KR101926488B1 - Method of manufacturing grapheme film - Google Patents

Method of manufacturing grapheme film Download PDF

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KR101926488B1
KR101926488B1 KR1020130013495A KR20130013495A KR101926488B1 KR 101926488 B1 KR101926488 B1 KR 101926488B1 KR 1020130013495 A KR1020130013495 A KR 1020130013495A KR 20130013495 A KR20130013495 A KR 20130013495A KR 101926488 B1 KR101926488 B1 KR 101926488B1
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graphene
temperature
carrier tape
film
catalytic metal
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KR1020130013495A
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Korean (ko)
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KR20140100326A (en
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윤종혁
원동관
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한화에어로스페이스 주식회사
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Priority to KR1020130013495A priority Critical patent/KR101926488B1/en
Priority to PCT/KR2014/000732 priority patent/WO2014123319A1/en
Publication of KR20140100326A publication Critical patent/KR20140100326A/en
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B01J19/1887—Stationary reactors having moving elements inside forming a thin film
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B01J19/22—Stationary reactors having moving elements inside in the form of endless belts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/247—Suited for forming thin films

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The present invention provides a method of manufacturing a catalyst metal substrate, comprising: preparing a catalytic metal substrate on which graphene is synthesized on at least one side; Bonding a carrier tape to the graphene at a first temperature; Removing the catalytic metal substrate and bonding the exposed graphene to a target substrate; And peeling the carrier tape at a second temperature lower than the first temperature; And a method for producing the graphene film.

Description

TECHNICAL FIELD The present invention relates to a method of manufacturing a graphene film,

An embodiment of the present invention relates to a method for producing a graphene film.

Graphene is a material in which carbon is hexagonally connected to form a honeycomb two-dimensional planar structure. Its thickness is very thin, transparent, and has high electrical conductivity. Many attempts have been made to apply graphene to a touch panel, a transparent display, or a flexible display using such characteristics of graphene. With the growing interest in graphene, a method for mass production of high quality graphene is required.

Graphene is synthesized on the surface of the catalyst metal by chemical vapor deposition or the like by feeding a carbon source, and a thermal peeling tape is attached to the synthesized graphene. Next, the catalytic metal on one surface of the graphene was removed, a predetermined heat and pressure were applied thereto, the thermal release tape was peeled off, and the graphene was transferred to the target substrate. Here, the heat peeling tape includes a foaming cell on the bonding surface, and when the predetermined heat is applied, the foaming cell is foamed and the graphene and the heat peeling tape are peeled off. Therefore, the heat peeling tape once used is not reusable. Further, when the heat peeling tape is peeled off, the graphene is liable to be damaged by foaming of the foaming cell.

An embodiment of the present invention provides a method for producing a graphene film having less damage.

According to an embodiment of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: preparing a catalyst metal substrate on which graphene is synthesized on at least one side; Bonding a carrier tape to the graphene at a first temperature; Removing the catalytic metal substrate and bonding the exposed graphene to a target substrate; And peeling the carrier tape at a second temperature lower than the first temperature; And a method for producing the graphene film.

The step of bonding to the target substrate is performed at a third temperature, and the third temperature is higher than the second temperature.

Wherein the carrier tape has an adhesive force at a temperature higher than the switching temperature and loses the adhesive force at a temperature lower than the switching temperature and the first temperature and the third temperature are higher than the switching temperature, .

Bonding the carrier tape to the graphene, and bonding the graphene to the target substrate are performed under a pressurized condition.

The carrier tape is repeatedly used to produce a graphene film.

According to an aspect of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: preparing a catalytic metal film on which graphene is synthesized on at least one side; Pressing with a heating roller to bond the carrier tape to the graphene at a first temperature; Removing the catalyst metal film, pressing the exposed graphene with a heating roller to bond the graphene to the target film; And peeling the carrier tape at a second temperature lower than the first temperature; Wherein all of the steps are performed in a roll-to-roll manner.

According to the embodiment of the present invention, a graphene film with less damage can be obtained and the carrier tape can be reused, which is economical.

