WO2013009056A2 - Électrode transparente contenant du graphène et de l'oxyde d'étain et d'indium (ito) - Google Patents
Électrode transparente contenant du graphène et de l'oxyde d'étain et d'indium (ito) Download PDFInfo
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- WO2013009056A2 WO2013009056A2 PCT/KR2012/005422 KR2012005422W WO2013009056A2 WO 2013009056 A2 WO2013009056 A2 WO 2013009056A2 KR 2012005422 W KR2012005422 W KR 2012005422W WO 2013009056 A2 WO2013009056 A2 WO 2013009056A2
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J29/00—Details of cathode-ray tubes or of electron-beam tubes of the types covered by group H01J31/00
- H01J29/02—Electrodes; Screens; Mounting, supporting, spacing or insulating thereof
- H01J29/08—Electrodes intimately associated with a screen on or from which an image or pattern is formed, picked-up, converted or stored, e.g. backing-plates for storage tubes or collecting secondary electrons
- H01J29/085—Anode plates, e.g. for screens of flat panel displays
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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
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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
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
Definitions
- the present invention relates to a transparent electrode containing graphene and ITO.
- the transparent electrode is a functional thin film electrode that transmits light in the visible light region and has electrical conductivity, and is widely used as an electrode substrate for flat panel displays, touch panels, and solar cells.
- Examples of the conductive material that can be used for the transparent electrode include metals, metal oxides, conductive polymers, and carbon materials.
- Metal materials, such as silver and copper, are excellent in conductivity, but they are not preferable because they are low in permeability even when produced in a thin film.
- a representative example of the metal oxide conductive material is indium tin oxide (ITO), and such indium tin oxide is most widely used as a transparent electrode material because of excellent transmittance and low resistance value.
- ITO indium tin oxide
- the price of indium, the main raw material of ITO has risend, and the high cost of equipment such as vacuum deposition equipment is required for the production of ITO thin films (electron beam deposition, sputtering, laser deposition, etc.).
- the advantage of the conductive polymer electrode is that it is much more flexible and less brittle than the ITO electrode, so the mechanical stability when bent or folded is very good.
- the conductive polymer absorbs light in the visible light region, when the polymer film is thickly coated to obtain proper sheet resistance, the visible light transmittance of the electrode is sharply deteriorated.
- the thinning process is difficult, and the applicable process temperature is low.
- Graphene which is a kind of carbon material, has excellent electrical conductivity and adhesive stability with a substrate, and has a small deformation due to thermal expansion, but is difficult to manufacture in large areas.
- An object of the present invention is to provide a low-cost transparent electrode that is low in surface resistance and can be manufactured in large areas while solving the problems of the prior art.
- the present invention provides a transparent electrode comprising a graphene and ITO.
- the graphene and ITO is present in the form of a nanocomposite, and the peak size of In 2 O 3 (222) in the nanocomposite by XRD analysis is 1.5 to 1.8 times larger than the peak size of single ITO grains. desirable.
- the sheet resistance of the transparent electrode is preferably in the range of 300 to 3000 ⁇ / sq.
- the graphene and ITO is preferably prepared by a solution process.
- the graphene is obtained by reducing the graphene oxide prepared by the Hummus method, the reducing method is i) a method of reducing using para phenylene diamine, hydrazine hydrate, or both; And ii) it is preferable to use at least one method selected from the group consisting of a reduction method using heat.
- the ITO is preferably a sol-gel solution
- the sol-gel solution is (a) indium nitrate hydrate and tin chloride in a molar fraction of 8 to 10: 1 dissolved in a solvent, tin chloride Preparing a mixed solution of 0.02 to 0.1 M based on the molar concentration of; and (b) sol-gelling the mixed solution obtained in step (a) for 2 to 5 hours. It may be.
- the transparent electrode according to the present invention can be manufactured at low cost, low surface resistance while maintaining transmittance, and can be manufactured in a large area.
- a transparent electrode such as a solar cell, a touch panel, an organic light emitting diode, there is a high efficiency and low power effect.
- FIG. 2 is a graph showing the ITO transparent electrode sheet resistance of Preparation Example 2 according to the molarity (Molarity) of the tin chloride and rpm of the spin coating.
- FIG 3 is a graph showing the light transmittance of the ITO transparent electrode of Preparation Example 2 in the visible light region (400 to 900nm) according to the molarity of tin chloride.
- Example 5 is a graph showing the light transmittance of the transparent electrode of Example 4 heat-treated at 500 °C.
- FIG. 6 is a view of the surface of the transparent electrode of Example 4 heat-treated at 500 ° C. using a field emission scanning electron microscope (FE-SEM).
