KR101682501B1 - Transparant electrode containing silver nanowire-patterned layer and graphene layer, and manufacturing method thereof - Google Patents
Transparant electrode containing silver nanowire-patterned layer and graphene layer, and manufacturing method thereof Download PDFInfo
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Abstract
A transparent electrode according to the present invention includes a substrate, a graphene layer formed on the substrate, and a silver (Ag) nanowire pattern layer formed on the graphene layer. In the method of manufacturing a transparent electrode according to the present invention, (a) forming a graphene layer on a substrate, (b) forming a photoresist pattern on a surface of the graphene layer formed on the substrate, (c) forming a photoresist pattern on the graphene layer, Coating a solution to form a silver nanowire pattern layer, and (d) removing the photoresist pattern.
The transparent electrode according to the present invention includes a graphene layer and a silver nanowire pattern layer formed by reduction of graphene oxide and having a stable sp 2 hybrid carbon structure and excellent in electrical, thermal and mechanical properties, It is possible to secure a uniform transmittance over the entire surface of the transparent electrode as well as to have electrical conductivity and permeability sufficiently high enough to replace the transparent metal oxide electrode such as FTO and to control the aperture ratio at will, Since the transparent electrode can be manufactured at a low temperature and an atmospheric pressure state by solving the entire process, the electrode manufacturing method has advantages such as reduction of the manufacturing cost, simplification of the manufacturing process, It is possible to form a transparent electrode having the above-mentioned excellent characteristics, Can be usefully used.
Description
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a transparent electrode that can be used for a semiconductor device, a display device, a photovoltaic device, and the like, and a method of manufacturing the same. More specifically, the present invention relates to a transparent electrode including a silver nanowire pattern layer and a graphene layer .
The development of a new electrode material with high conductivity and high transparency, which has excellent chemical stability and is now highly transparent, is a key component in the display device or the solar cell that transmits light and transmits an image and generates current. It is indispensable for device development and researches in related fields are actively being carried out.
Currently, indium tin oxide (ITO), fluorinedoped tin oxide (ITO), and silver (Ag) nanowire are mainly used for the production of transparent electrodes.
First, a manufacturing method of a transparent electrode using indium tin oxide (ITO) is the most widely used manufacturing method, and an ITO transparent electrode is manufactured using a vacuum deposition, an etching, and a corrosive chemical, It produces sensitive solar cells and organic solar cells.
However, ITO does not have abundant reserves of ore, which is expensive, requires high-priced equipment to manufacture, and is expensive because of the use of expensive corrosive chemicals.
In addition, when a transparent electrode made of an oxide such as ITO is bent, the oxide thin film is cracked or broken to increase the surface resistance of the transparent electrode, which is a drawback that it is difficult to apply to a flexible electronic device.
In a dye-sensitized solar cell or an organic solar cell, a transparent electrode coated with fluorine-doped tin oxide (FTO) is also widely used. In the method of fabricating a transparent electrode using FTO, the substrate is coated with FTO, a method of producing a colorless transparent FTO conductive film using a post-treatment process of coating a polymer is commercially available.
However, since the transparent electrode made of fluorine-doped tin oxide (FTO) often has a very rough surface, the process of FTO coating on the substrate is also complicated and expensive deposition or sputtering is used Therefore, the price of the FTO electrode is increased and a large amount of substitution is required. Therefore, it is not applicable to an electrode material of an optoelectronic device.
In the case of a transparent electrode using silver nanowires, a silver nanowire is formed by applying a liquid silver-containing ionic solution on a substrate or by sputtering or the like. Since transparent electrodes made of nanowires are easily formed on the surfaces of silver nanowires, the flexible electrodes made of silver nanowires having surface resistances similar to those of conventional oxide-based transparent electrodes are formed by stacking nanowires Due to the nonconductive portions present between the electrodes, a high criticality concentration is required, making electrodes made of pure silver nanowire films difficult to apply to displays or solar cells.
In addition, it is known that the critical concentration of silver nanowire network can be successfully changed by controlling the diameter and length of the nanowires. Since the nanowires having a crossing structure have a sparsely spaced structure, And a film or a coating having a structure in which silver nanowires are overlapped with each other has defects having an insulating property and thus has a problem in that it does not have electrical properties or catalytic properties required in electronic devices.