1 is a perspective view schematically illustrating the graphene referred to herein.
2 is a perspective view schematically showing a carrier tape referred to in this specification;
Fig. 3 shows the characteristics of the carrier tape shown in Fig.
FIGS. 4 to 9 are schematic cross-sectional side views of a laminate including graphene corresponding to each step of the method of manufacturing a graphene film according to an embodiment of the present invention.
10 is a graph schematically showing temperature corresponding to each step of the method for producing a graphene film according to an embodiment of the present invention and the method for producing a graphene film according to a comparative example of the present invention.
Fig. 11 shows data obtained by repeatedly carrying out adhesion and peeling of the carrier tape 2 in the manufacturing process of the graphene film shown in Figs. 4 to 9. Fig.
FIG. 12 shows a method of manufacturing a graphene film according to an embodiment of the present invention by a roll-to-roll method.

BRIEF DESCRIPTION OF THE DRAWINGS The present invention is capable of various modifications and various embodiments, and specific embodiments are illustrated in the drawings and described in detail in the detailed description. It is to be understood, however, that the invention is not to be limited to the specific embodiments, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

The terms first, second, etc. used in this specification may be used to describe various elements, but the elements should not be limited by terms. Terms are used only for the purpose of distinguishing one component from another.

It will be understood that when a layer, film, region, plate, or the like is referred to as being "on" or "on" another portion, do.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. Referring to the drawings, substantially identical or corresponding elements are denoted by the same reference numerals, do. In the drawings, the thickness is enlarged to clearly represent the layers and regions. In the drawings, the thicknesses of some layers and regions are exaggerated for convenience of explanation.

1 is a perspective view schematically illustrating the graphene referred to herein.

As used herein, the term "graphene" refers to a graft in which a plurality of carbon atoms are covalently linked to one another to form a polycyclic aromatic molecule, A 6-membered ring is formed as a repeating unit, but it is also possible to further include a 5-membered ring and / or a 7-membered ring. Thus, the graphene film forms a single layer of covalently bonded carbon atoms (C) (usually sp2 bonds). The graphene film may have various structures, and such a structure may vary depending on the content of the 5-membered ring and / or the 7-membered ring which may be contained in the graphene.

The graphene film may be formed of a single layer of graphene as shown in the figure, but it is also possible to form a plurality of layers by stacking a plurality of the graphene films. Usually, the lateral end portions of the graphene film may be saturated with hydrogen atoms (H) .

On the other hand, the term "graphene film" as used herein can mean a laminate in which the graphene of FIG. 1 is transferred to a target substrate or a target film.

2 is a perspective view schematically illustrating a carrier tape 120 referred to herein. Fig. 3 shows the characteristics of the carrier tape 120 of Fig.

As used herein, the term " carrier tape " is a member that supports graphene until the graphene is transferred to the target substrate in the process of manufacturing the graphene film. The carrier tape 120 is adhered to and peeled from the graphene, and the electrical characteristics and optical characteristics of the graphene film obtained vary depending on the degree of damage to the graphene.

The carrier tape 120 includes a base layer 121 and an adhesive layer 122 that is several tens of micrometers thick. The adhesive layer 122 is characterized in that it comprises a semi- crystalline graft copolymer, for example an intel- termer polymer. The adhesive layer 122 containing such a component is different in adhesion force based on the switching temperature Ts as shown in Fig. 3 (a). In detail, as shown in FIG. 3 (b), the intelimore polymer has a crystalline state at a temperature lower than the switching temperature Ts, which is reduced in volume and lost its adhesion. For example, it can have a small adhesive force of about 0.001 N / 25 mm to 0.1 N / 25 mm. However, as shown in FIG. 3 (c), the ionomeric polymer has an amorphous stoichiometry at a temperature higher than the switching temperature Ts, thereby increasing its volume and having an adhesive force. For example, it can have a large adhesive force of about 1 N / 25 mm to 10 N / 25 mm.

