KR101654043B1 - Method for manufacturing graphene - Google Patents

Method for manufacturing graphene Download PDF

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Publication number
KR101654043B1
KR101654043B1 KR1020160019552A KR20160019552A KR101654043B1 KR 101654043 B1 KR101654043 B1 KR 101654043B1 KR 1020160019552 A KR1020160019552 A KR 1020160019552A KR 20160019552 A KR20160019552 A KR 20160019552A KR 101654043 B1 KR101654043 B1 KR 101654043B1
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KR
South Korea
Prior art keywords
graphene
film
basic cleaning
cleaning liquid
cleaning solution
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KR1020160019552A
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Korean (ko)
Inventor
김찬웅
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주식회사 가온인터내셔널
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    • C01B31/0469—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/044—Cleaning involving contact with liquid using agitated containers in which the liquid and articles or material are placed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/102—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration with means for agitating the liquid
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble compounds
    • C11D7/10—Salts
    • C11D7/12—Carbonates bicarbonates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B2203/00—Details of cleaning machines or methods involving the use or presence of liquid or steam
    • B08B2203/02—Details of machines or methods for cleaning by the force of jets or sprays

Abstract

The present invention provides a synthesis method of graphene, in which foreign materials attached to graphene can be removed effectively by washing the synthesized graphene with an alkaline washing solution during synthesis of graphene. The synthesis method of graphene according to the present invention comprises: a step for attaching synthesized graphene on a film; a step for washing the graphene attached on the film with an alkaline washing solution to remove foreign materials attached on the graphene; a step for drying the graphene attached on the film to remove the alkaline washing solution from the graphene; and a step for releasing the graphene from the film. By washing the graphene attached on the film with the alkaline washing solution, the synthesis method of graphene according to the present invention can effectively remove various foreign materials, such as organic materials including residual resin on the film and graphene, or materials attached on the graphene during an etching process (metal ions from catalysts, ions in etching solutions, etc.).

Description

{METHOD FOR MANUFACTURING GRAPHENE}

The present invention relates to a graphene production method, and more particularly, to a graphene production method capable of producing high quality graphene by washing synthesized graphene through a cleaning process.

As is well known, graphene is a conductive material having a thickness of one layer of atoms, with the carbon atoms forming a honeycomb arrangement in a two-dimensional fashion. It has become an important model for studying various low-dimensional nano phenomena as graphite when accumulated in three dimensions, carbon nanotubes when dried one-dimensionally, and fullerene as a zero-dimensional structure when it is in a ball shape.

Graphene is not only very stable both structurally and chemically, but it is also known to be a very good conductor that can transport electrons 100 times faster than silicon and about 100 times more current than copper. The characteristics of graphene were experimentally confirmed in 2004, when the method of separating graphene from graphite was found.

Graphene is made of only carbon, which is a relatively light element, which makes it very easy to fabricate 1D or 2D nanopatterns, which can control the semiconductor-conductor properties. In addition, by using the variety of chemical bonds of carbon, it is possible to manufacture a wide variety of functional devices such as sensors and memories.

Graphene has the advantage of being able to be synthesized and patterned in a relatively simple manner while having excellent stretchability, flexibility and transparency. In OLEDs and organic solar cells, which are currently under widespread use, the use of conventional inorganic-based electrodes degrades electrode characteristics due to differences in work function of the contact sites. When graphene is used, the work function difference This problem can be solved easily because it is not large. Graphene transparent electrodes are expected to revolutionize the entire next-generation flexible electronic industry technology as well as import substitution effects through the establishment of mass production technology in the future.

Graphene is largely manufactured using mechanical stripping, chemical vapor deposition, epitaxial synthesis, or chemical stripping. Among them, the chemical vapor deposition method can control the number of graphene layers by controlling the type and thickness of the catalyst, the reaction time, the cooling rate, and the concentration of the reaction gas, and has a surface resistance and a transparency Graphene can be produced.

