KR20140133263A - Apparatus for manufacturing graphene, the manufacturing method using the same and the graphene manufactured by the same - Google Patents

Apparatus for manufacturing graphene, the manufacturing method using the same and the graphene manufactured by the same Download PDF

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Publication number
KR20140133263A
KR20140133263A KR1020130053200A KR20130053200A KR20140133263A KR 20140133263 A KR20140133263 A KR 20140133263A KR 1020130053200 A KR1020130053200 A KR 1020130053200A KR 20130053200 A KR20130053200 A KR 20130053200A KR 20140133263 A KR20140133263 A KR 20140133263A
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South Korea
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graphene
thermal expansion
axial direction
force
catalytic metal
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KR1020130053200A
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Korean (ko)
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문진산
김태형
최민석
정명희
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엘지전자 주식회사
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Priority to KR1020130053200A priority Critical patent/KR20140133263A/en
Publication of KR20140133263A publication Critical patent/KR20140133263A/en

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    • 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
    • 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]

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

Abstract

The present invention relates to graphene and, more specifically, to an apparatus to manufacture high quality graphene, a manufacturing method, and the manufactured graphene by the method and the apparatus. According to the present invention, the apparatus to manufacture graphene comprises: a chamber including a gas inlet and a gas outlet where catalyst metal is loaded; and a thermal expansion compensation unit installed in the heating unit of the chamber and allowed to compensate the difference of thermal expansion between the graphene and a catalyst metal.

Description

TECHNICAL FIELD [0001] The present invention relates to a graphene manufacturing apparatus, a manufacturing method thereof, and a graphene manufacturing method using the same,

TECHNICAL FIELD The present invention relates to graphene, and more particularly, to an apparatus, a manufacturing method, and graphene for manufacturing graphene capable of forming high quality graphene.

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.

Such graphene can be formed on a metal layer that is a catalyst substrate. However, graphene has a negative thermal expansion coefficient, but metal usually has a positive thermal expansion coefficient. Accordingly, wrinkles may occur in the graphene when the graphenes are formed due to the difference in thermal expansion coefficient.

SUMMARY OF THE INVENTION The present invention has been made in view of the above problems, and it is an object of the present invention to provide a graphene manufacturing apparatus capable of growing high quality graphene by compensating for a phenomenon that may occur due to a difference in thermal expansion between a catalytic metal and graphene formed on the catalytic metal. , A manufacturing method, and a graphene.

According to a first aspect of the present invention, there is provided an apparatus for producing graphene, comprising: a chamber including a gas inlet and an outlet and to which a catalyst metal is loaded; And a thermal expansion compensation unit positioned at one side of the heating region of the chamber to compensate for a difference in thermal expansion between the graphene and the catalytic metal.

Here, the thermal expansion compensation section may be located in a cooling region located outside the heating region.

The thermal expansion compensation unit may further include: a first portion for applying a force in the first axial direction of the catalytic metal; And a second portion for applying a second axial force perpendicular to the first axial direction of the catalytic metal.

At this time, the first axis direction may be a direction for supplying the catalyst metal into the chamber.

Further, the force applied in the first axial direction or the force applied in the second axial direction may have a range of 0.1 to 5 kg / m.

At this time, the force applied in the first axial direction can be applied by the roller supplying the catalytic metal.

On the other hand, at least one of the force applied in the first axial direction and the force applied in the second axial direction can be applied through the jig.

According to a first aspect of the present invention, there is provided a method of manufacturing graphene, comprising: loading a catalytic metal into a chamber; Feeding a carbon source into the chamber to form graphene on the catalytic metal; Cooling the catalyst metal; And compensating for thermal expansion between the catalyst metal and the graphene.

Here, compensating for the thermal expansion may include applying a force in a first axial direction which is the direction of feeding the catalytic metal into the chamber.

In addition, the step of compensating for the thermal expansion may further comprise the step of applying a force in a second axial direction perpendicular to the first axial direction of the catalytic metal.