In addition, when the silver nanowire is used alone, the surface resistance may be similar to that of the conventional transparent electrode. However, since the silver oxide insulating particles formed on the surface of the silver nanowire have a problem of increasing the surface resistance in use, The silver nanowire network structure requires a high silver nanowire critical concentration in order to have a high electrical conductivity because there is an insulating space that can not allow electrons to pass through due to the uncovered area generated by the silver nanowires crossing each other, There is a problem in manufacturing electrodes for solar cells and a film made of a network of silver nanowires has a problem of causing a short circuit in an electronic device due to a high surface roughness.
Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made keeping in mind the above problems occurring in the prior art, and it is an object of the present invention to provide a transparent electrode having silver nanowires excellent in electrical conductivity and light transmittance, A transparent electrode which can be replaced with an oxide electrode, and a manufacturing method thereof.
According to an aspect of the present invention, there is provided a transparent electrode comprising a substrate, a graphene layer formed on the substrate, and a silver (Ag) nanowire pattern layer formed on the graphene layer .
In addition, the substrate may be formed of glass, polyethylsulfone (PES), polyethylene phthalate (PET), polymethylmethacrylate, polystyrene (PS), cyclic olefin copolymer a cyclic olefin copolymer, a polyethylene naphthalate (PEN), and a polyimide.
Further, the graphene layer is formed by reduction of graphene oxide (GO).
Also, the transmittance of the silver nanowire pattern layer is controlled by adjusting the aperture ratio of the silver nanowire pattern layer by controlling the thickness of the silver nanowire forming the silver nanowire pattern layer and the gap between the neighboring silver nanowires.
(A) forming a graphene layer on a substrate, (b) forming a photoresist pattern on the surface of the graphene layer formed on the substrate, (c) ) Coating a silver nanowire solution on a graphene layer on which the photoresist pattern is formed to form a silver nanowire pattern layer, and (d) removing the photoresist pattern. .
In addition, the step (a) may be performed by using one method selected from among spin coating, dip coating, and zone casting to uniformly disperse the graphene oxide solution on the substrate And the graphene oxide is reduced by applying a reducing agent solution.
Also, the reducing agent solution may be at least one selected from the group consisting of hydrazine, hydrazine monohydrite, hydroquinone, dimethylhydrazine, phenylhydrazine, ethylenediamine, thionylchloride ) And sodium borohydride. ≪ / RTI >
In addition, the step (c) is characterized in that silver nanowires are coated using one method selected from spin coating, dip coating, and zone casting.
The step (c) may further include forming a titanium contact layer on the patterned graphene layer to facilitate coating of the silver nanowire.
A display device including a transparent electrode manufactured using the method for manufacturing a transparent electrode according to the present invention is proposed.
A photovoltaic device including a transparent electrode manufactured by the method of manufacturing a transparent electrode according to the present invention is proposed.
The transparent electrode according to the present invention includes a graphene layer and a silver nanowire pattern layer formed by reduction of graphene oxide and having a stable sp 2 hybrid carbon structure and excellent in electrical, thermal and mechanical properties, It is possible to secure a uniform transmittance over the entire surface of the transparent electrode as well as having excellent electrical conductivity and transparency to replace the transparent metal oxide electrode such as FTO and to control the aperture ratio at will.
In addition, the transparent electrode manufacturing method of the present invention can produce transparent electrodes at a low temperature and an atmospheric pressure state through solubilization in the entire process. Therefore, in addition to advantages such as reduction of manufacturing cost, simplification of the manufacturing process, It is possible to form transparent electrodes having the above-mentioned excellent characteristics on a flexible substrate such as a substrate, and thus can be usefully used in the production of various flexible devices.
1 is an image showing the structure of a transparent electrode including a graphene layer and a silver nanowire pattern layer formed by reduction of graphene oxide according to the present invention.
2 is a process diagram of a method for manufacturing a transparent electrode including a graphene layer and a silver nanowire pattern layer formed by reduction of graphene oxide according to the present invention.
3 is a conceptual diagram schematically showing a manufacturing process of a transparent electrode including a graphene layer and a silver nanowire pattern layer formed by reduction of graphene oxide according to the present invention.
FIG. 4 is an image of a transparent electrode element photographed by a scanning electron microscope (SEM) of a transparent electrode including a graphene layer and a silver nanowire pattern layer formed by reduction of graphene oxide according to the present invention.
5 is a graph showing the transmittance of a transparent electrode including a graphene layer and a silver nanowire pattern layer formed by reduction of graphene oxide according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, a detailed description of preferred embodiments of the present invention will be given with reference to the accompanying drawings.
In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.