In a simple chemical vapor deposition method, copper or the like to be used as a catalyst layer is deposited on a substrate, and reacted with methane and hydrogen mixed gas at a high temperature of about 1000 degrees Celsius so that an appropriate amount of carbon is dissolved or adsorbed in the catalyst layer. After cooling, the carbon atoms contained in the catalyst layer are crystallized on the surface to form a graphene crystal structure. The graphene thus synthesized can be separated from the substrate by etching the catalyst layer and then used for a desired application.

During the production of graphene by chemical vapor deposition, foreign substances such as etchant ions and organic substances are likely to adhere to the graphene during the etching of the catalyst layer. However, since foreign materials such as organic substances can not be easily removed by a cleaning process using a cleaning liquid such as deionized water, graphene produced by a conventional manufacturing method has a problem of poor quality such as permeability.

Patent Registration No. 1560029 (Oct. 26, 2015)

Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made to solve the above problems occurring in the prior art, and it is an object of the present invention to provide a graphene fabrication method capable of effectively removing foreign substances on graphene by washing the graphene synthesized in the graphene production process with a basic cleaning solution .

According to an aspect of the present invention, there is provided a method of manufacturing a graphene comprising the steps of: (a) attaching a graphene to a film; (b) washing the graphene adhering to the film with a basic cleaning solution to remove foreign substances adhering to the graphene; (c) drying the graphene adhered to the film to remove the basic cleaning solution from the graphene; And (d) peeling the graphene from the film.

The basic cleaning liquid may include sodium carbonate (Na2CO3).

The basic cleaning liquid may contain 1-3 wt% sodium carbonate (Na 2 CO 3) and 97-99 wt% deionized water.

The step (b) may include immersing the graphene attached to the film in the basic cleaning solution.

The step (b) may further include flowing the basic cleaning liquid around the graphene immersed in the basic cleaning liquid.

In the step (b), the basic cleaning liquid may be flowed around the graphene by spraying the basic cleaning liquid toward the graphen with a nozzle installed so as to be submerged in the basic cleaning liquid.

The step (b) includes the step of winding the film with the graphene on a drum type jig and immersing the film in the basic cleaning solution, and flowing the basic cleaning solution around the graphene immersed in the basic cleaning solution can do.

In the step (b), the basic cleaning liquid may be flowed around the graphene by spraying the basic cleaning liquid toward the graphen with a nozzle installed so as to be submerged in the basic cleaning liquid.

The step (b) may rotate the drum type jig in which the film is wound to flow the basic cleaning liquid around the graphene.

The method of manufacturing graphene according to the present invention is a method of manufacturing a graphene film by cleaning an organic material such as a resin remaining in the film and graphene by washing the graphene adhered to the film with a basic cleaning liquid or an organic material such as a catalyst metal ion, ) Can be effectively removed. By removing various defects from the graphene, defects can be reduced when transferring the graphene to another substrate, and the transmittance of graphene can be improved.

FIG. 1 is a step-by-step view illustrating a method of manufacturing a graphene according to an embodiment of the present invention.
FIG. 2 is a front view of a process tank containing graphene to illustrate another embodiment of the graphene cleaning process in the method of manufacturing graphene according to the present invention.
Fig. 3 is a side view of the process tank containing graphene to explain the graphene cleaning process shown in Fig. 2. Fig.

Hereinafter, a method of manufacturing graphene according to the present invention will be described in detail with reference to the drawings.

FIG. 1 is a step-by-step view illustrating a method of manufacturing a graphene according to an embodiment of the present invention.

1, the method of manufacturing graphene according to an embodiment of the present invention includes the steps of synthesizing graphene 10, attaching the synthesized graphene 10 to the film 30, And cleaning the graphene 10 attached to the base 30 with a basic cleaning liquid S. The graphene 10 thus produced can be used as various functional elements by being separated from the film 30 and transferred to another substrate or the like.

In the step of synthesizing the graphene 10, various graphene synthesis methods can be used. In this embodiment, graphene synthesis using chemical vapor deposition (CVD) is taken as an example.

