KR20150001087A - Transparent electrode film and method for manufacturing thereof - Google Patents

Transparent electrode film and method for manufacturing thereof Download PDF

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Publication number
KR20150001087A
KR20150001087A KR1020130073758A KR20130073758A KR20150001087A KR 20150001087 A KR20150001087 A KR 20150001087A KR 1020130073758 A KR1020130073758 A KR 1020130073758A KR 20130073758 A KR20130073758 A KR 20130073758A KR 20150001087 A KR20150001087 A KR 20150001087A
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South Korea
Prior art keywords
transparent electrode
average roughness
transparent
graphene oxide
substrate
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KR1020130073758A
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Korean (ko)
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김운천
이진욱
신승주
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삼성전기주식회사
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Priority to KR1020130073758A priority Critical patent/KR20150001087A/en
Publication of KR20150001087A publication Critical patent/KR20150001087A/en

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • 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

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Manufacturing Of Electric Cables (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Non-Insulated Conductors (AREA)

Abstract

The present invention provides a transparent electrode film and a method for manufacturing a transparent electrode film using the same. Specifically, the transparent electrode film according to the present invention is a transparent electrode film which is formed by applying and reducing a transparent electrode layer on a substrate, preventing corrosion, deterioration and whitening during coating and curing of the transparent substrate, It is effective to strengthen the adhesive force of the adhesive layer.

Description

TECHNICAL FIELD [0001] The present invention relates to a transparent electrode film and a method of manufacturing the same,

The present invention relates to a transparent electrode film and a manufacturing method thereof.

The development of next-generation transparent electrode materials to replace indium tin oxide (ITO), which is currently used as a transparent electrode, is becoming increasingly important, and the development of transparent electrodes using carbon-based materials that are inexpensive and rich in raw materials is actively underway . Among them, attention is focused on the development of transparent electrodes using graphene, which is a two-dimensional conductor.

Conventionally, graphene is manufactured using a chemical vapor deposition (CVD) method at a high temperature of about 1000 캜 and transferred to a transparent film, or graphene oxide (GO), which is an insulator, is coated on the transparent film, The graphene oxide was reduced to form a reduced graphene oxide (rGO) as a conductor. However, the chemical vapor deposition method has disadvantages that it is costly to use expensive equipment and complicated processes, and mass production is difficult. The method using graphene oxide has a problem in that the transparent film is deteriorated or denatured by the reducing agent in the course of reduction, although the cost is low and mass production is possible by separating and separating graphite. In addition, there is a disadvantage that the adhesive strength with the transparent film is weak in the absence of additional overcoating.

On the other hand, although the transparent film using graphene oxide is disclosed in Patent Document 1, there is a problem in that the degradation phenomenon or whitening phenomenon caused by the reducing agent used when the graphene oxide is reduced can not be improved.

Patent Document 1: Korean Patent Publication No. 2012-0070973

In the present invention, a transparent electrode film having a transparent substrate and a transparent electrode layer, which is manufactured using the substrate to be removed, can prevent corrosion, deterioration and whitening of the transparent substrate, which occurs during reduction of graphene oxide, And the present invention has been completed on the basis thereof.

Accordingly, a first aspect of the present invention is to provide a transparent electrode film which does not exhibit corrosion, deterioration and whitening.

A second aspect of the present invention is to provide a method of manufacturing the transparent electrode film.

The transparent electrode film (hereinafter referred to as "first invention") for achieving the first aspect of the present invention comprises: a transparent substrate having a first average roughness (Ra 1 ) on its surface; And is formed on the surface of the transparent substrate, a second average roughness transparent electrode layer having a (Ra 2); has, characterized in that the first mean roughness (Ra 1) greater than said second average roughness (Ra 2) do.