The switching temperature (Ts) of the Intel reamer polymer can be controlled through the length of the aliphatic side-chain crystallizing group and the amount of active ingredient added. For example, the longer the length of the aliphatic side chain crystallization group, the higher the switching temperature Ts, and vice versa, the lower the switching temperature Ts. Further, when the amount of the active ingredient to be added is increased, the switching temperature Ts is lowered, and when the amount is decreased, the switching temperature Ts can be increased.

According to one embodiment of the present invention, since the carrier tape 120 is directly adhered to the graphene and is peeled off from the graphene, the range of the adhesive force is preferably maintained at about 0.05 N / 25 mm to 5 N / 25 mm. If the adhesive force exceeds 5 N / 25 mm at a temperature higher than the switching temperature, there is a problem that the graphene damage is large when the carrier tape 120 is peeled off, thereby deteriorating the electrical characteristics and optical characteristics of the graphene.

According to an embodiment of the present invention, the switching temperature Ts of the carrier tape 120 is suitably in the range of about 30 degrees to about 80 degrees. If the switching temperature Ts is 30 degrees Celsius or less, it takes a long time to cool the graphene film when peeling off the carrier tape 120, which is not advantageous in terms of the process. In addition, when the switching temperature Ts is 80 degrees Celsius or more, the process of removing the catalytic metal substrate in the state where the carrier tape 120 is bonded progresses at 80 degrees Celsius or less. Therefore, when removing the catalytic metal substrate, There is a problem that graphene transfer to the target film is impossible.

The base layer 121 included in the carrier tape 120 may be made of polyethylene terephthalate (PET), silicon, polyimide, or the like, and serves to support the adhesive layer 122. The carrier tape 120 is disposed on the adhesive layer 122 and may further include a protective layer (not shown) that protects the adhesive layer 122 until the carrier tape 120 is adhered to the graphene. The protective layer is peeled off when the carrier tape 120 is adhered to the graphene, for example, with a release paper.

Hereinafter, a method of manufacturing a graphene film using such a carrier tape 120 will be described.

4 to 9 show that the catalytic metal substrate, the carrier tape and the target substrate used in the production of the graphene film are discontinuous panel type. However, the present invention is not limited thereto, and the catalyst metal film, the carrier film, and the target film used in the production of the graphene film may be a continuous roll type in one direction as shown in FIG. Therefore, in the case of the roll type, the term is described as a film separately from the panel type. Hereinafter, for the sake of convenience, the panel type will be described first.

FIGS. 4 to 9 are schematic cross-sectional side views of a laminate including graphene corresponding to each step of the method of manufacturing a graphene film according to an embodiment of the present invention. 10 is a graph schematically showing temperatures corresponding to the respective steps of the method for producing a graphene film according to an embodiment of the present invention and the method for producing a graphene film according to a comparative example of the present invention.

A in FIG. 10 is a temperature value used in the step of manufacturing a graphene film according to an embodiment of the present invention. In case of A, the carrier tape of Fig. 2 is used to produce a graphene film. Meanwhile, B is the temperature value used in the graphene film producing step according to the comparative example of the present invention. In case of B, the thermal release tape mentioned in the Background of the Invention is used to produce a graphene film. In FIG. 10, the x-axis is divided into the respective steps. The x-axis is divided into the graphene forming step I, the carrier tape bonding step II, the catalyst metal removing step III, the target substrate bonding step IV and the carrier tape peeling step V )to be.

The term "laminate " as used herein refers to a plurality of layers including a graphene 110, and the graphene 110 may be formed with a catalyst metal substrate 101, The carrier tape 120, and the target substrate 130. In this case,

Referring to FIG. 4, first, a catalyst metal substrate 101 is prepared.

The catalyst metal substrate 101 may be in the form of a discontinuous panel as a catalyst thin film for graphene growth. The catalytic metal substrate 101 may be formed of at least one selected from the group consisting of copper (Cu), nickel (Ni), cobalt (Co), iron (Fe), platinum (Pt), gold (Au), silver (Ag) ), Magnesium (Mg), manganese (Mn), molybdenum (Mo), rhodium (Rh), silicon (Si), tantalum (Ta), titanium (Ti), tungsten (W), uranium V, at least one of Pd, Y, Zr, Ge, Brass, Bronze, White Brass and Stainless Steel. Metals, or alloys, but is not limited thereto.