In the graphene synthesis step using the chemical vapor deposition method, first, a metal catalyst layer 20 is prepared as shown in Fig. 1 (a). The metal catalyst layer 20 may be formed of a metal such as Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Si, Ta, Ti, W, U, V, Zr, Ge, ), Bronze, white copper, stainless steel, and combinations thereof. Next, the graphene 10 is synthesized on the metal catalyst layer 20. Since the method of synthesizing the graphene 10 on the metal catalyst layer 20 is well known, a detailed description thereof will be omitted.

After the synthesis of the graphene 10, the graphene 10 is attached to the film 30 as shown in Fig. 1 (c). It is possible to attach the thin film 10 to the film 30 by attaching the film 30 to one surface of the metal catalyst layer 20 on which the graphene 10 is formed. As the film 30, various types of graphene 10, such as a thermal release film, which are not corroded or damaged in a subsequent etching process can be used without being crushed.

Next, the metal catalyst layer 20 is removed through an etching process. Various known methods can be used for the etching process. After the etching process, the graphene 10 is exposed to the outside in a state of being attached to the film 30. During the etching process, the graphene 10 is provided with an organic material such as a material (catalyst metal ion (e.g. Cu ion), etchant ion (e.g., So4 ion) Foreign matter can stick. Foreign matter may lead to defects of the graphene 10, such as causing the graphene 10 to be colored or degrading the transparency of the graphene 10.

After the etching process, a cleaning process is performed to remove defects of the graphene 10 due to such foreign substances. The cleaning step is a step of cleaning the graphene 10 attached to the film 30 with the basic cleaning liquid S. The cleaning process may be performed in the same manner as shown in Fig. 1 (d). A basic cleaning liquid (S) is used for the cleaning process. By immersing the basic cleaning liquid S in the processing tank 40 and immersing the film 30 having the graphene 10 in the basic cleaning liquid S, foreign substances such as organic substances sticking to the graphene 10 are effectively Can be removed.

As the basic cleaning liquid (S), a solution containing various bases may be used. Since a strong basic solution may damage the graphene (10), a weakly basic solution is preferably used. As the basic cleaning liquid (S), a solution containing sodium carbonate (Na2CO3) may be used. Sodium carbonate (Na2CO3) can be added to deionized water to make a basic basic cleaning solution (S). A basic cleaning liquid (S) containing 1 to 3 wt% of sodium carbonate (Na 2 CO 3) and 97 to 99 wt% of deionized water can be used as the basic cleaning liquid (S) capable of improving the cleaning efficiency while preventing damage to the graphene have. The basic cleaning liquid having a sodium carbonate (Na2CO3) content of less than 1 wt% has a poor cleaning efficiency of graphene 10 and the basic cleaning liquid having a sodium carbonate (Na2CO3) content of more than 3 wt% The effect of increasing the cleaning efficiency is small and it is inefficient only to increase the consumption of sodium carbonate (Na2CO3).

The basic cleaning liquid S is caused to flow around the graphene 10 in a state in which the graphene 10 is immersed in the basic cleaning liquid S in order to improve the cleaning efficiency of the graphene 10 by the basic cleaning liquid S good. 1 (d), a nozzle 45 is provided inside the process tank 40, and a basic cleaning liquid S is sprayed toward the graphen 10 by the nozzle 45, The basic cleaning liquid S can flow. Various other methods other than the method using the nozzle 45 as shown in the drawing may be used as a method of flowing the basic cleaning liquid S around the graphen 10 during the cleaning process.

Organic materials such as resin remaining in the film 30 and the graphen 10 are removed by washing the graphene 10 attached to the film 30 with the basic cleaning liquid S and the organic material such as resin sticking to the graphen 10 during the etching process It is possible to effectively remove various foreign substances such as substances (catalyst metal ions (e.g., Cu ions), etchant ions (e.g., So4 ions), etc.). By removing various defect inducing materials from the graphene 10, defects can be reduced when transferring the graphene 10 to another substrate, and the transmittance of graphene can be improved.