In the first aspect of the present invention, the transparent substrate may be at least one selected from the group consisting of polymethylmethacrylate (PMMA), polyethyleneterephthalate (PET), polyethylenenaphthalate (PEN), polyetheretherketone (PEEK) Is selected from the group consisting of polycarbonate (PC), polyimide (PI), polyethersulfone (PES), polyarylite, and cyclic olefin copolymer (COC) do.

In the first invention, the first average roughness (Ra 1 ) is in the range of 10 to 20 nm, and the second average roughness (Ra 2 ) is in the range of 1 to 10 nm.

In the first invention, the transparent electrode layer is characterized by being reduced graphene oxide.

The method for manufacturing a transparent electrode film (hereinafter referred to as " second invention ") for achieving the second aspect of the present invention includes: forming a graphene oxide layer by applying an aqueous solution of graphene oxide on a substrate and then drying;

Reducing the graphene oxide layer to form a transparent electrode layer composed of a reduced graphene oxide layer;

Applying a transparent base solution on the transparent electrode layer to form a first average roughness (Ra 1 ) on a surface of the transparent base;

Curing the applied transparent substrate solution; And

And forming a second average roughness (Ra 2 ) on the transparent electrode layer by removing the substrate,

Here, larger than the first average roughness (Ra 1) and the second average roughness (Ra 2).

In the second invention, the substrate is not deteriorated by the reducing agent and is a material having low surface roughness, and is a material selected from the group consisting of a nonmetal such as a polymer, glass, a metal, a mixture thereof, and a compound thereof.

In the second invention, the graphene oxide aqueous solution or the transparent base solution is applied by spray coating, dip coating, spin coating, or slot die coating.

In the second aspect of the present invention, the graphene oxide layer may include at least one selected from the group consisting of hydrogen iodide (HI), hydrazine (N 2 H 4 ), potassium hydroxide (KOH), sodium hydroxide (NaOH), sodium sulfite (NA 2 SO 3 ) 2 ). ≪ / RTI >

In the second invention, the first average roughness (Ra 1 ) is in the range of 10 to 20 nm, and the second average roughness (Ra 2 ) is in the range of 1 to 10 nm.

In the second invention, the curing is carried out with a UV in the wavelength range of 340 to 380 nm.

In the second invention, the curing is performed with heat at a temperature ranging from 50 to 200 캜.

The transparent electrode film and the manufacturing method using the transparent electrode film according to exemplary embodiments of the present invention prevent corrosion, deterioration and whitening of the transparent material appearing in the process of applying and reducing the graphene oxide and improve the adhesion between the transparent electrode layer and the transparent material .

1 is a cross-sectional view of a transparent electrode film according to the present invention.
2 is an explanatory view showing a method of manufacturing a transparent electrode film according to the present invention.

Before describing the invention in more detail, it is to be understood that the words or words used in the specification and claims are not to be construed in a conventional or dictionary sense, It should be interpreted as meaning and concept consistent with the technical idea of the present invention. Therefore, the constitution of the embodiments described in the present specification is merely a preferred example of the present invention, and does not represent all the technical ideas of the present invention, so that various equivalents and variations And the like.

Hereinafter, preferred embodiments of the present invention will be described in detail so that those skilled in the art can easily carry out the present invention. In the following description, well-known functions or constructions are not described in detail since they would obscure the invention in unnecessary detail.

The transparent electrode film according to exemplary embodiments of the present invention may be formed by applying and drying a graphene oxide aqueous solution on a substrate, reducing the graphene oxide through a reducing agent to form a transparent electrode layer, And a transparent electrode layer formed on the surface of the transparent substrate and having a transparent electrode layer having a second average roughness (Ra 2 ), wherein the transparent electrode layer has a first average roughness Ra 1 on the surface thereof, An electrode film can be produced.