Embodiments in accordance with the concepts of the present invention can make various changes and have various forms, so that specific embodiments are illustrated in the drawings and described in detail in this specification or application. It should be understood, however, that the embodiments according to the concepts of the present invention are not intended to be limited to any particular mode of disclosure, but rather all variations, equivalents, and alternatives falling within the spirit and scope of the present invention.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The singular expressions include plural expressions unless the context clearly dictates otherwise. In this specification, the terms "comprises ",or" having ", and the like, are intended to specify the presence of stated features, integers, steps, operations, elements, , Steps, operations, components, parts, or combinations thereof, as a matter of principle.
Hereinafter, a transparent electrode including a patterned silver nanowire and a reduced graphene oxide layer according to the present invention and a method of manufacturing the same will be described in detail.
A transparent electrode including a silver (Ag) nanowire pattern layer according to the present invention includes a substrate, a graphene layer formed on the substrate, and a silver (Ag) nanowire pattern layer formed on the graphene layer .
In order to manufacture the transparent electrode having the above-described structure, the substrate may be formed of glass, polyethylsulfone (PES), polyethylene phthalate, polymethylmethacrylate, polystyrene, PS ), Cyclic olefin copolymer, polyethylene naphthalate (PEN), polyimide, and the like can be used, and materials other than glass can be used to manufacture One transparent electrode has flexibility and can be manufactured as a flexible transparent substrate.
The graphene layer formed on the transparent substrate according to the present invention is preferably formed by reduction of graphene oxide (GO).
For reference, graphene is a collection of carbon atoms having a planar structure, having a two-dimensional thin film of a honeycomb structure composed of one layer or plural layers of carbon (C) atoms, and a single layer has a thickness of about 0.3 nm . Such graphene is metallic in nature, has conductivity in the layer direction, is excellent in thermal conductivity, and has high mobility of a carrier, so that a high-speed electronic device can be realized.
Further, the electron mobility of the graphene sheet made of graphene has a value of about 20,000 to 50,000 [cm 2 / Vs], excellent mechanical durability and chemical stability, and both semiconductor and conductor properties, Because of its thin thickness, it can be applied to flat panel display devices, transistors, energy storage devices and nano-sized electronic devices. Therefore, using graphene makes it easy to manufacture devices using semiconductor process technology. There is one advantage.
In addition, the present invention can vary the transmittance by controlling the aperture ratio of the silver nanowire pattern layer by controlling the thickness of the silver nanowire forming the silver nanowire pattern layer and the gap between neighboring silver nanowires, FIG. 1 is an image showing the structure of a transparent electrode including patterned silver nanowires and reduced graphene oxide according to the present invention, and the transparent electrode according to the present invention may be a transparent electrode having the stacked structure shown in FIG. 1 .
The transparent electrode according to the present invention described in detail above includes a graphene layer and a silver nanowire pattern layer formed by reduction of graphene oxide and having a stable sp 2 hybrid carbon structure and excellent in electrical, thermal and mechanical properties, It is possible to secure a uniform transmittance over the entire surface of the transparent electrode as well as to have excellent electrical conductivity and transparency enough to replace the conventional transparent metal oxide electrode such as ITO or FTO and to control the aperture ratio at will.
Therefore, the transparent electrode according to the present invention can be widely and usefully used for manufacturing a touch panel, a display device, a photovoltaic device, and a semiconductor device.
Next, a method of fabricating a transparent electrode including patterned silver nanowires and reduced graphene oxide according to the present invention will be described in detail in each step.
(A) forming a graphene layer on a substrate; (b) forming a graphene layer on the substrate, wherein the graphene layer is formed on the substrate, (C) forming a silver nanowire pattern layer by coating a silver nanowire solution on the graphene layer on which the photoresist pattern is formed, and (d) .
In the step (a), the graphene oxide solution is uniformly coated on the substrate by using a known wet coating method such as spin coating, dip coating and zone casting, A reducing agent solution is applied to reduce the graphene oxide to form a graphene layer.
At this time, as a method for uniformly coating the graphene oxide solution on the substrate, a known wet coating method such as spin coating, dip coating, and zone casting may be used, But is not limited thereto.
Also, the reducing agent solution may be at least one selected from the group consisting of hydrazine, hydrazine monohydrite, hydroquinone, dimethylhydrazine, phenylhydrazine, ethylenediamine, thionylchloride ), And sodium borohydride, but is not limited thereto.