- FE-SEM field emission scanning electron microscope
- Example 7 is an EDS graph of the transparent electrode surface of Example 4 heat-treated at 500 ° C.
- Example 8 is an XRD graph of the transparent electrode of Example 4 heat-treated at 500 ° C.
- Fig. 9 is a cross sectional view of an OLED manufactured in Example 4.
- FIG. 10 is a graph showing current density-voltage curves of OLEDs having transparent electrodes manufactured in Examples 1 to 3 and Comparative Example 1, respectively.
- glass substrate 2 transparent electrode
- the present invention is a transparent electrode characterized in that it contains graphene and ITO.
- Graphene refers to a two-dimensional plate-shaped nanostructure in which graphite is formed in one layer or a plurality of layers. Such graphene may be prepared by various methods known in the art, and is not particularly limited. High ordered pyrolytic graphite (HOPG) flakes, chemical reduction of graphite oxide flakes, epitaxial growth, chemical vapor deposition, thermal exfoliation, electrostatic deposition Electrostatic deposition, liquid phase expoliation of graphite, arc discharging, solvent thermal synthesis, etc. are known for use in graphene production.
- HOPG High ordered pyrolytic graphite
- a graphene production method using a solution process which is inexpensive, is preferable.
- Methods using the solution process include chemical reduction of graphite oxide flakes, graphite liquid flakes, solvent thermal synthesis, and the like.
- One preferred embodiment for preparing graphene using a solution process is as follows. After preparing graphene oxide (GO) by a process known as the Hummers method, it is finally reduced by heat and / or an amine group-containing compound (paraphenylene diamine, hydrazine hydrate, etc.). You get graphene. As described in Preparation Example 1-1, a method of preparing graphene by reducing graphene oxide using a Hummus method and a compound uses a solution process.
- ITO Indium tin oxide
- examples of the method for producing ITO include an electron beam deposition method, a sputtering method, a laser deposition method, a method synthesized using a solution process.
- the indium source and the tin source may use any conventional compound known in the art without limitation.
- the indium source may be an indium nitrate hydrate (In (NO 3 ) 3 ).
- ITO indium nitrate hydrate (In (NO 3 ) 3 .xH 2 O) and tin chloride (SnCl 2 ) may be mixed and dissolved in a solvent (ethanol, etc.) and then sol-gelled to prepare an ITO solution.
- a solvent ethanol, etc.
- the mole fraction of the indium source and the tin source is not particularly limited.
- the mole fraction may be in the range of 8 to 10: 1 (mole fraction), and preferably 9: 1.
- the mixed solution in which the indium source and the tin source are dissolved in the solvent may be 0.02 to 0.1M based on the molar concentration of tin chloride, but is not particularly limited thereto.
- the method for producing the transparent electrode of the present invention using the graphene and ITO described above is various, and is not particularly limited. In consideration of the manufacturing cost, it is preferable to manufacture a transparent electrode using graphene and ITO prepared by using a solution process.
- An example of preparing a transparent electrode using graphene (Preparation Example 1) prepared through a solution process and ITO (Preparation Example 2) prepared through a solution process is described in Example 1 below.
- the melting points of In and Sn are 156.63 ° C and 231.93 ° C, respectively.
- the heat treatment temperature since the transparent electrode is manufactured using a solution process, the heat treatment temperature must be higher than their melting point so that In and Sn are mixed with each other to form a solution process. Accordingly, in the transparent electrode manufacturing method of the present invention, the heat treatment temperature may be 250 °C or more, which can be appropriately adjusted according to the experimental conditions.
- the heat treatment temperature may be in the range of 250 to 600 ° C. under atmospheric conditions, and may be in the range of 250 to 1000 ° C. under inert atmosphere.
- the heat treatment time may be appropriately adjusted within a conventional range in consideration of the sheet resistance value of the transparent electrode, and may be, for example, in the range of 1 minute to 3 hours.
- the transparent electrode heat-treated at 500 ° C. showed the lowest sheet resistance (see FIG. 4), and exhibited low sheet resistance even in the range of 500 to 600 ° C.
- FIG. Increasing temperature increases the crystallization of In and Sn due to the high energy, so that the sheet resistance value may be low.
- the transparent electrode of the present invention manufactured using the above-described graphene and ITO has a sheet resistance value in the range of 300 to 3000 ⁇ / sq and a light transmission characteristic of 80% or more. This excellent electrical conductivity and light transmittance can be usefully applied to flat panel displays, touch panels, solar cells, and the like.
- An example of applying a transparent electrode manufactured using graphene and ITO to an organic electroluminescent device (OLED) is described in Example 4 below.