A transparent electrode film according to exemplary embodiments of the present invention includes a substrate having a graphene oxide layer formed thereon and then dried to form a graphene oxide layer, and the graphene oxide layer is reduced to form a reduced graphene oxide layer Forming a transparent electrode layer on the transparent electrode layer, applying a transparent base solution on the transparent electrode layer to form a first average roughness (Ra 1 ) on the transparent base material coated surface, curing the applied transparent base solution, And forming a second average roughness (Ra 2 ) on the transparent electrode layer by removing the substrate, wherein the first average roughness (Ra 1 ) is greater than the second average roughness (Ra 2 ) And a method for producing the same.

The substrate according to exemplary embodiments of the present invention may be selected from the group consisting of a non-metal such as a polymer and a glass, a metal, a mixture thereof, and a compound thereof, but is not limited to a material having a low surface roughness without being deteriorated by a reducing agent But a glass substrate can be generally used. It is preferable that the substrate is cleaned to remove impurities, and the cleaning may use both dry and wet cleaning.

The transparent electrode layer

The transparent electrode layer according to exemplary embodiments of the present invention is composed of reduced graphene oxide and has a thickness in the range of 1 to 20 nm in the transparent electrode film. If the thickness of the transparent electrode layer is less than 1 nm, the increase of the electrical conductivity may not actively progress. If the thickness exceeds 20 nm, the transmittance may fall below 80%, thereby failing to serve as a transparent electrode. Graphene oxide is a material to be applied to the transparent electrode layer. Graphite is oxidized in strong acid, then dispersed in water or an alcohol solvent, and graphene oxide, which is a graphene oxide, is separated through ultrasonic treatment.

The coating of the graphene oxide aqueous solution on the substrate can be performed by spray coating, dip coating, spin coating, or slot die coating. The coating solution is suitably a graphene oxide aqueous solution, Alcohol or a mixture of water and alcohol may be used.

The coated graphene oxide aqueous solution is dried and then formed with a reducing agent to form a reduced graphene oxide layer. The reducing agent hydroiodide the gas phase or liquid phase (HI), hydrazine (N 2 H 4), the group consisting of potassium hydroxide (KOH), sodium hydroxide (NaOH), sodium sulfite (NA 2 SO 3) and sulfur dioxide (SO 2) Or more.

Transparent substrate

The transparent substrate according to exemplary embodiments of the present invention may be formed of at least one selected from the group consisting of polymethylmethacrylate (PMMA), polyethyleneterephthalate (PET), polyethylenenaphthalate (PEN), polyetheretherketone (PEEK) Polycarbonate (PC), polyimide (PI), polyethersulfone (PES), polyarylite, and cyclic olefin copolymer (COC) Typically, polyethylene terephthalate is used.

The transparent substrate is applied on a transparent electrode layer having a first average roughness Ra 1 formed in a solution state, for example, by any one of spray coating, dip coating, spin coating, slot die coating, Can be applied. In addition, the transparent base solution may permeate between the reduced graphene oxide forming the transparent electrode layer before the curing step. Then, when the transparent substrate is cured by heat or UV, physical anchoring is formed between the transparent substrate and the transparent electrode layer impregnated with the transparent substrate solution, thereby enhancing the adhesive strength.

The curing may be carried out with a UV in the wavelength range of 340 to 380 nm. If the wavelength is less than 340 nm, the curing time may be prolonged. If the wavelength exceeds 380 nm, the physical properties may be deteriorated due to rapid curing.

The curing may be performed in a temperature range of 50 to 200 ° C. If the temperature is less than 50 ° C, the curing time may be prolonged. If the temperature is more than 200 ° C, the physical properties of the transparent base material may be changed due to strong heat.

When the curing reaction is completed, the substrate is removed to obtain a final transparent electrode film.

