KR20130099451A - Method of manufacturing graphene - Google Patents

Method of manufacturing graphene Download PDF

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Publication number
KR20130099451A
KR20130099451A KR1020120020972A KR20120020972A KR20130099451A KR 20130099451 A KR20130099451 A KR 20130099451A KR 1020120020972 A KR1020120020972 A KR 1020120020972A KR 20120020972 A KR20120020972 A KR 20120020972A KR 20130099451 A KR20130099451 A KR 20130099451A
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KR
South Korea
Prior art keywords
graphene
layer
graphene layer
substrate
target substrate
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KR1020120020972A
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Korean (ko)
Inventor
김택수
윤태식
조병진
신우철
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한국과학기술원
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Priority to KR1020120020972A priority Critical patent/KR20130099451A/en
Priority to PCT/KR2013/001450 priority patent/WO2013129807A1/en
Publication of KR20130099451A publication Critical patent/KR20130099451A/en

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/184—Preparation
    • C01B32/186—Preparation by chemical vapour deposition [CVD]
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/194—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching

Abstract

PURPOSE: A method for manufacturing graphene is provided to massively manufacture graphene devices with an environment-friendly method. CONSTITUTION: A method for manufacturing graphene comprises: a step (S100) of forming a graphene layer on a base substrate; a step (S110) of attaching a target substrate to the graphene layer; and a step (S120) of transcribing the graphene layer on the target substrate by separating the graphene layer from the base substrate. [Reference numerals] (AA) Start; (BB) Yes; (CC) No; (DD) End; (S100) Forming a graphene layer on a base substrate; (S110) Attaching a target substrate to the graphene layer; (S120) Transcribing the graphene layer on the target substrate by separating the graphene layer from the base substrate; (S130) Whether S100 or S120 is implemented again or not on the same base substrate

Description

Graphene manufacturing method {METHOD OF MANUFACTURING GRAPHENE}

The present invention relates to a method for producing graphene, and more particularly, to a method for producing graphene using a chemical vapor deposition method.

Graphene refers to a planar two-dimensional carbon structure that forms sp2 bonds, and has a high physical and chemical stability. At room temperature, electrons can move 100 times faster than silicon, and 100 times more current per unit area than copper. In addition, the thermal conductivity is more than two times higher than diamond, the mechanical strength is more than 200 times stronger than steel and has transparency. In addition, the spatial clearance of the hexagonal honeycomb structure where carbon is connected like a net creates elasticity and does not lose its electrical conductivity when stretched or folded.

A general method for producing graphene is a chemical vapor deposition (CVD) method, which can produce graphene having a large area and high quality on a metal substrate.

In such a conventional CVD method, a large area of high quality graphene formed on a metal substrate needs to be removed by a wet etching method for transfer to a target substrate. However, the wet etching may cause structural and chemical damage to the graphene. In addition, such a wet etching method has a problem that the metal substrate should be discarded after being used once, which is uneconomical, and the etching process takes a long time, so it is not suitable for mass production. Moreover, there is a problem of generating a chemical contaminant consisting of a metal and an etchant through a wet etching method.

One object of the present invention is to provide a graphene manufacturing method capable of mass-producing graphene-based devices and devices in an economical and environmentally friendly way.

It is to be understood, however, that the present invention is not limited to the above-described embodiments and various modifications may be made without departing from the spirit and scope of the invention.

In the graphene manufacturing method according to the embodiments of the present invention to achieve the object of the present invention, to form a graphene layer on a base substrate. A target substrate is attached to the graphene layer through an adhesive layer. The graphene layer is separated from the base substrate to transfer the graphene layer onto the target substrate.

In example embodiments, the forming of the graphene layer may include forming a catalyst layer on the base substrate and growing the graphene layer on the catalyst layer.

In example embodiments, the growing of the graphene layer may be performed by a chemical vapor deposition process.

In example embodiments, the catalyst layer may include a metal. For example, the catalyst layer may comprise copper.

In example embodiments, the attaching the target substrate on the graphene layer may include applying a polymer material on the graphene layer and curing the polymer material between the graphene layer and the target substrate. It may include.

In this case, the method may further comprise applying a mechanical load between the graphene layer and the target substrate.

In example embodiments, the separating the graphene layer from the base substrate may include separating the target substrate from the base substrate by applying a mechanical force.

In example embodiments, the method may further include forming a new graphene layer on the base substrate from which the graphene layer has been removed after transferring the graphene layer onto the target substrate. .

In this case, the method may further include transferring the graphene layer onto a new target substrate.

In the graphene manufacturing method according to embodiments of the present invention, (i) a graphene layer is formed on the base substrate on which the metal layer is formed. (Ii) A target substrate is attached onto the graphene layer via an adhesive layer. (Iii) The graphene layer is mechanically peeled from the metal layer to transfer the graphene layer onto the target substrate. (Iii) Steps (iii) to (iii) are repeatedly performed on the same base substrate.

