KR101706963B1 - Method for manufacturing graphene hybrid electrode - Google Patents

Method for manufacturing graphene hybrid electrode Download PDF

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Publication number
KR101706963B1
KR101706963B1 KR1020150052902A KR20150052902A KR101706963B1 KR 101706963 B1 KR101706963 B1 KR 101706963B1 KR 1020150052902 A KR1020150052902 A KR 1020150052902A KR 20150052902 A KR20150052902 A KR 20150052902A KR 101706963 B1 KR101706963 B1 KR 101706963B1
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South Korea
Prior art keywords
graphene
transparent conductive
composite electrode
conductive oxide
layer
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KR1020150052902A
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Korean (ko)
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KR20160122977A (en
Inventor
문진산
박수범
박원배
홍병희
조인수
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엘지전자 주식회사
서울대학교산학협력단
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Priority to KR1020150052902A priority Critical patent/KR101706963B1/en
Priority to US15/563,087 priority patent/US10497893B2/en
Priority to EP16780306.3A priority patent/EP3284718B1/en
Priority to CN201680021660.5A priority patent/CN107635918B/en
Priority to PCT/KR2016/003910 priority patent/WO2016167583A1/en
Publication of KR20160122977A publication Critical patent/KR20160122977A/en
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Publication of KR101706963B1 publication Critical patent/KR101706963B1/en

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof  ; Multistep manufacturing processes therefor
    • H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
    • H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
    • H01L29/16—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only elements of Group IV of the Periodic System
    • H01L29/1606—Graphene

Abstract

The present invention relates to graphene, and more particularly, to a method for producing a graphene composite electrode using graphene and an inorganic material. The present invention provides a method for producing a graphene composite electrode, comprising: forming graphene on a catalyst metal; Forming a transparent conductive oxide on the graphene; Crystallizing the transparent conductive oxide by applying heat of at least 150 ° C; And transferring the composite electrode composed of the graphene and the transparent conductive oxide to a final substrate.

Description

TECHNICAL FIELD The present invention relates to a method for manufacturing a graphene hybrid electrode,

The present invention relates to graphene, and more particularly, to a method for producing a graphene composite electrode using graphene and an inorganic material.

As materials composed of carbon atoms, fullerene, carbon nanotube, graphene, graphite and the like exist. Among them, graphene is a structure in which carbon atoms are composed of one layer on a two-dimensional plane.

In particular, graphene is not only very stable and excellent in electrical, mechanical and chemical properties, but it is also a good conductive material that can move electrons much faster than silicon and can carry much larger currents than copper, It has been proved through experiments that a method of separation has been discovered.

Such graphene can be formed in a large area and has electrical, mechanical and chemical stability as well as excellent conductivity, and thus is attracting attention as a basic material for electronic circuits.

In addition, since graphenes generally have electrical characteristics that vary depending on the crystal orientation of graphene of a given thickness, the user can express the electrical characteristics in the selected direction and thus design the device easily. Therefore, graphene can be effectively used for carbon-based electric or electromagnetic devices.

In general, applications such as display devices require transparent electrodes. In order to maintain the properties required for such transparent electrodes, a very thick transparent conductive oxide film is used.

However, such a thick transparent electrode may be unsuitable for use in a process for depositing on a plastic substrate for producing a flexible device and a display, and may also be unsuitable in terms of transparency and low surface roughness, and an alternative thereto is required.

SUMMARY OF THE INVENTION The present invention provides a method of manufacturing a graphene composite electrode using graphene and a transparent conductive layer.

It is another object of the present invention to provide a method of manufacturing a graphene composite electrode that can reduce the thickness of an electrode and can be applied to a flexible device and a display.

According to an aspect of the present invention, there is provided a method of manufacturing a graphene composite electrode, comprising: forming graphene on a catalyst metal; Forming a transparent conductive oxide on the graphene; Crystallizing the transparent conductive oxide by applying heat of at least 150 ° C; And transferring the composite electrode composed of the graphene and the transparent conductive oxide to a final substrate.

Here, the step of forming graphene may further include doping the graphene.

Here, the crystallization may be performed at a temperature of 150 ° C to 400 ° C.