When the cleaning process is completed, the film 30 with the graphene 10 attached thereto is taken out from the basic cleaning liquid S to dry the graphene 10, and the graphene 10 is peeled off from the film 30. Various methods can be used as the method of peeling the graphene 10 from the film 30. For example, when a heat peelable film is used as the film 30, the graphene 10 may be peeled off from the film 30 by applying heat to the film 30. That is, the film 30 on which the graphene 10 is attached is laminated on the substrate so that the graphene 10 is in contact with one side of the substrate, heat is applied to the film 30, The graphene 10 can be separated from the film 30 and transferred to the substrate.

Various functional elements can be manufactured by separating the graphene 10 from the film 30 and transferring it to another substrate or the like. Particularly, since the graphene 10 manufactured by the graphene manufacturing method according to the present embodiment is excellent in transmittance, it can be applied to a transparent electronic device such as an OLED and exhibit excellent performance.

FIGS. 2 and 3 illustrate graphene fabrication processes according to the present invention, in which graphene process tanks are cut from the front and side surfaces, respectively, in order to explain another embodiment of the graphene cleaning process.

2 and 3, the film 50 on which the graphene 10 is attached is wound around a drum-type jig 60 provided so as to be submerged in the basic cleaning liquid S to clean the graphene 10 . The drum type jig 60 is rotatably installed inside the process tank 70 in which the basic cleaning liquid S is filled. The drum type jig 60 is engaged with the rotation axis 82 of the drum type jig driver 80 and rotated by the drum type jig driver 80. A plurality of nozzles 90 are disposed inside the process tank 70 toward the drum-type jig 60. The nozzle 90 ejects the basic cleaning liquid S toward the film 50 wound on the drum-shaped jig 60.

During the cleaning process, the film 50 with the graphene 10 is wound around the drum-shaped jig 60 so that the graphene 10 is disposed on the outer side and placed inside the process tank 70, ) Can be filled with a basic cleaning liquid (S) to remove foreign substances sticking to the graphene (10) with a basic cleaning liquid (S). As the basic cleaning liquid (S), the same materials as those described above can be used. When the drum type jig 60 is rotated by the drum type jig driving device 80 while the drum type jig 60 is immersed in the basic washing liquid S and the drum type jig 60 is rotated around the graphen 10 disposed on the outer peripheral surface of the drum type jig 60 The basic washing liquid (S) can be flown, and the cleaning efficiency by the basic washing liquid (S) can be increased. When the basic cleaning liquid S is sprayed toward the drum type jig 60 by the plurality of nozzles 90 while rotating the drum type jig 60, the flow of the basic cleaning liquid S around the graphen 10 becomes more active So that the cleaning efficiency for the graphene 10 can be further improved.

The cleaning method using the drum type jig 60 is advantageous for cleaning the large-area graphen 10. That is, by carrying out the cleaning process by winding the large area graphene 10 around the outer circumferential surface of the drum-type jig 60, the risk that the graphene 10 is damaged, such as being crumpled, It is possible to perform cleaning work in a smaller space than flat cleaning method. By rotating the drum type jig 60 by winding the graphene 10 around the drum type jig 60, it is possible to make a flow of the basic cleaning liquid S uniform over the entire graphene 10, ) Can be increased.

As a method of flowing the basic cleaning liquid S around the graphen 10 wrapped around the drum-type jig 60, only the method of discharging the use of the nozzle 90 and rotating the drum-type jig 60 may be used. Or by simply spraying the basic washing liquid S onto the drum type jig 60 with the nozzle 90 being rotated without rotating the drum type jig 60 by rotating the drum type jig 60, (S). In addition, it is possible to make a flow of the basic cleaning liquid S around the graphene 10 by various other methods such as a method of flowing the basic cleaning liquid S in the process tank 70.