At this time, the force applied in the first axial direction can be applied by the roller supplying the catalytic metal.

On the other hand, the force applied in the first axial direction or the force applied in the second axial direction may have a range of 0.1 to 5 kg / m.

Graphene produced by the method described above can be provided.

The present invention has the following effects.

It is possible to prevent the occurrence of wrinkles in the graphene formed on the catalyst metal by applying a force to the catalyst metal in at least one of a first axial direction force and a second axial direction force to compensate for the difference in thermal expansion.

Thus, the quality of graphene can be greatly improved by compensating for the difference in thermal expansion between graphene and the catalyst metal, and in particular, the electrical characteristics of graphene can be greatly improved.

1 is a schematic view showing an example of an apparatus for producing graphene.
2 is a schematic diagram showing the difference in thermal expansion between the catalytic metal and the graphene.
3 is a schematic view showing a thermal expansion compensation section.
Figure 4 is a photograph of a graphene grown without compensation for thermal expansion.
5 is a photograph of graphene grown by compensating for thermal expansion.
6 is a flowchart showing a method for producing graphene.

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 schematic view showing an example of an apparatus for producing graphene.

1, the apparatus for producing graphene includes a chamber 10 including a gas inlet 12 and an outlet 13, in which the catalyst metal 50 is loaded.

The loading of the catalytic metal 50 can be carried out in both a batch mode in which the catalytic metal 50 in the form of a single sheet can be supplied and a roller mode in which the catalytic metal 50 can be continuously supplied in the form of a roll.

1 shows a roller system including a supply roll 31 capable of supplying a catalytic metal 50 in the form of a roll and a winding roll 32 for winding the catalytic metal 50 through the chamber 10 have.

And a thermal expansion compensation unit 40 located at one side of the heating region 11 where the graphen is formed in the chamber 10 and compensating for the difference in thermal expansion between the graphene and the catalyst metal 50.

Here, the thermal expansion compensation section 40 may be located in a cooling region located outside the heating region 11.

The heating section 20 located in the chamber 10 may define a heating zone 11 on which the graphene may be formed on the catalytic metal 50 and may optionally be located outside the chamber 10 It is possible.

Here, the chamber 10 may be provided with a gas inlet 12 and a gas outlet 13. Therefore, the chamber 10 can be injected with a carbon source capable of forming graphene on the catalyst metal 50 through the inlet 12.

As described above, the catalytic metal 50 is heated in the heating zone 11 by using the heating unit 20, and a reaction gas (raw material gas), which is a gas containing carbon, is supplied as a carbon supply source, To form a graphene.

Such reaction gas (CxHx) is a compound containing carbon and may be a compound having not more than 6 carbon atoms, a compound having not more than 4 carbon atoms, or a compound having not more than 2 carbon atoms. As an example, a compound of carbon and hydrogen (CxHx) can be used as a reaction gas.

A cooling region in which the temperature of the catalytic metal 50 is rapidly lowered when the catalyst metal 50 is transferred out of the heating region 11 is positioned so that a cooling region can be defined from a portion where the catalyst metal 50 is out of the heating region 11 .

The thermal expansion compensation unit 40 includes a first portion 41 for applying a force in a first axial direction of the catalytic metal 50 and a second portion 41 for applying a force in a second axial direction perpendicular to the first axial direction of the catalytic metal 50 And a second portion 42 for applying a force.

Here, the first axis direction may be the direction of supplying the catalyst metal 50 into the chamber 10.

As described above, when the catalytic metal 50 is supplied in a roller manner including the supply roll 31 and the wind-up roll 32, the supply roll 31 and the wind- It is possible to apply tension in the axial direction.

It is also possible to apply the tension in the first axial direction by using the feed roller 41 located between the feed roll 31 and the take-up roll 32.

A tension adjusting unit (not shown) may be provided to adjust the tension applied to the catalyst metal 50 by adjusting the position of the feed roller 41. [

At this time, the force applied in the first axis direction or the force applied in the second axis direction may have a range of 0.1 to 5 kg / m.

