Fig. 15 shows an image of a transparent conductive film produced according to Comparative Example 5. Fig. Specifically, in FIG. 15, the bright solid line region indicates that the AgNW forms a two-dimensional network on the substrate.
16 shows an image after forming a surface scratch to measure the surface hardness of the transparent conductive film produced according to Comparative Example 5. Fig. Specifically, FIG. 15 shows scratches formed on the surface of the transparent conductive film according to Comparative Example 5 with a pencil hardness of H. FIG. According to Comparative Example 5, as shown in Fig. 16, most of the AgNW was lost in the region where the scratch was formed with the pencil hardness H, and the electrical conductivity was remarkably lowered.
[Comparative Example 6]
Ag nanowire (AgNW) with an aspect ratio of about 1000 nm and PVA with a degree of saponification of 87% to 89% (Sigma-aldrich catalog) with a diameter of about 30 nm and an aspect ratio of 1000: 1 were added to a 5: 5 mixture of water and IPA no.363081), and PETA (pentaerythritol triacrylate) were added in a weight ratio of 9.9: 0.06: 0.03, a transparent conductive film having a thickness of 400 nm was prepared.
The sheet resistance of the transparent conductive film prepared in Comparative Example 6 was 50 Ω / □, the surface hardness was less than H, the light transmittance was 87.87% at a wavelength of 550 nm, and the haze was 0.6.
17 shows an image of a transparent conductive film produced according to Comparative Example 6. Fig. Specifically, in FIG. 17, the bright solid line region indicates that the AgNW forms a two-dimensional network on the substrate.
18 shows an image after forming a surface scratch in order to measure the surface hardness of the transparent conductive film produced according to Comparative Example 6. Fig. Specifically, FIG. 18 shows that scratches were formed on the surface of the transparent conductive film of Comparative Example 6 with the pencil hardness H. According to Comparative Example 6, as shown in Fig. 18, most of the AgNW was lost in the region where the scratch was formed with the pencil hardness H, and the electrical conductivity was remarkably lowered.
Claims (24)
Wherein the electrically conductive layer comprises polyvinyl alcohol (PVA) based polymer and an electrically conductive material constituting a three-dimensional network,
The light transmittance of the electrically conductive layer has a light transmittance of 85% or more in a light having a wavelength of 550 nm,
Wherein the surface hardness of the electrically conductive layer is a pencil hardness H or higher.
Wherein the saponification degree of the PVA polymer is 80% or more and 90% or less.
Wherein the PVA polymer has a weight average molecular weight of 50,000 or more and 500,000 or less.
Wherein the PVA polymer is cross-linked by an acrylate-based compound.
Wherein the content of the PVA polymer is 0.5 wt% or more and 15 wt% or less with respect to the electroconductive layer.
Wherein the electrically conductive layer comprises a polymeric matrix comprising a PVA-based polymer; And an electrically conductive material provided on an interface of the PVA polymer to constitute a three dimensional network.
And the surface roughness value (Ra) of the electrically conductive layer is 3 占 퐉 or less.
Wherein the haze value of the electrically conductive layer is 3 or less.
Wherein the sheet resistance of the electrically conductive layer is 300? /? Or less.
Wherein the electrically conductive material comprises at least one selected from the group consisting of a metal nanowire, a conductive metal oxide, and a conductive polymer material.
Wherein the electrically conductive material comprises a metal nanowire and a conductive metal oxide,
Wherein the metal nanowires form a three dimensional network and the conductive metal oxide electrically connects at least two of the metal nanowires.
Wherein the electrically conductive layer is a single layer structure.
Wherein the thickness of the electrically conductive layer is 300 nm or more and 2 占 퐉 or less.
Wherein the transparent substrate is a glass substrate or a plastic substrate.
The adhesion of the electrically conductive layer to a PET (polyethylene terephthalate) substrate is 4B or more and 5B or less,
Wherein the adhesive force value is according to ASTM D3359-02, the adhesive force test.
Wherein the transparent conductive film is flexible.
Forming a composition comprising a solvent, a PVA-based polymer, and an electrically conductive material;
Forming an electrically conductive layer using the composition;
A method for producing a transparent conductive film according to any one of claims 1 to 16.
Wherein the composition further comprises an acrylate-based compound.
Wherein the content of the acrylate compound is 10 wt% or more and 50 wt% or less with respect to the PVA-based polymer.
Wherein the composition further comprises at least one member selected from the group consisting of a thermal initiator, a photoinitiator, a dispersant, and an antioxidant.
Wherein the content of the electroconductive material is 0.05 wt% or more and 1 wt% or less with respect to the total composition.
Wherein the step of forming the electrically conductive layer comprises coating the composition on the transparent substrate and then curing the composition.
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| KR20180119067A (en) * | 2017-04-24 | 2018-11-01 | (주)에버켐텍 | Graphene laminate comprising cvd graphene, method for manufacturing same, eletrode material using same, and electronic device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20120066544A (en) | 2010-12-14 | 2012-06-22 | 엘지이노텍 주식회사 | Nanowire and method for manufacturing the same |
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| KR20120066544A (en) | 2010-12-14 | 2012-06-22 | 엘지이노텍 주식회사 | Nanowire and method for manufacturing the same |
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| KR20180119067A (en) * | 2017-04-24 | 2018-11-01 | (주)에버켐텍 | Graphene laminate comprising cvd graphene, method for manufacturing same, eletrode material using same, and electronic device |
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