In the case of the graphene manufacturing method using such a cleaning method, the drum type jig 60 and the process tank 70 may be used in the etching process. That is, the film 50 is attached to the metal catalyst layer 20 and the graphene 10 in a state in which the film 50 is attached to the graphene 10 synthesized on the metal catalyst layer 20 (see FIG. 1) The metal catalyst layer 20 can be etched in a state in which the graphene 10 is wound around the drum-shaped jig 60 by being wound around the drum 60 and filling the process tank 70 with the etching solution. When the etching process is completed, the etching liquid is discharged from the process tank 70 and then the basic cleaning liquid S is filled, so that the graphen 10 wound around the drum-type jig 60 is not separated from the drum-type jig 60 The cleaning process can be performed immediately. By performing the etching process and the cleaning process while the graphen 10 is wound around the drum-shaped jig 60, the overall manufacturing time can be shortened.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. Those skilled in the art will appreciate that numerous modifications and variations can be made in the present invention without departing from the spirit and scope of the appended claims.

10: graphene 20: metal catalyst layer
30, 50: Film 40, 70: Process tank
45, 90: Nozzle 60: Drum type jig
80: Drum type jig driver 82:
S: Basic cleaning liquid

Claims (9)

(a) attaching the synthesized graphene to a film;
(b) washing the graphene adhering to the film with a basic cleaning solution to remove foreign substances adhering to the graphene;
(c) drying the graphene adhered to the film to remove the basic cleaning solution from the graphene; And
(d) peeling the graphene from the film,
Wherein the basic cleaning liquid is a mixture of sodium carbonate (Na2CO3) and deionized water. delete The method according to claim 1,
Wherein the basic cleaning solution contains 1-3 wt% sodium carbonate (Na2CO3) and 97-99 wt% deionized water. The method according to claim 1,
Wherein the step (b) comprises dipping the graphene attached to the film in the basic cleaning solution. 5. The method of claim 4,
Wherein the step (b) further comprises flowing the basic cleaning solution around the graphene immersed in the basic cleaning solution. 6. The method of claim 5,
Wherein the step (b) comprises injecting the basic cleaning solution toward the graphene by a nozzle installed so as to be submerged in the basic cleaning solution, thereby flowing the basic cleaning solution around the graphene. The method according to claim 1,
The step (b)
Winding the film with the graphene on a drum type jig and immersing the film in the basic cleaning liquid,
And flowing the basic cleaning liquid around the graphenes immersed in the basic cleaning liquid. 8. The method of claim 7,
Wherein the step (b) comprises injecting the basic cleaning solution toward the graphene by a nozzle installed so as to be submerged in the basic cleaning solution, thereby flowing the basic cleaning solution around the graphene. 8. The method of claim 7,
Wherein the step (b) comprises rotating the drum-type jig in which the film is wound to flow the basic cleaning liquid around the graphene.
KR1020160019552A 2016-02-19 2016-02-19 Method for manufacturing graphene KR101654043B1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113522816A (en) * 2021-06-16 2021-10-22 苏州世沃电子科技有限公司 Graphene cooling fin cleaning device for smart phone processing and cleaning method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20120052648A (en) * 2010-11-16 2012-05-24 삼성테크윈 주식회사 Apparatus for transferring graphene and method for transferring graphene
JP2013245116A (en) * 2012-05-23 2013-12-09 Osaka Gas Co Ltd Graphene sheet aqueous dispersion, method for producing the same, and graphene-containing structure
KR101560029B1 (en) 2012-05-07 2015-10-26 성균관대학교산학협력단 Direct transfer methods of graphene

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20120052648A (en) * 2010-11-16 2012-05-24 삼성테크윈 주식회사 Apparatus for transferring graphene and method for transferring graphene
KR101560029B1 (en) 2012-05-07 2015-10-26 성균관대학교산학협력단 Direct transfer methods of graphene
JP2013245116A (en) * 2012-05-23 2013-12-09 Osaka Gas Co Ltd Graphene sheet aqueous dispersion, method for producing the same, and graphene-containing structure

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113522816A (en) * 2021-06-16 2021-10-22 苏州世沃电子科技有限公司 Graphene cooling fin cleaning device for smart phone processing and cleaning method thereof

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