In example embodiments, the step of mechanically peeling the graphene layer from the metal layer may include separating the base substrate and the target substrate by applying a mechanical force.

In example embodiments, the forming of the graphene layer may include forming a catalyst layer on the base substrate and growing the graphene layer on the catalyst layer.

In example embodiments, the growing of the graphene layer may be performed by a chemical vapor deposition process.

In example embodiments, the catalyst layer may include a metal.

In the graphene manufacturing method according to the invention configured as described above, it is possible to repeatedly grow the high-quality single layer of graphene without damaging the metal substrate by performing an etch-free mechanical transfer process, it is cost competitive and environmentally friendly In this way, graphene devices can be mass produced.

However, the effects of the present invention are not limited to the above-mentioned effects, and may be variously expanded without departing from the spirit and scope of the present invention.

1 is a flowchart illustrating a method of manufacturing graphene according to an embodiment of the present invention.
2A to 2E are perspective views illustrating a method of manufacturing graphene according to an embodiment of the present invention.
3A is a cross-sectional view illustrating graphene peeled by a mechanical transfer process according to an exemplary embodiment of the present invention.
FIG. 3B is a scanning electron microscope (SEM) image showing the portion “I” of FIG. 3A.
FIG. 4 is a graph showing Raman Spectra of a graphene layer prepared as a result of repeated performing mechanical transfer processes according to an embodiment of the present invention.

For the embodiments of the invention disclosed herein, specific structural and functional descriptions are set forth for the purpose of describing an embodiment of the invention only, and it is to be understood that the embodiments of the invention may be practiced in various forms, The present invention should not be construed as limited to the embodiments described in Figs.

As the inventive concept allows for various changes and numerous modifications, particular embodiments will be illustrated in the drawings and described in detail in the text. It is to be understood, however, that the invention is not intended to be limited to the particular forms disclosed, but on the contrary, is intended to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.

Terms such as first and second may be used to describe various components, but the components should not be limited by the terms. The terms may be used for the purpose of distinguishing one component from another component. For example, without departing from the scope of the present invention, the first component may be referred to as a second component, and similarly, the second component may also be referred to as a first component.

When a component is referred to as being "connected" or "connected" to another component, it may be directly connected to or connected to that other component, but it may be understood that other components may be present in between. Should be. On the other hand, when an element is referred to as being "directly connected" or "directly connected" to another element, it should be understood that there are no other elements in between. Other expressions that describe the relationship between components, such as "between" and "between" or "neighboring to" and "directly adjacent to" should be interpreted as well.

The terminology used herein is for the purpose of describing particular example embodiments only and is not intended to be limiting of the present invention. Singular expressions include plural expressions unless the context clearly indicates otherwise. In the present application, the terms "comprise", "having", and the like are intended to specify the presence of stated features, integers, steps, operations, elements, components, or combinations thereof, , Steps, operations, components, parts, or combinations thereof, as a matter of principle.

Unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries should be construed as meaning consistent with meaning in the context of the relevant art and are not to be construed as ideal or overly formal in meaning unless expressly defined in the present application .

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. The same reference numerals are used for the same constituent elements in the drawings and redundant explanations for the same constituent elements are omitted.

1 is a flowchart illustrating a method of manufacturing graphene according to an embodiment of the present invention. 2A to 2E are perspective views illustrating a method of manufacturing graphene according to an embodiment of the present invention.

1 to 2E, a method of manufacturing graphene according to an embodiment of the present invention includes forming the graphene layer by chemical vapor deposition (CVD) and forming the graphene layer by a reproducible mechanical transfer process. The transfer may be performed based on the step of transferring onto the target substrate.

First, the graphene layer 120 is formed on the base substrate 100 (S100).

As shown in FIG. 2A, the catalyst layer 110 may be formed on the base substrate 100. In one embodiment of the present invention, the base substrate 100 may be a silicon substrate, the silicon oxide layer 102 may be formed on the base substrate 100.

The catalyst layer 110 may serve to help the carbon components combine with each other to form a hexagonal plate-like structure. For example, the catalyst layer 110 is from the group consisting of Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Si, Ta, Ti, W, U, V and Zr One or more selected metals or alloys may be used.

In this embodiment, the catalyst layer 110 may include copper. Copper may be advantageous for forming large area monolayer graphene because of the relatively low solubility of carbon.

As shown in FIG. 2B, the graphene layer 120 may be formed on the catalyst layer 110. After depositing the catalyst layer 110 made of metal on the base substrate 100, the base substrate 100 is loaded into a chamber of an inductively coupled plasma chemical vapor deposition (ICP-CVD) apparatus, and then a graphene growth process is performed. Thus, a large area graphene single layer may be formed on the catalyst layer 110. Thus, a high quality single layer graphene 120 having a low defect density can be formed over a large area with good uniformity on the copper catalyst layer 110.