The catalytic metal substrate 101 may be a single layer, and one layer of the multilayer substrate of at least two layers may be the catalytic metal layer 101. In this case, the catalytic metal layer 101 is disposed at the outermost portion of the multilayer substrate.

The surface of the catalytic metal substrate 101 is cleaned before the graphene 110 is formed. The pretreatment process is for removing foreign substances existing on the surface of the catalytic metal substrate 101, and hydrogen gas can be used. Further, by cleaning the surface of the catalytic metal substrate 101 using an acid or an alkali solution or the like, defects can be reduced in the subsequent process of forming the graphene 110. [ This step of cleaning the surface of the catalytic metal substrate 101 may be omitted if necessary.

Next, referring to FIG. 5, a process of forming the graphene 110 proceeds.

The graphene 110 may be formed by a chemical vapor deposition (CVD) method, a thermal chemical vapor deposition (TCVD) method, a rapid thermal chemical vapor deposition (PTCVD) method, an inductively coupled plasma Various processes such as inductively coupled plasma chemical vapor deposition (ICP-CVD) and atomic layer deposition (ATLD) may be used.

When the catalytic metal substrate 101 is transported to the graphene formation chamber, a gaseous carbon source is introduced into the graphene formation chamber and is heat-treated. The heat treatment consists of heating and cooling. Specifically, an inert gas or an inert gas is injected into the graphene forming chamber, and then the internal space is heated. For example, the temperature of the interior space may be about 500 캜 or 1000 캜 or higher. Thereafter, the carbon source of the gas phase is supplied to the inner space.

A carbon source of the vapor is methane (CH 4), carbon monoxide (CO), ethane (C 2 H 6), ethylene (CH 2), ethanol (C 2 H 5), acetylene (C 2 H 2), propane (CH 3 CH 2 CH 3), propylene (C 3 H 6), butane (C 4 H 10), pentane (CH 3 (CH 2) 3 CH 3), pentene (C 5 H 10), dicyclopentadiene (C 5 H 6 carbon atoms such as hexane (C 6 H 14 ), cyclohexane (C 6 H 12 ), benzene (C 6 H 6 ), and toluene (C 7 H 8 ).

Such a gaseous carbon source is separated into carbon atoms and hydrogen atoms at high temperatures. The separated carbon atoms are deposited on the heated catalytic metal substrate 101 and the graphene 110 of FIG. 1 is formed as the catalytic metal substrate 101 is cooled.

Fig. 10 shows the temperature of the graphene forming chamber when the internal space is heated in the graphening step (I). In the case of the graphene forming process (I), the temperature values are the same because they are processes common to Example A and Comparative Example B of the present invention.

The graphene 110 may be formed on at least one side of the catalytic metal substrate 101. The graphene 110 may be formed on only one side of the catalytic metal substrate 101, but the graphene 110 may be formed on both sides of the catalytic metal substrate 101. Hereinafter, the remaining process will be described with reference to an example in which the graphene 110 is formed on one surface of the catalytic metal substrate 101. [

Next, referring to FIG. 6, the laminate 50 of FIG. 5 is bonded to one surface of the carrier tape 120 of FIG.

First, the laminate 50 of FIG. 5 and the carrier tape 120 of FIG. 2 are disposed such that the upper surface of the graphene 110 and the adhesive layer 122 of FIG. 2 face each other. Next, heat and pressure are applied to bond the laminate 50 of Fig. 5 and the carrier tape 120 to each other.

According to the embodiment A of the present invention, since the carrier tape 120 of FIG. 2 has an adhesive force at a temperature higher than the switching temperature Ts, the bonding step (II) of the carrier tape 120 is performed as shown in FIG. 10 As well as at a temperature higher than the switching temperature Ts. For example, if the switching temperature Ts of the carrier tape 120 is about 30 degrees Celsius, the present process can be performed at about 50 degrees Celsius to about 70 degrees Celsius. On the other hand, a step of pressing is carried out in order to prevent wrinkles or voids between the graphene 110 and the adhesive layer 122 (FIG. 2) when the carrier tape 120 is bonded.