Here, the transparent conductive oxide may include at least one of ITO, IZO, ZnO, GZO, and AZO.

Here, the transferring step may include: positioning a supporting layer on the transparent conductive oxide; Removing the catalyst metal; Attaching the composite electrode to the final substrate; And removing the support layer.

In addition, the transferring step may include: forming the final substrate on the transparent conductive oxide; And removing the catalyst metal.

Here, the final substrate may be a polymer substrate.

The method may further include forming an organic EL layer on the graphene.

The present invention has the following effects.

First, the transparent conductive layer formed on the graphenes can form a transparent composite electrode. That is, a transparent composite electrode having a low resistance value can be formed through an organic / inorganic hybrid of graphene and an ITO layer.

Such a composite electrode can be directly applied to a sputtering method which is currently used in industry, thereby reducing the amount of ITO used to one fifth. This is because, due to the composite electrode, a condition that can be used as a transparent electrode can be satisfied even if it is formed in a small thickness.

Further, the ITO layer can simultaneously serve as a protective film of the graphene. If graphene is doped, the effect of such doping may be made longer.

On the other hand, flexible transparent electrodes can be fabricated through a hybrid of graphene and an ITO layer, which are two-dimensional materials. That is, since the composite electrode can have conductivity and flexibility at the same time, it is possible to overcome the limitations of the flexible display, which was impossible with only the ITO layer.

As described above, the present process can be directly applied to the ITO roll-to-roll process and can be applied together with the roll-to-roll-based graphene process.

1 is a flow chart showing an example of a method for producing a graphene composite electrode.
Figs. 2 to 9 are cross-sectional schematic views showing respective steps of manufacturing the graphene composite electrode.
10 is a schematic view showing a process of forming a transparent conductive layer.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings.

While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail. Rather, the intention is not to limit the invention to the particular forms disclosed, but rather, the invention includes all modifications, equivalents and substitutions that are consistent with the spirit of the invention as defined by the claims.

It will be appreciated that when an element such as a layer, region or substrate is referred to as being present on another element "on," it may be directly on the other element or there may be an intermediate element in between .

Although the terms first, second, etc. may be used to describe various elements, components, regions, layers and / or regions, such elements, components, regions, layers and / And should not be limited by these terms.

1 is a flow chart showing an example of a method for producing a graphene composite electrode.

As shown in FIG. 1, the manufacturing process of the graphene composite electrode includes forming graphene on the catalyst metal (S10), forming a transparent conductive layer using the transparent conductive oxide on the graphene (S30) applying heat (heat treatment) to the transparent conductive oxide (S30), and transferring the composite electrode composed of the graphene and the transparent conductive oxide to a final substrate (S40). Hereinafter, each manufacturing step will be described with reference to FIG. 1 and the drawings.

Figs. 2 to 9 are cross-sectional schematic views showing respective steps of manufacturing the graphene composite electrode.

As shown in FIG. 2, in order to produce a composite electrode including graphene, a graphen 20 is formed on the catalyst metal 10 (S20).

Metals such as Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Si, Ta, Ti, W, U, V and Zr may be used as the catalytic metal 10 And may be used as a single layer of any one of them, or as an alloy of at least two of them.

The graphene 20 may be formed by a method such as thermal-chemical vapor deposition (CVD), inductively coupled plasma chemical vapor deposition (ICP-CVD), plasma chemical vapor deposition (PE-CVD) Chemical vapor deposition may be used. In addition, various methods such as rapid thermal annealing (RTA), atomic layer deposition (ALD), and physical vapor deposition (PVD) may be used.

As an example, the chemical vapor deposition method is a method of growing graphene 20 by placing catalyst metal 10 in a chamber (not shown), introducing a carbon source, and providing suitable growth conditions to be.

Examples of the carbon source include a gas such as methane (CH 4 ), acetylene (C 2 H 2 ), etc., and a solid form such as powder or polymer and a liquid such as bubbling alcohol It is possible.

In addition, various carbon sources such as ethane, ethylene, ethanol, acetylene, propane, butane, butadiene, pentane, pentene, cyclopentadiene, hexane, cyclohexane, benzene, toluene,

Hereinafter, examples in which copper (Cu) is used as the catalytic metal 10 and methane (CH 4 ) is used as the carbon source are described.

