KR101900758B1 - Copper based thin metal layer and manufacturing method of graphene using the same - Google Patents

Copper based thin metal layer and manufacturing method of graphene using the same Download PDF

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KR101900758B1
KR101900758B1 KR1020110126273A KR20110126273A KR101900758B1 KR 101900758 B1 KR101900758 B1 KR 101900758B1 KR 1020110126273 A KR1020110126273 A KR 1020110126273A KR 20110126273 A KR20110126273 A KR 20110126273A KR 101900758 B1 KR101900758 B1 KR 101900758B1
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South Korea
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copper
thin film
metal thin
based metal
graphene
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KR1020110126273A
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Korean (ko)
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KR20130060005A (en
Inventor
윤종혁
나덕화
송영일
원동관
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한화에어로스페이스 주식회사
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Priority to KR1020110126273A priority Critical patent/KR101900758B1/en
Priority to CN201280058356.XA priority patent/CN103958730B/en
Priority to PCT/KR2012/008858 priority patent/WO2013081302A1/en
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • 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
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon

Abstract

The present invention relates to a copper-based metal thin film for catalytic metal for graphene synthesis, which comprises 0.001 to 0.05 wt% of silver and a method for producing graphene using the same.

Description

TECHNICAL FIELD [0001] The present invention relates to a metal thin film for graphene synthesis and a method for manufacturing graphene using the thin metal film.

The present invention relates to a metal thin film used for graphene synthesis and a method for producing graphene using the same.

Generally, graphite has a structure in which a plate-shaped two-dimensional graphene sheet in which carbon atoms are connected in a hexagonal shape is laminated. Recently graphene was stripped from graphite and its properties were investigated.

The most notable feature is that when electrons move from graphene, the mass of electrons flows like zero. This means that the electrons flow at the speed at which the light travels in the vacuum, that is, the light flux. Graphene also has an unusual half-integer quantum Hall effect on electrons and holes. Also, to date, the electron mobility of graphene is known to have a high value of about 20,000 to 50,000 cm 2 / Vs.

Chemical vapor deposition (CVD) may be used as a method for synthesizing graphene. However, in order to utilize it in various fields throughout the industry, research for manufacturing high-quality graphene must be continuously carried out.

One embodiment of the present invention relates to a copper-based metal thin film for synthesizing high-quality graphene and a graphene manufacturing method using the same.

According to one aspect of the present invention, there is provided a copper-based metal thin film for catalyst metal for graphene synthesis, which comprises 0.001 to 0.05 wt% of silver.

According to an aspect of the present invention, the size of the copper crystal grains of the copper-based metal thin film may be at least 20 μm or more.

According to another aspect of the present invention, at least one selected from the group consisting of S, As, Sb, Bi, Se, Te, Pb, and Sn and oxygen may be contained.

According to another aspect of the present invention, the oxygen content may be 0.01 to 0.05 wt%.

According to another aspect of the present invention, at least one selected from the group consisting of S, As, Sb, Bi, Se, Te, Pb and Sn may be contained in an amount of 0.003 wt% or less.

According to another aspect of the present invention, the thickness of the copper-based metal thin film may be 5 to 75 탆.

According to another aspect of the present invention, the copper crystal grains of the copper-based metal thin film oriented toward the (100) direction may be 80% or more.

According to another aspect of the present invention, the copper-based metal thin film can be produced by rolling.

According to another aspect of the present invention, there is provided a method of manufacturing a copper-based metal thin film, comprising: preparing a copper-based metal thin film containing 0.001 to 0.05 wt% of silver and having a copper grain size of at least 20 μm or more; And growing graphene on the copper-based metal thin film by reacting the copper-based metal thin film with a carbon-containing reaction gas and heat to produce graphene.

According to an aspect of the present invention, the thickness of the copper-based metal thin film may be 5 to 75 μm.

According to another aspect of the present invention, more than 80% of the copper grains of the copper-based metal thin film can be oriented in the same plane direction.

According to another aspect of the present invention, the plane direction may be a (1 0 0) direction.

According to another aspect of the present invention, the copper-based metal thin film may include at least one selected from the group consisting of S, As, Sb, Bi, Se, Te, Pb, and Sn and oxygen.

According to another aspect of the present invention, the oxygen content may be 0.01 to 0.05 wt%.