On the other hand, the force applied in the second axial direction can be applied through the parallel moving device such as the jig 42. [

The jig 42 may be located just outside the heating zone 11 and may be located outside the chamber 10 in some cases. That is, it may be located at any position among the positions of the two jigs 42 shown in Fig.

If the catalytic metal 50 is not supplied in a roller manner, the force applied in the first axial direction can also be applied by using the jig 41a (see FIG. 3) That is, at a position adjacent to the heating region 11.

The thermal expansion compensation unit 40 compensates for the phenomenon that may occur due to the difference in thermal expansion between the catalytic metal 50 as shown in Fig. 2 and the graphene 60 formed on the catalytic metal 50 You can compensate.

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 catalyst metal 50 have. Also, the catalytic metal 50 is available in the form of a foil of approximately 10 [mu] m to 10 mm thickness.

This catalyst metal 50 has a positive thermal expansion coefficient, and has a thermal expansion coefficient of, for example, 16.4 ppm / K in the case of copper (Cu).

On the other hand, graphene 60 has a thermal expansion coefficient of -8 ppm / K. In the case of the graphene 60, the length thereof contracts as the heat increases.

Therefore, when the graphene 60 is formed on the catalyst metal 50 under the temperature condition of about 300 to 1500 ° C., the temperature of the catalyst metal 50 and the graphene 60 are rapidly And cooled.

At this time, as shown in Fig. 2, the catalyst metal 50 shrinks and the graphene 60 expands due to the difference in thermal expansion.

Therefore, it is possible to compensate for the phenomenon caused by thermal expansion by compensating such shrinkage of the catalytic metal 50 in the cooling region.

Fig. 3 is a schematic diagram illustrating the action of the thermal expansion compensating unit. Fig. 3 shows a state in which a force is applied to the catalytic metal 50 in one axial direction or two axial directions at one side of the heating region 11. Fig.

That is, it is possible to apply the force to the catalyst metal 50 in at least one direction of the force in the first axial direction and the force in the second axial direction.

At this time, the first axial direction may be exerted by the rollers 31, 32, 41 as a direction in which the catalyst metal 500 is fed. Therefore, it is preferable that the direction of the mechanical direction (LD). ≪ / RTI >

In addition, the second axial direction perpendicular to the first axial direction may be referred to as a transverse direction (TD).

As mentioned above, the force in the first axial direction MD can be exerted by the rollers 31, 32 and 41, but it can also be applied by using a parallel moving device such as the jig 41a.

When graphenes are formed in such a state that a force is applied to compensate for the difference in thermal expansion, many wrinkles are generated in the graphene, as shown in FIG. This adversely affects the electrical properties of graphene.

Thus, as noted above, thermal expansion compensation may be performed during the formation of graphene, particularly when the catalyst metal 50 is located in the cooling zone after passing through the cooling zone after formation of the graphene in the catalyst metal 50 Lt; / RTI >

That is, when the difference in thermal expansion is compensated for by applying a force to the catalytic metal 50 in at least one direction of the force in the first axial direction and the force in the second axial direction, it can be seen that wrinkles do not occur as shown in FIG. 5 .

Thus, by compensating for the difference in thermal expansion between the graphene and the catalytic metal 50, the quality of the graphene can be greatly improved. In particular, the electrical characteristics of the graphene can be greatly improved.

FIG. 6 is a flowchart showing a method of manufacturing graphene using the above-described manufacturing apparatus. Hereinafter, the manufacturing process of graphene will be described with reference to the drawings.

A process of loading the catalyst metal 50 into the chamber 10 using the supply roll 31 and the winding roll 32 and supplying the catalyst metal 50 to the heating region 11 is performed.

Thereafter, a carbon source and / or a carrier gas are supplied to the chamber 10, and the temperature is set to the appropriate condition using the heating unit 20. [

Next, when all the conditions are stabilized, the supply roll 31 and the wind-up roll 32 are driven to continuously form the graphene while moving the catalyst metal 50 (S20).