When methane gas is introduced into the hydrogen atmosphere while maintaining a proper temperature on the catalyst metal 10, the hydrogen reacts with methane to form the graphene 20 on the catalyst metal 10. The formation of the graphene 20 may be performed at a temperature of approximately 300 to 1500 ° C.

At this time, if there is no space on the lower surface of the catalytic metal 10, the graphene 20 may be formed only on the upper surface of the catalytic metal 10. If there is a space on the lower surface of the catalytic metal 10, The graphenes 20 may be formed on both sides of the substrate.

As the catalytic metal 10, copper has a low solubility in carbon and may be advantageous for forming a mono-layer of graphene. This graphene 20 can be formed directly on the catalyst metal 10.

The catalyst metal 10 may be supplied in the form of a sheet, but it may be fed continuously using a roller, and a catalyst metal 10 in the form of a copper foil having a thickness of approximately 10 [mu] m to 10 mm may be used have. That is, the graphene 20 may be formed on the catalyst metal 10 using a roll-to-roll process.

If the graphenes 20 are formed on both sides of the catalyst metal 10 as described above, the graphenes 20 formed on one side of the catalyst metal 10 are removed. .

2, the graphene 20 may be formed on one surface of the catalyst metal 10. In this case, as shown in FIG.

Thereafter, a process (S11) of doping the graphene 20 can be performed.

By such a doping process S11, the conductivity of the graphene 20 can be improved. That is, the graphene 20 may be deteriorated in conductivity due to crystal defects (such as a defect due to a boundary between the crystal faces of the metal) due to the catalytic metal 10, A carrier may be generated while being substituted, and thus a carrier density may be increased.

The dopant for such doping may include an organic dopant, an inorganic dopant, or a combination thereof. As an example, a vapor or a solution of a substance containing nitric acid and nitric acid can be used. In particular, it may be more advantageous to perform vapor doping using steam.

The dopant may be selected from the group consisting of NO 2 BF 4 , NOBF 4 , NO 2 SbF 6 , HCl, H 2 PO 4 , CH 3 COOH, H 2 SO 4 , HNO 3 , PVDF, Nafion, , AuCl 3 , SOCl 2 , Br 2 , CH 3 NO 2 , dichlorodicyanoquinone, oxone, di-myristoyl phosphatidyl inositol, and trifluoromethanesulfonimide.

FIG. 3 shows a state in which the transparent conductive layer 31 is formed on the graphene 20. Thus, the transparent conductive layer 31 is formed on the graphene 20 using the transparent conductive oxide (S20).

Here, the transparent conductive oxide (TCO) may be one of indium tin oxide (ITO), indium zinc oxide (IZO), zinc oxide (ZnO), gallium doped zinc oxide (GZO), and aluminum doped zinc oxide And may include at least any one of them.

Of these, ITO is a material prepared by the solid solution of SnO 2 in In 2 O 3 , and is an oxide stable at room temperature having a light-transmitting property in a visible light region, a reflection property in an infrared region, and a relatively low electric resistance.

Thereafter, step (S30) of crystallizing the transparent conductive layer 31 by applying heat (heat treatment) may be performed.

The step (S30) of crystallizing the transparent conductive layer 31 through the heat treatment may be performed at a temperature of 150 ° C to 400 ° C.

Through the crystallization step S30, the crystallization of the transparent conductive layer 31 can be enhanced and the resistance can be lowered. Thus, as shown in FIG. 4, the crystallized transparent conductive layer 30 is located on the graphene 20.

The formation (S20) of the transparent conductive layer 31 and the step (S30) of crystallizing the transparent conductive layer 31 may be performed using a sputtering apparatus as shown in FIG.

10 is a schematic view showing a process of forming the transparent conductive layer of the present invention.

First, a degree of vacuum in the chamber 100 of the apparatus is firstly formed to about 10 mTorr by using a first rotary pump 110, and then a second vacuum pump 120 is used Thereby forming a vacuum of 3 x 10 -6 mTorr.

The RF power supply 150 has a power amount of 300 W or more, which can be adjusted higher or lower. The applied frequency is usually around 14 MHz, and can be adjusted to more or less.