According to another aspect of the present invention, at least one selected from the group consisting of S, As, Sb, Bi, Se, Te, Pb and Sn may be contained in an amount of 0.003 wt% or less.

According to one embodiment of the present invention, high-quality graphene having uniform and improved sheet resistance characteristics can be produced.

1A and 1B are conceptual views schematically showing copper grains of a copper-based metal thin film according to an embodiment of the present invention and copper grains of a copper thin film according to a comparative example of the present invention.
2A shows an FIB-SIMS cross-sectional image of a copper-based metal thin film according to an embodiment of the present invention.
FIG. 2B shows an FIB-SIMS cross-sectional image of a copper thin film according to a comparative example of the present invention.
3A shows an EBSP image of a copper-based metal thin film according to an embodiment of the present invention.
3B shows an EBSP image of a copper thin film according to a comparative example of the present invention.
3C shows an EBSP in-situ determination range diagram.
4 is a flowchart schematically illustrating a process of manufacturing graphene using a copper-based metal thin film according to an embodiment of the present invention.

BRIEF DESCRIPTION OF THE DRAWINGS The advantages and features of the present invention, and the manner of achieving them, will be apparent from and elucidated with reference to the embodiments described hereinafter in conjunction with the accompanying drawings. The present invention may, however, be embodied in many different forms and should not be construed as being limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. Is provided to fully convey the scope of the invention to those skilled in the art, and the invention is only defined by the scope of the claims. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In the present specification, the singular form includes plural forms unless otherwise specified in the specification. It is noted that the terms "comprises" and / or "comprising" used in the specification are intended to be inclusive in a manner similar to the components, steps, operations, and / Or additions. The terms first, second, etc. 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.

(Copper-based metal thin film)

The copper-based metal thin film 100 according to the present invention basically includes copper and silver. Silver may be included in the range of about 0.001 to 0.05 wt%. If silver is contained in an amount less than 0.001 wt%, it is difficult to produce high-quality graphene because it can not have large-size copper grains. When silver is contained in an amount exceeding 0.05 wt%, copper grains May be difficult to form, and may be detrimental to graphene seed formation.

 The copper-based metal thin film 100 may be manufactured by rolling. In this case, the copper-based metal thin film 100 may be formed of at least one selected from the group consisting of S, As, Sb, Bi, Se, Te, Pb, And oxygen. Oxygen, and at least one element selected from S, As, Sb, Bi, Se, Te, Pb, and Sn may be included in an amount of about 0.003 wt% or less . ≪ / RTI >

1A and 1B are conceptual views schematically showing copper grains of a copper-based metal thin film according to an embodiment of the present invention and copper grains of a copper thin film according to a comparative example of the present invention.

1A and 1B, the size of the copper grains G1 of the copper-based metal thin film 100 containing 0.001 to 0.05 wt% of silver is determined by the size of the copper grains G2 of the copper thin film 10 according to the comparative example, As shown in FIG. The size of the copper grain represents the value measured by the linear crossing method. The straight line crossing method is a method of determining the size of a crystal grain by measuring the length of a crystal grain passing through an arbitrary straight line in an EBSD map or a microstructure image.

The phenomenon that the size of the copper grains G1 of the copper based thin film 100 containing 0.001 to 0.05 wt% of silver is larger than the size of the copper grains G2 of the copper thin film 10 according to the comparative example It is judged that the compositions of the copper-based metal thin film 100 are recrystallized in the rolling process to be described below, thereby helping the grain size G1 to be formed to be large.

As described above, the copper-based metal thin film 100 can be manufactured through a rolling process. Hereinafter, an example of a manufacturing process of the copper-based metal thin film 100 according to an embodiment of the present invention will be described.

First, a raw material is blended based on the composition of the copper-based metal thin film 100 set in advance, followed by melting and casting. That is, the alloy raw material constituting the metal thin film is appropriately introduced and dissolved, and then injected into a mold and solidified to cast a billet or the like. A casting body such as a billet may be subjected to a load-deformation process at an appropriate size, or a heat treatment may be applied to re-soften the cured billet by processing.