1, the transparent electrode film 200 according to a representative embodiment of the present invention is composed of a transparent substrate 21 and a transparent electrode layer 13, and the transparent substrate 21 and the transparent electrode layer 13, between a first average roughness (Ra 1) is formed, and is formed with a second average roughness (Ra 2) formed on the transparent electrode layer (13). Also, the first average roughness (Ra 1) is from 10 to 20㎚ range, wherein the second average roughness (Ra 2) in the range of 1 to 10㎚, the first average roughness (Ra 1) a second Is always larger than the average roughness (Ra 2 ). If the first average roughness (Ra 1 ) is less than 10 nm, the adhesive force may be weakened, and if it exceeds 20 nm, the permeability may be deteriorated. If the second average roughness (Ra 2 ) is less than 1 nm, separation on the substrate may not be free, and if it exceeds 10 nm, the permeability may be deteriorated.

Meanwhile, unlike the conventional transparent electrode film, the transparent electrode film manufactured according to the exemplary embodiment of the present invention can prevent the transparent substrate from being corroded, deteriorated and whitened due to the reducing agent. Conventionally, there is a problem that when a transparent electrode layer is formed on a transparent substrate, the transparent substrate is corroded or deteriorated by heat generated during reduction, thereby causing a bleaching phenomenon. However, as shown in FIG. 2, the transparent electrode film prepared according to the present invention is formed by applying and drying a graphene oxide aqueous solution 11 on a substrate 100, drying the graphene oxide aqueous solution 11 ) To form a transparent electrode layer 13. Then, a transparent base material solution is applied and cured on the transparent electrode layer 13 to form a transparent substrate 21, and the substrate 100 is removed, so that corrosion of the transparent substrate, which occurs during reduction of the graphene oxide, The transparent electrode film 200 that can prevent deterioration and whitening can be manufactured.

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples are not intended to limit the scope of the present invention.

Example 1

The glass substrate was immersed in a solution of sulfuric acid (H 2 SO 4 : 95 to 97%, MERCK) and hydrogen peroxide (H 2 O 2 : 30%, JUNSEI) in a ratio of about 7: 3 at about 110 ° C. for 1 hour Respectively. The graphene oxide aqueous solution was mixed with ethanol (ACS Reagent, JT Baker) at a ratio of about 1: 1, spray coated on the cleaned glass substrate, and dried to obtain uniform graphene oxide of about 10 to 20 nm, .

Approximately 3 mL of a hydrazine solution (N 2 H 4 : 98%, SIGMA ALDRICH) was dropped on the graphene oxide formed on the glass substrate and maintained at about 110 ° C on a hot plate for about 30 minutes to remove the chemical And a transparent electrode layer was fabricated through this. Then, a PET solution was poured onto the transparent electrode layer and cured at a temperature of about 145 캜 for 1 hour on a hot plate to form a transparent substrate and separated from the substrate to prepare a transparent electrode film.

It is confirmed that the transparent electrode film exhibits the effect of preventing the corrosion, deterioration and bleeding phenomenon in the process of applying and reducing the transparent electrode layer and applying and curing the transparent substrate, and strengthening the adhesion between the transparent electrode layer and the transparent substrate there was.

Example 2

The glass substrate was immersed in a solution of sulfuric acid (H 2 SO 4 : 95 to 97%, MERCK) and hydrogen peroxide (H 2 O 2 : 30%, JUNSEI) in a ratio of about 7: 3 at about 110 ° C. for 1 hour Respectively. The graphene oxide solution was mixed with ethanol (ACS Reagent, JT Baker) at a ratio of about 1: 1, spray-coated on the cleaned glass substrate and dried to obtain uniform graphene oxide of about 10 to 20 nm, .

Approximately 3 mL of a hydrazine solution (N 2 H 4 : 98%, SIGMA ALDRICH) was dropped on the graphene oxide formed on the glass substrate and maintained at about 110 ° C on a hot plate for about 30 minutes to remove the chemical And a transparent electrode layer was fabricated through this. Then, a PET solution was poured onto the transparent electrode layer and cured at a UV wavelength of about 365 nm for 20 seconds to form a transparent substrate and separated from the substrate to prepare a transparent electrode film.