Ar may be implanted to cause plasma, and a step of mixing and injecting a small amount of oxygen may be added to perform the crystallization step S30.

The ITO 30 may be formed on the graphene 20 formed on the catalyst metal 10 by the above process, and the graphene 20 is omitted in FIG.

When plasma is generated on the side of the target 130 after power is applied by the RF power source 150, the target 130 evaporates and ITO is formed on the graphene 20 as the transparent conductive layer 30 do. The permanent magnet 140 may be positioned below the target 130.

Hereinafter, the crystallized transparent conductive layer 30 will be described as an ITO layer, for example.

The transparent conductive layer 30 formed on the graphenes 20 may form a transparent composite electrode. That is, a transparent composite electrode having a low resistance value can be formed through the organic / inorganic hybrid of the graphene 20 and the ITO layer 30.

Such a composite electrode can be directly applied to a sputtering method which is currently used in industry, thereby reducing the amount of ITO used to one fifth. This is because, due to the composite electrode, a condition that can be used as a transparent electrode can be satisfied even if it is formed in a small thickness.

In addition, the ITO layer 30 can serve as a protective film for the graphenes 20 at the same time. If the graphene 20 is doped, the effect of such doping may be maintained for a longer period of time.

Thereafter, a step S40 of transferring the composite electrode composed of the graphene 20 and the ITO layer 30 to the final substrate may be performed.

This transfer step S40 can be largely performed in two ways.

First, a temporary support layer is used.

For this purpose, as shown in Fig. 5, the supporting layer is placed on the ITO layer 30. [ This support layer 40 may be deposited on the ITO layer 30 or may be formed directly. A transfer film may be used for the support layer 40 to be adhered on the ITO layer 30. Such a transfer film includes a pressure sensitive adhesive layer and is liable to lose adhesiveness when heat or light is applied thereto, Can be separated.

The adhesive layer may be a rework adhesive. That is, it is possible to easily peel off during or after the process, and to retain the residual material even after peeling off.

Next, as shown in Fig. 6, a step of removing the catalyst metal 10 is performed.

Thereafter, the final substrate 50 may be attached to the side from which the catalyst metal 10 is removed. Optionally, this final substrate 50 may be formed directly on the side from which the catalyst metal 10 is removed.

This final substrate 50 may refer to a layer that can be bonded to the electronic device intact with the graphene 20.

That is, it may be a transparent or opaque substrate that can be directly used for various display devices, or may be a substrate that can be directly used in a device such as a touch panel.

As the final substrate 50, a polymer material such as PET (polyethylen terephthalate), TAC (triacetyl cellulose), and PC (poly carbonate) may be used and a semiconductor wafer such as silicon (Si) may be used. In addition, any member in the form of a transparent or opaque film can be used.

Thereafter, the step of removing the support layer 40 may be included. 7, the composite electrode composed of the graphene 20 and the ITO layer 30 is placed on the final substrate 50. As shown in Fig.

On the other hand, the final substrate 50 may be directly attached or formed on the ITO layer 30 without using a supporting layer, and may be transferred.

Thereafter, the catalyst metal 10 can be removed.

The composite electrode made of the graphene 20 and the ITO layer 30 may be placed on the final substrate 50 through such a transfer method. However, as shown in FIG. 9, the ITO layer 30 is first placed on the final substrate 50.

As described above, a flexible transparent electrode can be manufactured using the composite electrode transferred onto the final substrate 50. That is, since the composite electrode can have conductivity and flexibility at the same time, it is possible to overcome the limitations of the flexible display, which was impossible with only the ITO layer.

As described above, the present process can be directly applied to the ITO roll-to-roll process and can be applied together with the roll-to-roll-based graphene process.

Since the composite electrode including the graphene 20 includes an organic material (graphene), it is possible to form a transparent composite electrode through the hybrid of the graphene 20 and the ITO layer 30, It can be excellent in adhesion to an EL display.

Therefore, as shown in FIG. 9, the organic EL layer 60 may further be formed on the graphene 20. As described above, the composite electrode manufactured according to the embodiment of the present invention can be used as a transparent electrode of an organic EL display, and in particular, it can be used as a flexible electrode. However, the object of application is not limited to the organic EL display.