For reference, since graphene oxide originally has many epoxy groups, hydroxyl groups, carboxyl groups, and the like, it is electrically insulative and can not be used as an electrode material in itself. However, the functional groups impart graphene oxide water- Therefore, it can be used as a preferable precursor in the production of graphene having excellent electrical conductivity through a reduction process.
In the step (b), a photoresist pattern is formed on the surface of the graphene layer formed on the substrate using a photo-resist.
In this step, unlike in the prior art in which metal nanowires are deposited directly on the substrate surface to form metal nanowire networks in which metal nanowires are randomly arranged, a photoresist solution is applied on the entire surface by a photolithography process The photoresist pattern is formed by fixing a mask having a back pattern and exposing it to ultraviolet rays to remove a developed portion, and silver nanowires are coated on the pattern thus formed to form silver nanowires as in the following step (c) Of the patterned layer.
Particularly, in this step, the pattern of the photoresist can be deformed by adjusting the shape and size of the opening of the mask used for the photolithography, so that the pattern of the photoresist pattern in the step (c) The thickness of the silver nanowire of the silver nanowire pattern layer formed by filling the silver nanowire through the wet coating or the like and the gap between the neighboring silver nanowires can be controlled so that the aperture ratio of the silver nanowire pattern layer The transmittance of the transparent electrode can be arbitrarily adjusted through adjustment.
Next, in step (c), a silver nanowire solution layer is coated on the graphene layer formed with the photoresist pattern to form a silver nanowire pattern layer. Specifically, as shown in FIG. 3, The silver nanowire dispersion formed by dispersing silver nanowires in a solvent such as distilled water, ethanol, or methanol is spin coated, dip coated, or zone cast on the photoresist pattern formed in step (b) or by a known wet coating method such as zone casting or the like.
At this time, it is preferable that silver nanowires used in this step have a length of 1 to 500 m, because when the length of the silver nanowires is less than 1 m, the number of contact points generated by the silver nanowires crossing each other increases, However, when the silver nanowire has a length exceeding 500 탆, the morphology of the silver nanowire is uneven, which may cause difficulties in controlling the light transmittance It is because.
Meanwhile, in this step, a step of forming a metal layer may be further performed to improve adhesion between the silver nanowire and the graphene layer prior to the coating of the silver nanowire solution. At this time, the metal constituting the metal layer may be titanium (Ti) , Tantalum (Ta), or an alloy thereof, but is not limited thereto.
Finally, in step (d), the photoresist pattern formed on the graphene layer for the formation of the silver nanowire pattern layer is removed, whereby the transparent electrode according to the present invention as shown in FIG. 4 is finally obtained Loses.
The method of manufacturing a transparent electrode according to the present invention has advantages such as reduction of manufacturing cost, simplification of manufacturing process, and easiness of large-sized transparent electrode because the transparent electrode can be manufactured at a low temperature and an atmospheric pressure state by solving the whole process.
Further, since the manufacturing method according to the present invention is performed by a solution process at room temperature / atmospheric pressure, it can be manufactured on a flexible plastic substrate, which is advantageous in that it can be applied to the production of a transparent electrode for a flexible device. That is, since the transparent electrode having excellent properties described above can be formed on a flexible substrate such as a plastic substrate, it can be advantageously used in the production of various flexible devices.
BRIEF DESCRIPTION OF THE DRAWINGS The invention will be described in detail below on the basis of embodiments. The presented embodiments are illustrative and are not intended to limit the scope of the invention.
<Examples>
First, a glass substrate prepared at 1.5 cm x 1.5 cm was sequentially sonicated using acetone, ethanol, isopropanol and deionized water (DI water) In each case for 10 minutes.
In order to impart hydrophilicity to the surface of the cleaned substrate, a plasma etching treatment was performed for 10 minutes at a power of 200 W while flowing oxygen at a rate of 4.0 sccm, followed by formation of a self-assembled monolayer (SAMs) To enhance the contact force between graphene oxide and the glass substrate, the substrate was immersed in 200 μl of 3-aminopropyltriethoxysilane (APTES) and 20 μl of isopropanol for 10 minutes to treat solid chemically self-assembled monolayer Respectively.
Then, graphene oxide was applied to the entire surface of the substrate having the self-assembled monolayer formed thereon by spin coating (500 rpm / 5 seconds or 2,500 rpm / 35 seconds) together with a hydrazine solution and then heat- Respectively.