However, unlike the embodiment A of the present invention, in the case of the comparative example B, the step of adhering the heat peeling tape to the laminate of Fig. 5 does not require high temperature and can be performed mainly at room temperature.

Next, referring to FIG. 7, the catalyst metal substrate 101 is removed from the laminate 60 of FIG.

The process of removing the catalytic metal substrate 101 may employ a wet etching process. However, the present invention is not limited to this, and it is possible to shorten the process time for removing the catalytic metal substrate 101 by adding a dry etching process for etching or polishing the one surface of the catalytic metal substrate 101 with plasma before the wet etching process have.

(NH 4 ) 2 S 2 O 8 ), hydrogen fluoride (HF), buffered oxide etch (BOE), ferric chloride (FeCl 3 ), and the like. iron nitrate (Fe (NO 3) 3) , may be used, such as yeomhwadong (CuCl 2), hydrogen peroxide (H 2 O 2), sulfuric acid (H 2 SO 4), and sodium persulfate (Na 2 S 2 O 8) . However, the present invention is not limited to this, and a solution of perhydrous sulfuric acid, which is a composition containing hydrogen peroxide (H 2 O 2 ), sulfuric acid (H 2 SO 4 ) and water (H 2 O)

 According to an embodiment A of the present invention, the catalytic metal removal step (III) can be performed at a temperature higher than the switching temperature Ts as shown in FIG. This is because, during the removal of the catalyst metal, the carrier tape 120 and the graphene 110 must be kept in a bonded state, and when the step of removing the catalyst metal is performed at a low temperature, It falls. For example, if the switching temperature Ts of the carrier tape 120 is about 30 degrees Celsius, the present process can be performed at about 30 degrees Celsius to about 50 degrees Celsius.

Meanwhile, in the case of the comparative example B similar to the embodiment A of the present invention, the temperature can be higher than the room temperature to accelerate the removal rate of the catalyst metal.

As a non-limiting example of the process of removing the catalytic metal substrate 101 using the catalytic metal removal liquid, Cu is used as the catalytic metal substrate 101, H 2 O 2 , H 2 SO 4, and water A solution of hydrous sulfuric acid can be used. As shown in Reaction Scheme 1 below, Cu is oxidized by H 2 O 2 to be converted to CuO, and CuO reacts with H 2 SO 4 to form CuSO 4 , which is a water soluble salt, The catalyst metal substrate 101 can be removed.

[Reaction Scheme 1]

Cu + H 2 O 2 ? CuO + H 2 O

[Reaction Scheme 2]

CuO + H 2 SO 4 → CuSO 4 + H 2 O

The step of removing the catalytic metal substrate 101 may further include a step of cleaning the catalytic metal removing liquid remaining in the laminate and a step of drying.

Next, referring to Fig. 8, the process of joining the laminate 70 of Fig. 7 to the target substrate 130 proceeds.

The target substrate 130 refers to the substrate on which the graphene 110 is finally formed. As the target substrate 130, at least one of polyethylene terephthalate (PET), polyimide (PI), polydimethylsiloxane (PDMS), plastic, glass, and metal may be used. It is not.

According to an embodiment A of the present invention, the target substrate bonding step (IV) can be performed by pressing at a temperature higher than the switching temperature Ts as shown in Fig. This is because the state in which the carrier tape 120 and the graphene 110 are bonded must be maintained while the target substrate 130 is bonded. Also, when the target substrate 130 is experimentally subjected to only pressing at room temperature, the target substrate 130 must be bonded to the target substrate 130 at a high temperature since the target substrate 130 is not bonded to the graphene 110. For example, if the switching temperature Ts of the carrier tape 120 is about 30 degrees Celsius, the present process can be performed at about 50 degrees Celsius to about 70 degrees Celsius.