- FIG. 1 shows graphene oxide (GO) prepared in Preparation Example 1-1, graphene reduced using phenylene diamine in Preparation Example 2-1 (PPD-rGO), and hydrazine hydrate in Preparation Example 2-2.
- the G peak generally generated in the graphite-based material appears in the region around 1580 cm ⁇ 1 , and the G peak of graphene oxide (GO) has a peak shift up to 1600 cm ⁇ 1 . It is assumed that the peak shift occurred due to the attachment of oxygen functional groups.
- the G peaks of PPD-rGO of Preparation Example 2-1 and HYD-rGO of Preparation Example 2-2 showed peaks around 1580 cm ⁇ 1 , confirming that the oxygen functional groups were dropped and reduced.
- the G peak is a peak named after G, which is the first letter of graphite, and is a peak common in carbon-containing materials, and the D peak represents a degree of deficiency.
- the ratio of the D peak and the G peak is the definitive evidence that the defect increases when the graphene oxide is reduced to graphene, resulting in an increase in defects.
- D peak size of graphene oxide (GO) prepared in Preparation Example 1-1 was 0.66 compared to the G peak size.
- the D peak size of the graphene (PPD-rGO) prepared in Preparation Example 2-1 was 0.90 compared to the G peak size
- the D peak size of the graphene (HYD-rGO) prepared in Preparation Example 2-2 was It was found to be 0.83.
- the ratio of the D peak to the G peak was increased, indicating that reduction of graphene oxide to graphene proceeded.
- Indium nitrate hydrate (In (NO 3 ) 3 xH 2 O) and tin chloride (SnCl 2 ) were mixed in a molar fraction of 9: 1 ratio and dissolved in ethanol, and then 0.02 based on the molarity of tin chloride (Molarity). , 0.03, 0.035, 0.04, 0.1M solutions were prepared and sol-gelled for 3 hours to prepare ITO solutions.
- the prepared ITO solution was spin coated on a glass substrate for 20 seconds at 1000, 2000, and 5000 rpm speeds, respectively.
- the thicknesses of the prepared ITO layer (transparent electrode) were 130 nm, 60 nm and 45 nm, respectively.
- the prepared ITO transparent electrode was heat-treated at 500 ° C. for 3 hours, and the sheet resistance and the light transmittance were measured using a 4-terminal probe and a UV / vis spectroscope, respectively.
- Figure 2 shows the change in the surface resistance of the ITO layer according to the molarity (Molarity) of the tin chloride and rpm during spin coating.
- Molarity molarity of the tin chloride
- the sheet resistance of the transparent electrode manufactured by spin coating at 3000 rpm was the lowest at about 2000 ⁇ s / sq. However, it was higher than 50 to 500 kW / sq, which is a general sheet resistance of the ITO transparent electrode manufactured by sputtering.
- Figure 3 shows the change in light transmittance in the visible region (400 ⁇ 900nm) according to the molarity of tin chloride (Molarity). It can be seen that all the manufactured transparent electrodes transmit more than 85% in the visible light region. Considering that the transmittance of the commercialized ITO transparent electrode is 80 to 90, it can be seen that all the prepared transparent electrodes are excellent in the light transmitting surface.
- 0.1 mg of the graphene oxide prepared in Preparation Example 1-1 was mixed with 1 ml of the ITO sol-gel solution prepared in Preparation Example 2 (the ITO solution prepared at 0.03 M based on tin molal chloride concentration) and dispersed using ultrasonic waves. .
- the dispersion solution was spin-coated on the washed glass substrate. After the heat treatment at 100 to 500 °C additionally to prepare a transparent electrode (GO + ITO).
- the transparent electrode prepared in Example 1 was used as an OLED anode at a heat treatment temperature of 500 ° C.
- the anode was patterned, and the OLED was fabricated by laminating in order of a hole injection layer, a light emitting layer, an electron injection layer, and a cathode using a thermal vacuum deposition machine.
- ⁇ -NPD (4'-bis [N- (1-naphtyl) -N-phenyl-amino] biphenyl) 70 nm as hole injection layer, Alq 3 (tris (8-hydroxyquinoline) aluminum) 60 nm as emission layer, electron injection layer LiF 10 nm, 80 nm aluminum was vacuum deposited by the cathode.
- a transparent electrode (ITO) was prepared by using the ITO sol-gel solution of Preparation Example 2 alone without using the graphene oxide prepared in Preparation Example 1-1.
- the transparent electrodes of Examples 1 to 3 manufactured by using graphene oxide or graphene and ITO in combination with the ITO alone transparent electrode of Comparative Example 1 had low sheet resistance.