Through Examples 1 and 2, it was visually confirmed that the transparent electrode film of the present invention was able to prevent corrosion, deterioration and whitening of the transparent substrate, which occurs in the process of applying and reducing graphene oxide, Physical anchoring between the electrode layer and the transparent substrate was formed, and the effect of improving the adhesion was confirmed.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, the same is by way of illustration and example only and is not to be construed as limiting the present invention. It is obvious that it can be modified or improved.

It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.

11: graphene oxide aqueous solution 13: transparent electrode layer
21: transparent substrate 100: substrate
200: transparent electrode film

Claims (11)

A transparent substrate having a first average roughness (Ra 1 ) on its surface; And
Is formed on the surface of the transparent substrate, a second transparent electrode layer has a mean roughness (Ra 2); it has a,
Here, the first average roughness Ra 1 is larger than the second average roughness Ra 2 .
The method according to claim 1,
The transparent substrate may be formed of a material selected from the group consisting of polymethylmethacrylate (PMMA), polyethyleneterephthalate (PET), polyethylenenaphthalate (PEN), polyetheretherketone (PEEK), polycarbonate (PC) Wherein the transparent electrode film is selected from the group consisting of polyimide (PI), polyethersulfone (PES), polyarylite, and cyclic olefin copolymer (COC).
The method according to claim 1,
It said first average roughness (Ra 1) is from 10 to 20㎚ range, wherein the second average roughness (Ra 2) a transparent electrode film, characterized in that from 1 to 10㎚ range.
The method according to claim 1,
Wherein the transparent electrode layer is reduced graphene oxide.
Applying a graphene oxide aqueous solution on the substrate and then drying to form a graphene oxide layer;
Reducing the graphene oxide layer to form a transparent electrode layer composed of a reduced graphene oxide layer;
Applying a transparent base solution on the transparent electrode layer to form a first average roughness (Ra 1 ) on a surface of the transparent base;
Curing the applied transparent substrate solution; And
And forming a second average roughness (Ra 2 ) on the transparent electrode layer by removing the substrate,
Here, the first average roughness Ra 1 is larger than the second average roughness Ra 2 .
The method of claim 5,
Wherein the substrate is not deteriorated by a reducing agent but is a material having a low surface roughness and is a material selected from the group consisting of a nonmetal such as polymer, glass, a metal, or a mixture or compound thereof.
The method of claim 5,
Wherein the graphene oxide aqueous solution or the transparent base solution is applied by spray coating, dip coating, spin coating, or slot die coating.
The method of claim 5,
The graphene oxide layer is from the group consisting of hydrogen iodide (HI), hydrazine (N 2 H 4), potassium hydroxide (KOH), sodium hydroxide (NaOH), sodium sulfite (NA 2 SO 3) and sulfur dioxide (SO 2) Wherein the reducing agent is reduced to one or more selected reducing agents.
The method of claim 5,
It said first average roughness (Ra 1) 10 to a 20㎚ range, wherein the second average roughness (Ra 2) The manufacturing method of the transparent electrode film, characterized in that from 1 to 10㎚ range.
The method of claim 5,
Wherein the curing is performed with a UV in a wavelength range of 340 to 380 nm.
The method of claim 5,
Wherein the curing is performed in a temperature range of 50 to 200 캜.
KR1020130073758A 2013-06-26 2013-06-26 Transparent electrode film and method for manufacturing thereof KR20150001087A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017028239A (en) * 2015-07-24 2017-02-02 現代自動車株式会社Ｈｙｕｎｄａｉ Ｍｏｔｏｒ Ｃｏｍｐａｎｙ Collector electrode protection film for dye-sensitized solar cell, method of forming the same, and dye-sensitized solar cell including the same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017028239A (en) * 2015-07-24 2017-02-02 現代自動車株式会社Ｈｙｕｎｄａｉ Ｍｏｔｏｒ Ｃｏｍｐａｎｙ Collector electrode protection film for dye-sensitized solar cell, method of forming the same, and dye-sensitized solar cell including the same

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