Subsequently, after attaching the target substrate 200 to the graphene layer 120 via the adhesive layer 130 (S110), the graphene layer 120 is separated from the base substrate 100 to be attached on the target substrate 200. Transfer to (S120).

2C and 2D, in one embodiment of the present invention, a polymer material such as epoxy is coated on the graphene layer 120, and then, between the graphene layer 120 and the target substrate 200. The epoxy material can be cured.

The epoxy material may be applied on selected regions on the graphene layer 120 according to the size of the graphene layer to be transferred. Subsequently, the base substrate 100 and the target substrate 200 may be attached to each other with a mechanical load such as a constant clamping pressure (eg, 150 kPa). The epoxy material may be cured at a temperature of 125 ° C. for 2 hours to form an epoxy adhesive layer 130 of 1 μm. For example, the target substrate 200 may be a flexible polyimide substrate.

In one embodiment of the present invention, the bond energy between the grown graphene layer 120 and the copper catalyst layer 110 may be smaller than the bond energy between the epoxy adhesive layer 130 and the target substrate 200. For example, the binding energy between the grown graphene layer 120 and the copper catalyst layer 110 may be measured by a double cantilever beam (DCB) test facility.

This measurement of binding energy can be used to perform repeatable and reproducible mechanical transfer processes on a single layer of graphene grown on copper. Using the accurately measured binding energy, the force required to overcome the bond between the graphene layer 120 and the copper catalyst layer 110 and the type of adhesive that can be used can be determined.

As shown in FIG. 2E, in the exemplary embodiment of the present invention, the graphene layer 120 may be separated from the base substrate 100 to transfer the graphene layer 120 onto the target substrate 200.

After the grips 310 of the mechanical separation apparatus are attached to one surface of the base substrate 100 and one surface of the target substrate 200, the base 100 and the target substrate 200 are opposite to each other. Can be moved to Accordingly, the graphene layer 120 may be mechanically peeled from the copper catalyst layer 110 and simultaneously transferred to the target substrate 200 by the epoxy adhesive layer 130 applied on the selected region on the graphene layer 120. have.

By accurately measuring the binding energy of the graphene 120 grown on the copper catalyst layer 110, the graphene layer 120 is transferred directly from the base substrate 100 onto the target substrate 200 without any etching process. can do. The graphene 120 on the copper catalyst layer 110 may be selectively bonded to the target substrate 200 such as a flexible polyimide substrate using the epoxy adhesive layer 130.

For example, graphene transferred directly onto a flexible polyimide substrate can be used to produce graphene devices such as top-gate graphene field effect transistors (FETs) with good top-gate modulation and bending stability. .

In one embodiment of the present invention, after the transfer of the graphene layer, the processes described with reference to FIGS. 2A to 2E may be repeatedly performed (S130). Specifically, after the graphene layer 120 is transferred onto the target substrate 200, the copper catalyst layer 110 from which the graphene layer 120 has been removed is reused in the graphene growth process to obtain a new single layer of graphene. After regrowth on a bare copper substrate, it can be transferred onto a new target substrate.

3A is a cross-sectional view illustrating graphene being peeled off by a mechanical transfer process according to an exemplary embodiment of the present invention, and FIG. 3B is a scanning electron microscope (SEM) image showing part “I” of FIG. 3A.

Referring to FIG. 3A, since the bonding energy between the grown graphene layer 120 and the copper catalyst layer 110 is smaller than the bonding energy between the epoxy adhesive layer 130 and the target substrate 200, the graphene layer 120 may be While peeling from the copper catalyst layer 110, the graphene layer 120 may be transferred onto the target substrate 200.

Referring to FIG. 3B, the mechanical exfoliation of the graphene layer 120 may be performed over a large area with high precision of micro or less through an adhesive layer. The boundary line I between the copper catalyst layer 110 from which the graphene layer 120 has been removed and the copper catalyst layer 110 covered by the graphene layer 120 is clearly shown.

FIG. 4 is a graph showing Raman Spectra of a graphene layer prepared as a result of repeated performing mechanical transfer processes according to an embodiment of the present invention.

Referring to FIG. 4, in one embodiment of the present invention, a process capable of transferring a large area of graphene reproducibly without etching is a mechanical device capable of regenerating a single layer of graphene on the copper catalyst layer 110. Peeling can be repeated.

After the graphene layer is transferred onto the target substrate, the copper catalyst layer 120 on the base substrate 100 may be used in the same graphene growth process to regrow the new monolayer graphene. High quality monolayer graphene can be regrown repeatedly without damaging the copper substrate by performing an etch free mechanical transfer process. The regrown graphene layer can be transferred onto a new target substrate and used directly in the manufacture of graphene devices.