Graphene can be formed on the catalyst metal 50 using a chemical vapor deposition (CVD) method using the apparatus for producing graphene.

Thereafter, the graphene and the catalyst metal 50 are cooled (S30).

Specifically, the catalytic metal 50 and the graphene 60 formed on the catalytic metal 50 are rapidly cooled while the catalytic metal 50 passes through the heating zone 11 and the cooling zone.

At this time, as a cooling method in the cooling region, a method of natural cooling or cooling while flowing argon (Ar), nitrogen (N 2 ), or other gas may be used.

When the catalyst metal 50 passes the cooling region, the force is applied to at least one of the first axial direction coinciding with the supply direction MD of the catalytic metal 50 and the second axial direction TD perpendicular thereto Thereby compensating for the phenomenon that may occur due to the difference in thermal expansion (S40).

That is to say, tension is applied in the feeding direction MD of the catalytic metal 50 using the rollers 31, 32 and 41 or the jig 41a, It is possible to prevent the catalytic metal 50, which has thermally expanded, from being excessively contracted as compared with the graphene 60 by applying a tensile force in the direction TD perpendicular to the direction of the graphene 60. [

The process of applying the force to the catalyst metal 50 may be continuously performed during the graphening process.

On the other hand, as mentioned above, the process of applying the force to the catalytic metal 50 may be performed at a position outside the chamber 10.

By this process, after the graphene is formed on the catalyst metal 50, the temperature of the heating portion 20 is lowered.

Thereafter, a vacuum pump (not shown) may be operated to remove the residual reaction gas through the discharge port 13.

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: chamber 11: heating zone
12: inlet 13: outlet
20: Heating section 31: Feed roll
32: Winding roll 40: Thermal expansion compensation unit
41: first part, conveying roller 41a: jig
42: second part, jig 50: catalytic metal
60: Grain Fins

Claims (13)

In the apparatus for producing graphene,
A chamber including a gas inlet and an outlet and into which the catalyst metal is loaded; And
And a thermal expansion compensator positioned at one side of the heating region of the chamber to compensate for a difference in thermal expansion between the graphene and the catalytic metal. The apparatus of claim 1, wherein the thermal expansion compensation unit comprises:
And the heating region is located in a cooling region located outside the heating region. The apparatus of claim 1, wherein the thermal expansion compensation unit comprises:
A first portion for applying a force in a first axial direction of the catalytic metal; And
And a second portion for applying a force in a second axial direction perpendicular to the first axis direction of the catalytic metal. The apparatus according to claim 3, wherein the first axis direction is a direction for supplying the catalyst metal into the chamber. 4. The apparatus for manufacturing graphene according to claim 3, wherein the force applied in the first axis direction or the force applied in the second axis direction is in the range of 0.1 to 5 kg / m. The apparatus for manufacturing graphene according to claim 3, wherein the force applied in the first axis direction is applied by a roller for supplying the catalyst metal. 4. The apparatus according to claim 3, wherein at least one of a force applied in the first axial direction and a force applied in the second axial direction is applied through the jig. Loading a catalytic metal within the chamber;
Feeding a carbon source into the chamber to form graphene on the catalytic metal;
Cooling the catalyst metal; And
And compensating for thermal expansion between the catalyst metal and the graphene. 9. The method of claim 8, wherein compensating for thermal expansion comprises applying a force in a first axial direction that is a direction of feeding the catalytic metal into the chamber. 10. The method of claim 9, wherein compensating for the thermal expansion further comprises applying a force in a second axial direction perpendicular to a first axial direction of the catalytic metal. The method according to claim 8, wherein the force applied in the first axis direction is applied by a roller supplying the catalyst metal. The method according to claim 8, wherein the force applied in the first axis direction or the force applied in the second axis direction is in the range of 0.1 to 5 kg / m. A graphene produced by the method of any one of claims 8 to 12.
KR1020130053200A 2013-05-10 2013-05-10 Apparatus for manufacturing graphene, the manufacturing method using the same and the graphene manufactured by the same KR20140133263A (en)

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