Thereafter, rolling is performed. Rolling can be repeatedly performed in the hot rolling process and the cold rolling process. For example, the step of annealing the hot-rolled cast body at a recrystallization temperature or higher and the cold rolling at a temperature lower than the recrystallization temperature can be repeatedly performed. Finally, the rolling step can be completed by cold rolling. Through such a rolling step, the cast body can be made of a copper-based thin metal plate having a thickness of about 5 to 75 μm. Through the rolling process, the copper-based metal thin film 100 including copper and silver is recrystallized.

The copper-based metal thin film 100 is recrystallized by rolling so that the size of the copper grains G1 is larger than that of the general copper thin film 10.

FIGS. 2A and 2B show FIB-SIMS cross-sectional images of a copper-based metal thin film according to an embodiment of the present invention, and FIG. 1B shows FIB-SIMS cross-sectional images of a copper thin film according to a comparative example of the present invention. Here, FIB-SIMS represents a focused ion beam instrument equipped with a secondary ion mass spectrometer. 2A shows an image of copper crystal grains of a copper-based metal thin film after recrystallization.

Referring to FIGS. 2A and 2B, it can be seen that the size of the copper grain G1 of the copper-based metal thin film 100 according to the embodiment of the present invention is larger. By adding silver, it is possible to form larger crystal grains G1, and such copper grains G1 favor the production of uniform quality graphenes.

FIG. 3A shows an EBSP image of a copper-based metal thin film according to an embodiment of the present invention, FIG. 3B shows an EBSP image of a copper thin film according to a comparative example of the present invention, and FIG. Here, EBSP represents an electron backscatter diffraction pattern.

Referring to FIG. 3A, it can be seen that a substantial portion of the copper grains of the copper-based metal thin film 100 according to the embodiment of the present invention are oriented in the same plane direction. That is, it is confirmed that more than 80% of the copper grains are uniformly oriented in the same plane direction in the (100) direction. On the other hand, referring to FIG. 3B, the copper thin film 10 according to the comparative example of the present invention shows various directions of crystal grains.

Since the copper-based metal thin film 100 according to the embodiment of the present invention is oriented in the same plane direction, the uniformity of graphene synthesized using such a copper-based metal thin film 100 can be improved.

Hereinafter, a process of manufacturing graphene using the copper-based metal thin film according to the present invention will be described with reference to FIG.

In step 410, a copper-based metal thin film 100 is prepared. The copper-based metal thin film 100 used in the manufacture of graphene may be a single layer of the copper-based metal thin film 100 described with reference to Figs. 1 to 3, or may be a single layer of the copper-based metal thin film 100 described with reference to Figs. 100) may be laminated on the base substrate. The concrete structure and characteristics of the copper-based metal thin film 100 are replaced with the contents described above.

For example, the copper based thin metal film 100 may be disposed inside the chamber for graphene synthesis. The inside of the chamber is kept in airtightness with the outside, and the reaction gas to be described below can be introduced.

In step 420, graphene is grown on the copper-based metal thin film 100 by reacting and reacting with the reaction gas containing carbon and heat.

Reaction gas containing carbon 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), hexane (C 6 H 14), cyclohexane (C 6 H 12), benzene (C 6 H 6), toluene (C 7 H 8), such as one selected from the included carbon atoms group or more may be used have.

The heat provided to the copper-based metal thin film 100 can decompose the reaction gas into carbon atoms and hydrogen atoms. The decomposed reaction gas reacts with the copper-based metal thin film 100 to grow graphene on the copper-based metal thin film 100.

As another embodiment of the present invention, the method may further include a pretreatment step of cleaning the surface of the copper-based metal thin film 100 prior to the step 420 of providing the carbon-containing reaction gas and heat. The pretreatment process is for removing foreign substances present on the surface of the copper-based metal thin film 100, and for example, a non-reactive gas such as hydrogen can be used.

In step 430, the copper-based metal thin film 100 on which graphenes are grown is cooled. Cooling can result in graphene having uniform alignment.

[Table 1] below is a table comparing the characteristics of graphene produced using the copper-based metal thin film according to the embodiment of the present invention. The left side of the table shows the characteristics of the graphene fabricated using the copper based metal thin film such as silver based copper thin film according to the embodiment of the present invention and the right side of the table shows the metal thin film according to the comparative example of the present invention It shows the characteristics of graphene fabricated using general copper thin film.