However, unlike the embodiment A of the present invention, in the case of the comparative example B, since the temperature for holding the adhesion between the graphene 110 and the heat peeling tape 120 is not required, bonding of the target substrate 130 is performed only at room temperature .

Next, referring to Fig. 9, the carrier tape 120 is peeled from the laminate 80 of Fig.

First, after the stacked body 80 is transferred to the peeling chamber in Fig. 8, the internal temperature is lowered to the switching temperature Ts or lower by the cooling device. Next, a predetermined force is applied to peel the carrier tape 120 from the laminate 80 in Fig.

According to the embodiment A of the present invention, since the carrier tape 120 of FIG. 2 loses its adhesive force at a temperature lower than the switching temperature Ts, the carrier tape peeling step (V) Lt; RTI ID = 0.0 > Ts. ≪ / RTI > For example, if the switching temperature Td of the carrier tape 120 is about 30 degrees Celsius, the present process can be performed at room temperature, about 25 degrees Celsius or less.

However, unlike the embodiment A of the present invention, in the case of the comparative example B, the heat peeling tape must be carried out at a high temperature since the foaming cell must be foamed at high temperature to peel off. For example, the process of removing the thermal peel tape may be performed at about 100 degrees Celsius or more. Therefore, in the case of Comparative Example B, the heat peeling tape peeling process is performed in a high temperature chamber.

As described above, according to the embodiment of the present invention, since the high temperature process is not required when peeling the carrier tape 120, the production of the graphene film 90, which is not limited to the thickness and material of the target substrate 130, Possible features. An attempt has been made to form the graphene film 90 into a thinner film according to a user's request. For this purpose, the thickness of the target substrate 130 must be reduced. Since the graphene film manufacturing process using the heat peeling tape involves a high temperature process after the transfer of the target substrate 130, the target substrate 130 must use a material having heat resistance, and the thickness of the target substrate 130 There is a restriction that it can not be made to a thin film beyond a certain level. According to an embodiment of the present invention, there is no high temperature process after the transfer of the target substrate 130, so that the material of the target substrate 130 is not limited and the thickness of the target substrate 130 can be made ultra thin.

Further, according to the embodiment of the present invention, the graphene film 90 having less damage can be obtained. In the case of using the heat peeling tape, graphene 110 was often damaged by foaming of the foaming cell when peeling off the heat peeling tape. However, when the carrier tape 120 of FIG. 2 is used, it is not related to the foam cell, and this problem is fundamentally solved, so that a graphene film 90 having good electrical and optical characteristics can be obtained.

Next, though not shown, the graphene 110 doping process proceeds.

Doping may be performed to improve the electrical characteristics of the exposed graphene 110, which may be performed by dry doping or wet doping. Further, a protective film may be further adhered on the doped graphene 110.

Next, the graphene film 110 thus fabricated may further be subjected to an analysis process or the like which has no damage or has any electrical characteristic.

The target substrate 130 coated with the graphene 110 as described above may be referred to as a graphene film 90 and may be used as a transparent electrode film such as a flexible display, an organic light emitting device, or a solar cell.

The manufacturing process of the graphene film 110 described above is not limited to the description, and some of the steps may be changed, or some steps may be omitted or added.

11 is a graph showing the degree of change in adhesive force when the carrier tape 120 of FIG. 2 is repeatedly used.

11 is data showing the result of repeatedly performing adhesion and peeling of the carrier tape 120 in the process of manufacturing the graphene film shown in Figs. 4 to 9. Fig. 11 shows one cycle of the manufacturing process of the graphene film. The step of adhering the carrier tape 120 at each turn is performed at a temperature higher than the switching temperature Ts and the step of peeling the carrier tape 120 is performed at a temperature lower than the switching temperature Ts.

As can be seen from FIG. 11, it can be confirmed that the adhesion strength is maintained even if the carrier tape 120 of FIG. 2 is repeatedly used up to five times. Experimentally, in the case of the carrier tape 120 of FIG. 2, the adhesive strength is maintained at about 50% or more of the initial use adhesive strength when the adhesive tape is repeatedly used three times or more. Therefore, according to the embodiment of the present invention, the manufacturing cost can be reduced by manufacturing the graphene film 90 using the carrier tape 120 of FIG. 2 which can be repeatedly used.