Next, a photoresist (AZ.GXR-601) was applied by spin coating (500 rpm / 5 seconds or 5,500 rpm / 35 seconds) on the entire surface of the reduced graphene oxide layer formed as above, (MJB3) was fixed on the photoresist layer, exposed to UV for 8.6 seconds, developed with a developer for 30 seconds, and deionized water was applied to the surface of the photoresist layer, And the remaining photoresist was removed to form a lattice pattern having a line length of 15 mu m and a line-line spacing of 150 mu m, and plasma etching treatment was performed again for 1 minute under the same conditions as above, Lt; RTI ID = 0.0 > photoresist < / RTI >
Then, a 3 nm thick titanium adhesive layer was deposited on the reduced graphene oxide layer patterned with photoresist using an E-beam evaporator to improve the adhesion between the silver nanowire and the reduced graphene oxide layer After that, the silver nanowire-containing solution was applied by spin coating (500 rpm / 5 seconds or 1,000 rpm / 60 seconds) and heat-treated for 60 seconds on a hot plate at 100 ° C. Followed by cooling for 5 minutes to prepare a transparent electrode in which a reduced graphene oxide layer and a silver nanowire pattern layer were sequentially laminated on the substrate.
FIG. 5 is a graph showing the results of measurement of light transmittance for a transparent electrode including a silver nanowire pattern layer and a graphene layer manufactured in this embodiment, and shows excellent transmittance of 80% or more over the entire visible light wavelength region . The sheet resistance of the transparent electrode was measured. As a result, it was confirmed that the sheet had an excellent electrical conductivity of less than 100? / ?.
Claims (10)
(b) forming a photoresist pattern on the surface of the graphene layer formed on the substrate;
(c) forming a metal layer including titanium (Ti), tantalum (Ta), or an alloy thereof on the graphene layer having the photoresist pattern formed thereon;
(d) coating a silver nanowire solution on the metal layer formed on the graphene layer to form a silver nanowire pattern layer; And
(e) removing the photoresist pattern.
The step (a) may include uniformly coating the graphene oxide solution on the substrate using one of the methods selected from spin coating, dip coating and zone casting. And a reducing agent solution is applied to reduce the graphene oxide.
The reducing agent solution may be at least one selected from the group consisting of hydrazine, hydrazine monohydrite, hydroquinone, dimethylhydrazine, phenylhydrazine, ethylenediamine, thionylchloride, And at least one reducing agent selected from sodium borohydride.
Wherein the step (d) comprises coating the silver nanowire solution using one of a method selected from spin coating, dip coating and zone casting. Electrode.
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| KR101905801B1 (en) | 2017-04-06 | 2018-10-08 | 충남대학교산학협력단 | Direct Synthesis of Ag Nanowires on Graphene Layer |
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| KR101995096B1 (en) * | 2016-02-26 | 2019-07-01 | 한국과학기술원 | Transparent electrode using belt-shaped metal line embedded colorless transparent polyimide for OLED Display and process for manufacturing the same |
| WO2018004092A1 (en) | 2016-06-29 | 2018-01-04 | 한양대학교에리카산학협력단 | Nanostructure network and method for manufacturing same |
| KR102054553B1 (en) * | 2017-09-25 | 2019-12-10 | 주식회사 엘지화학 | Transparent electrode substrate and method for manufacturing thereof |
| KR102118777B1 (en) * | 2017-11-29 | 2020-06-03 | 순천대학교 산학협력단 | Tansparent electrode using graphene and nanowire and method for fabricating the same |
| CN108562219B (en) * | 2018-03-23 | 2022-10-25 | 南京邮电大学 | Flexible strain sensor and preparation method and application thereof |
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| JP2011154940A (en) | 2010-01-28 | 2011-08-11 | Konica Minolta Holdings Inc | Transparent pattern electrode, method of manufacturing the electrode, and organic electronic device using the electrode and its manufacturing method |
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| KR101124302B1 (en) | 2010-03-25 | 2012-03-27 | 주식회사 하이닉스반도체 | Fabrication Method of Dual Damascene Pattern for Semiconductor Device |
| KR101220421B1 (en) | 2010-06-15 | 2013-01-09 | (재)한국나노기술원 | Method of forming graphene pattern utilizing imprint |
| KR101207403B1 (en) | 2011-01-28 | 2012-12-04 | 한국생산기술연구원 | Silver nanowire ink using liquid-crystalline polymer and preparation method thereof |
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| KR101905801B1 (en) | 2017-04-06 | 2018-10-08 | 충남대학교산학협력단 | Direct Synthesis of Ag Nanowires on Graphene Layer |
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