In both cases, a thin film having a thickness of 35 탆 was used, and all four graphenes were fabricated using the metal thin films according to Examples and Comparative Examples. The sheet resistance was measured at nine arbitrarily selected points for each graphene.

Example (35 占 퐉 silver + copper metal thin film) Comparative Example (Copper Thin Film of 35 占 퐉) Measuring point Sample 1 Sample 2 Sample 3 Sample 4 Sample 5 Sample 6 Sample 7 Sample 8 One 422 472 414 377 714 852 735 454 2 407 397 355 358 637 759 690 449 3 395 420 403 382 783 720 728 511 4 405 428 402 367 604 774 696 424 5 401 397 372 394 558 706 690 457 6 379 410 388 354 696 646 656 505 7 495 418 409 388 515 990 관 검출 이 478 8 403 381 367 386 548 709 probe
error 507 9 417 379 388 417 704 678 714 544 avg. 414 411 389 380 640 759 701 481 min. 379 379 355 354 515 646 656 424 max. 495 472 414 417 783 990 735 544 uniformity 14 11 8 8 21 23 6 12 total avg. 399 645 total
uniformity
10
15

The sheet resistance characteristics are as follows. Samples 1 to 4 of the graphene fabricated using the silver-based copper-based metal thin film according to the embodiment of the present invention show that the average sheet resistance per unit area is 399 Ω / sq., While the copper thin film according to the comparative example is used The average surface resistivity per unit area is 645 Ω / sq. The sheet resistance between the comparative example and the example shows a difference of about 246? / Sq.

On the other hand, the uniformity (%) is as follows. The uniformity can be obtained by [(max + min) / (2 * avg)]. The uniformity of sheet resistance of the graphene samples prepared using the copper-based metal thin film containing silver according to the embodiment of the present invention is about 10%, while the sheet resistance uniformity of the graphene samples produced using the copper thin film according to the comparative example is About 15%.

It can be seen that the graphene fabricated using the copper-based metal thin film according to the embodiment of the present invention is excellent both in sheet resistance and uniformity.

Although the present invention has been described in connection with the above-mentioned preferred embodiments, it is possible to make various modifications and variations without departing from the spirit and scope of the invention. Accordingly, it is intended that the appended claims cover all such modifications and variations as fall within the true spirit of the invention.

100: Copper-based metal thin film
10: Copper thin film according to comparative example
G1: Copper grain of copper-based metal thin film
G2: Copper grain of copper thin film according to comparative example

Claims (15)

delete delete delete delete delete delete delete delete Preparing a copper-based metal thin film containing 0.001 to 0.05 wt% of silver and having a thickness of 5 to 75 μm and a copper grain size of at least 20 μm or more; And
The copper-based metal thin film is reacted by supplying a reaction gas containing carbon and heat to the copper-based metal thin film to form an average sheet resistance of 420 Ω / sq. Or less of the graphene grains. delete 10. The method of claim 9,
Wherein at least 80% of the copper grains of the copper-based metal thin film are oriented in the same plane direction. 12. The method of claim 11,
Wherein the plane direction is a (1 0 0) direction. 10. The method of claim 9,
Wherein the copper-based metal thin film comprises at least one selected from the group consisting of S, As, Sb, Bi, Se, Te, Pb and Sn and oxygen. 14. The method of claim 13,
Wherein the content of oxygen is 0.01 to 0.05 wt%. 14. The method of claim 13,
Wherein at least one selected from among S, As, Sb, Bi, Se, Te, Pb and Sn is contained in an amount of 0.003 wt% or less.
KR1020110126273A 2011-11-29 2011-11-29 Copper based thin metal layer and manufacturing method of graphene using the same KR101900758B1 (en)

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KR1020110126273A KR101900758B1 (en) 2011-11-29 2011-11-29 Copper based thin metal layer and manufacturing method of graphene using the same
CN201280058356.XA CN103958730B (en) 2011-11-29 2012-10-29 For the synthesis of the thin metal film of Graphene and utilize its Graphene manufacture method
PCT/KR2012/008858 WO2013081302A1 (en) 2011-11-29 2012-10-29 Thin metal film for synthesizinggraphene and graphene manufacturing method using the same

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KR20170132450A (en) * 2016-05-24 2017-12-04 해성디에스 주식회사 Electric Wire Structure and the method of manufacturing thereof
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