- the surface resistance value is the lowest when the heat treatment temperature is 500 °C, it is estimated to have the lowest surface resistance value at 500 ⁇ 600 °C.
- Figure 5 shows the change in the light transmittance of the transparent electrode prepared at a heat treatment temperature of 500 ° C.
- FIG. 6 is an image of the surface of the transparent electrode manufactured by heat treatment at 500 ° C., observed with a field emission scanning electron microscope (FE-SEM).
- FE-SEM field emission scanning electron microscope
- the transparent electrodes of Examples 1 to 3 including graphene have increased grain size and thus have improved electrical conductivity.
- the EDS (Energy Dispersive Spectrometer) data of FIG. 7 also showed that the carbon peak of the transparent electrode including graphene was larger than that of the ITO transparent electrode. This confirmed that graphene is included.
- FIG. 8 shows XRD data of a transparent electrode manufactured at a heat treatment temperature of 500 ° C.
- In 2 O 3 (222) peaks were observed in XRD data of all the prepared transparent electrodes.
- the peak size of Example 1 (GO + ITO) is 1.75
- the peak size of Example 2 (PPD-rGO + ITO) is 1.7
- Example 3 HYD-rGO + ITO.
- the peak size was calculated as 1.6.
- Increasing the size of the In 2 O 3 (222) peak as described above means that the crystallization is well, it means that the crystallization and grain growth of ITO was affected by the addition of graphene. This means that the addition of graphene had an effect on improving the conductivity of the transparent electrode.
- Example 1 GO + ITO
- Example 2 PPD-rGO + ITO
- Example 3 HYD-rGO + It can be seen that the power of the OLED having the transparent electrode manufactured in ITO) is lower. More specifically, the OLED using the transparent electrode of Example 3 (HYD-rGO + ITO) has an operating voltage at 23.8V at 30 mA / cm 2 compared to the OLED using the transparent electrode of Comparative Example 1 (ITO). Significantly reduced to 14.2V.
- Table 1 shows the luminous efficiency of the manufactured OLED.
- Comparative Example 1 (ITO) light intensity (luminance) is 7,500 cd / m 2
- Example 3 (HYD-rGO + ITO of the OLED that uses a transparent electrode is at a current density of 90 mA / cm 2 OLED using the transparent electrode of 1) showed 11,000 cd / m 2 . Therefore, it was found that the light efficiency increased by 1.46 times when ITO and graphene were mixed.
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Abstract
La présente invention propose une électrode transparente contenant du graphène et de l'oxyde d'étain et d'indium (ITO). Selon la présente invention, une électrode transparente bon marché, ayant une faible résistance de surface tout en conservant une transmittance et apte à être fabriquée pour recouvrir une large zone de surface, peut être obtenue.
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CN110491547A (zh) * | 2019-08-22 | 2019-11-22 | 朱萍 | 一种导电材料及其制备工艺 |
CN116004041A (zh) * | 2023-02-13 | 2023-04-25 | 河北科技大学 | 一种钛双极板涂层材料的制备方法及应用 |
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CN103741094A (zh) * | 2014-01-22 | 2014-04-23 | 武汉理工大学 | 石墨烯复合导电氧化物靶材及其透明导电薄膜的制备方法 |
KR102384945B1 (ko) | 2015-01-02 | 2022-04-08 | 삼성디스플레이 주식회사 | 유기 발광 표시 장치 및 그의 제조 방법 |
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JP2010282729A (ja) * | 2009-06-02 | 2010-12-16 | Hitachi Ltd | 透明導電性膜およびそれを用いた電子デバイス |
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KR20100094224A (ko) * | 2009-02-18 | 2010-08-26 | 전북대학교산학협력단 | 태양전지 및 이의 제조방법 |
JP2010282729A (ja) * | 2009-06-02 | 2010-12-16 | Hitachi Ltd | 透明導電性膜およびそれを用いた電子デバイス |
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CN110491547A (zh) * | 2019-08-22 | 2019-11-22 | 朱萍 | 一种导电材料及其制备工艺 |
CN110491547B (zh) * | 2019-08-22 | 2023-01-17 | 朱萍 | 一种导电材料及其制备工艺 |
CN116004041A (zh) * | 2023-02-13 | 2023-04-25 | 河北科技大学 | 一种钛双极板涂层材料的制备方法及应用 |
CN116004041B (zh) * | 2023-02-13 | 2024-05-28 | 河北科技大学 | 一种钛双极板涂层材料的制备方法及应用 |
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WO2013009056A3 (fr) | 2013-03-07 |
KR20130007833A (ko) | 2013-01-21 |
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