As shown in FIG. 4, graphene layers re-grown (second growth, third growth) as a result of Raman spectroscopy of the graphene layer and the copper from which the graphene layer was removed by repeatedly performing a graphene growth process and a mechanical transfer process In the case of the first growth (first growth), as in the case of graphene, the G peak (peak) around Raman shift (Raman shift) 1580 cm -1 and the 2D peak around Raman shift 2700 cm -1 could be confirmed .

Thus, one of the most important advantages of the etch free mechanical transfer process according to one embodiment of the present invention is that it does not damage the substrate on which the copper catalyst layer is formed. Therefore, the copper substrate can additionally be reused for graphene growth and transfer processes.

Conventional wet chemical etching for removing a metal substrate after growing graphene on a metal substrate such as the copper substrate has been considered a necessary process for peeling the grown graphene from the metal substrate. However, this time-consuming etching process creates dangerous chemical wastes and can therefore be a serious cause of water contamination by copper solutions. In addition, the quality of graphene also tends to degrade when using this process. More importantly, the metal catalyst layer is removed by an etching process after one graphene transfer.

As described above, in the graphene manufacturing method according to the present invention, by performing such an etching-free mechanical transfer process it is possible to re-grow the high-quality single layer of graphene repeatedly without damaging the copper substrate, Graphene devices can be mass produced in a competitive and environmentally friendly way.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention as defined in the following claims. It can be understood that it is possible.

100: base substrate 102: silicon oxide layer
110: catalyst layer 120: graphene layer
130: adhesive layer 200: target substrate

Claims (15)

Forming a graphene layer on the base substrate;
Attaching a target substrate on the graphene layer through an adhesive layer;
Separating the graphene layer from the base substrate and transferring the graphene layer onto the target substrate. The method of claim 1, wherein the forming of the graphene layer
Forming a catalyst layer on the base substrate; And
Graphene manufacturing method comprising the step of growing the graphene layer on the catalyst layer. The method of claim 2, wherein the growing of the graphene layer is performed by a chemical vapor deposition process. The method of claim 2, wherein the catalyst layer comprises a metal. The method of claim 4, wherein the catalyst layer comprises copper. The method of claim 1, wherein attaching the target substrate to the graphene layer
Applying a polymer material on the graphene layer; And
And hardening the polymer material between the graphene layer and the target substrate. The method of claim 6, further comprising applying a mechanical load between the graphene layer and the target substrate. The method of claim 1, wherein the separating of the graphene layer from the base substrate comprises separating the target substrate from the base substrate by applying a mechanical force. The method of claim 1, further comprising forming a new graphene layer on the base substrate from which the graphene layer is removed after transferring the graphene layer onto the target substrate. Way. The method of claim 9, further comprising transferring the graphene layer onto a new target substrate. (Iii) forming a graphene layer on the base substrate on which the metal layer is formed;
(Ii) attaching a target substrate on the graphene layer through an adhesive layer;
(Iii) mechanically peeling the graphene layer from the metal layer to transfer the graphene layer onto the target substrate; And
(Iii) repeatedly performing steps (iii) to (iii) on the same base substrate. The method of claim 11, wherein the step of mechanically peeling the graphene layer from the metal layer comprises separating the base substrate and the target substrate by applying a mechanical force. The method of claim 11, wherein forming the graphene layer
Forming a catalyst layer on the base substrate; And
Graphene manufacturing method comprising the step of growing the graphene layer on the catalyst layer. The method of claim 13, wherein the growing the graphene layer is performed by a chemical vapor deposition process. The method of claim 11, wherein the catalyst layer comprises a metal.
KR1020120020972A 2012-02-29 2012-02-29 Method of manufacturing graphene KR20130099451A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015037848A1 (en) * 2013-09-16 2015-03-19 덕산하이메탈 주식회사 Stacked transparent electrode comprising nano-material layer and manufacturing method therefor

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8753468B2 (en) * 2009-08-27 2014-06-17 The United States Of America, As Represented By The Secretary Of The Navy Method for the reduction of graphene film thickness and the removal and transfer of epitaxial graphene films from SiC substrates
KR101454463B1 (en) * 2009-09-21 2014-10-23 삼성테크윈 주식회사 Method for manufacturing graphene
KR20110090397A (en) * 2010-02-03 2011-08-10 삼성테크윈 주식회사 Apparatus and method for forming graphene pattern
KR101451138B1 (en) * 2010-05-04 2014-10-15 삼성테크윈 주식회사 Method for manufacturing graphene sheet

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015037848A1 (en) * 2013-09-16 2015-03-19 덕산하이메탈 주식회사 Stacked transparent electrode comprising nano-material layer and manufacturing method therefor
KR101524069B1 (en) * 2013-09-16 2015-06-10 덕산하이메탈(주) Stacking type transparent electrode having nano material layer

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