As described above, the composite electrode of the graphene 20 and the ITO layer 30 can be heat-treated at a temperature of 150 ° C to 400 ° C, thereby greatly improving the conductivity. In the case of using only ITO located on a conventional polymer substrate as a transparent electrode, heat treatment can not be performed at 150 ° C. or higher. Therefore, the conductivity of the transparent electrode manufactured according to the present invention can be greatly improved.

In addition, in the case of having the same conductivity, the thickness of the electrode can be reduced to half or less, and the electrode material can be consumed in a small amount.

It should be noted that the embodiments of the present invention disclosed in the present specification and drawings are only illustrative of specific examples for the purpose of understanding and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that other modifications based on the technical idea of the present invention are possible in addition to the embodiments disclosed herein.

10: catalyst metal 20: graphene
30: transparent conductive layer (ITO) 40: support layer
50: final substrate 60: organic EL layer

Claims (8)

In the method for producing a graphene composite electrode,
Forming graphene on the catalytic metal;
Doping the graphene;
Forming a transparent conductive oxide covering the doped graphene to protect the doped graphene on the doped graphene;
Crystallizing the transparent conductive oxide by applying heat of at least 150 ° C; And
And transferring the composite electrode composed of the graphene and the transparent conductive oxide to a final substrate,
Wherein the step of forming the transparent conductive oxide and the step of crystallizing the transparent conductive oxide use sputtering. delete The method of claim 1, wherein the crystallizing step is performed at a temperature of 150 ° C to 400 ° C. The method of claim 1, wherein the transparent conductive oxide comprises at least one of ITO, IZO, ZnO, GZO, and AZO. The method according to claim 1,
Positioning a support layer on the transparent conductive oxide;
Removing the catalyst metal;
Attaching the composite electrode to the final substrate; And
And removing the supporting layer. The method of manufacturing a graphene composite electrode according to claim 1, The method according to claim 1,
Forming the final substrate on the transparent conductive oxide; And
And removing the catalyst metal. The method of manufacturing a graphene composite electrode according to claim 1, The method of claim 1, wherein the final substrate is a polymer substrate. The method of claim 1, further comprising forming an organic EL layer on the graphene.
KR1020150052902A 2015-04-15 2015-04-15 Method for manufacturing graphene hybrid electrode KR101706963B1 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
KR1020150052902A KR101706963B1 (en) 2015-04-15 2015-04-15 Method for manufacturing graphene hybrid electrode
US15/563,087 US10497893B2 (en) 2015-04-15 2016-04-15 Method for doping graphene, method for manufacturing graphene composite electrode, and graphene structure comprising same
EP16780306.3A EP3284718B1 (en) 2015-04-15 2016-04-15 Method for doping graphene, and graphene structure
CN201680021660.5A CN107635918B (en) 2015-04-15 2016-04-15 Graphene doping method, graphene composite electrode manufacturing method, and graphene structure including same
PCT/KR2016/003910 WO2016167583A1 (en) 2015-04-15 2016-04-15 Method for doping graphene, method for manufacturing graphene composite electrode, and graphene structure comprising same

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CN107293348A (en) * 2017-06-30 2017-10-24 西安电子科技大学 Flexible and transparent combination electrode based on three-dimensional grapheme and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003306400A (en) * 2002-04-10 2003-10-28 Seiko Epson Corp Processes for manufacturing electro-optical device and substrate therefor
KR101221581B1 (en) * 2011-10-20 2013-01-14 한국기계연구원 Fabrication method of flexible transparent electrode substrate with graphene, and the flexible transparent electrode substrate substrate thereby

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KR101295664B1 (en) * 2011-06-24 2013-08-13 그래핀스퀘어 주식회사 Stable graphene film and preparing method of the same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003306400A (en) * 2002-04-10 2003-10-28 Seiko Epson Corp Processes for manufacturing electro-optical device and substrate therefor
KR101221581B1 (en) * 2011-10-20 2013-01-14 한국기계연구원 Fabrication method of flexible transparent electrode substrate with graphene, and the flexible transparent electrode substrate substrate thereby

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