On the other hand, a cleaning process for removing foreign matter and dust adhering to the carrier tape 120 before reusing the carrier tape 120 may be added.

FIG. 12 shows a method of manufacturing a graphene film according to an embodiment of the present invention by a roll-to-roll method. In the case of the roll-to-roll method, the continuous roll type catalytic metal film 101a and the carrier film 120a and the target film 130a are used. In the case of the roll-to-roll method, since the roll-type material is transported in one direction, mass production of the graphene film is possible.

First, the catalyst metal film 101a is prepared, and the catalyst metal film 101a is wound on the first take-up roll 10. The catalyst metal film 101a wound on the first roll 10 is transferred to the graphening step I chamber so that the catalyst metal film 101a on at least one side of the catalyst metal film 101a, A pin (110 of FIG. 5) is formed.

Next, the carrier film 120a wound on the second roll 20 is unwound, transferred to the carrier film bonding process (II) chamber, and then bonded to the fifth stacked body 50. The carrier film 120a and the fifth laminate 50 are adhered via the first heating-pressing roller set 21. That is, the first heating-pressing roller set 21 heats the carrier film 120a to have an adhesive force, and the carrier film 120a and the fifth laminate body 50 are pressed and adhered to form a sixth laminate body 60 ).

Next, the sixth laminate 60 is transferred to the catalytic metal removal process (III) chamber to remove the catalytic metal film 101a, whereby the seventh laminate 70 is produced.

Next, the target film 130a wound on the third take-up roll 30 is transferred to the target film joining process (IV) chamber and joined to the seventh laminate 70. [ The target film 130a and the tee laminate 70 are bonded through the second heating-pressing roller set 32. [ That is, the second heating-pressing roller set 32 heats the carrier film 120a to maintain the adhesive force, and the target film 130a and the seventh laminate 70 are pressed and adhered to form the eighth laminate 80 ).

Finally, the carrier film 120a is peeled from the eighth laminate 80 transferred to the chamber (V). This chamber contains a cooling device and maintains an internal temperature lower than the switching temperature Ts of the carrier film 120a. Therefore, the adhesive force of the carrier film 120a in this chamber is lost, and the carrier film 120a easily peels off from the eighth laminate 80. [ The peeled carrier film 120a is again collected in the fourth winding roll and reused.

The detailed description of each step of FIG. 12 has already been described with reference to FIG. 4 to FIG. 9 and FIG. 10, so that redundant description will be omitted.

While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the invention. Accordingly, the true scope of the present invention should be determined by the technical idea of the appended claims.

101: catalytic metal substrate 110: graphene
120: Carrier tape 130: Target substrate

Claims (6)

A method for producing a graphene film using a carrier tape having an adhesive force at a temperature higher than a switching temperature and losing an adhesive force at a temperature lower than the switching temperature,
Preparing a catalytic metal substrate on which graphene is synthesized on at least one side;
Bonding the carrier tape to the graphene at a temperature higher than the switching temperature;
Removing the catalyst metal substrate at a temperature higher than the switching temperature;
Bonding the graphene to a target substrate at a temperature greater than the switching temperature; And
And peeling the carrier tape at a temperature lower than the switching temperature,
Wherein the carrier tape maintains an adhesive force even when repeatedly used, and comprises a base layer and an adhesive layer contacting the base layer and including a semi-crystalline graft copolymer. delete delete The method according to claim 1,
Wherein the step of bonding the carrier tape to the graphene and the step of bonding the graphene to the target substrate are performed in a pressurized state. delete delete
KR1020130013495A 2013-02-06 2013-02-06 Method of manufacturing grapheme film KR101926488B1 (en)

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KR1020130013495A KR101926488B1 (en) 2013-02-06 2013-02-06 Method of manufacturing grapheme film
PCT/KR2014/000732 WO2014123319A1 (en) 2013-02-06 2014-01-27 Method for producing graphene film

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