KR101093657B1 - Fabrication method of graphene film by using joule heating - Google Patents

Fabrication method of graphene film by using joule heating Download PDF

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KR101093657B1
KR101093657B1 KR20090078057A KR20090078057A KR101093657B1 KR 101093657 B1 KR101093657 B1 KR 101093657B1 KR 20090078057 A KR20090078057 A KR 20090078057A KR 20090078057 A KR20090078057 A KR 20090078057A KR 101093657 B1 KR101093657 B1 KR 101093657B1
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metal film
graphene
graphitized metal
film
substrate
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KR20090078057A
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KR20110020444A (en
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박원일
이정민
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한양대학교 산학협력단
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

Abstract

It provides a graphene film manufacturing method using a heat resistance heating (joule heating). In the present invention, a substrate on which a graphitized metal film is formed is charged into a chamber, and a current is passed through at least one of the graphitized metal film and the substrate in the chamber to heat the graphitized metal film by the heat transfer effect at that time. By supplying a gaseous carbon source into the chamber to solidify a carbon component in the graphitized metal film while the graphitized metal film is heated, the amount of current is controlled to cool the graphitized metal film at a controlled rate. Graphene is deposited on the surface of the graphitized metal film from the solid solution of carbon.

Description

Graphene film manufacturing method using heat resistance heating method {Fabrication method of graphene film by using joule heating}

The present invention relates to a method for producing a graphene film, and more particularly, to a method for producing graphene by supplying a gaseous carbon source to a substrate on which a graphitized metal catalyst is formed.

Graphene is a material composed of carbon atoms bonded in two dimensions like graphite, and unlike graphite, it is formed as a single layer or a very thin layer of 2-3 layers. Since graphene is flexible, very high in electrical conductivity, and transparent, studies are being conducted to use it as a transparent and curved electrode or to use it as an electron transport material such as an electron transport layer in an electronic device.

Graphene has attracted much attention as an electron transport layer and a transparent electrode of an electronic device, in particular, using a photovoltaic principle of receiving light and converting it into electricity, such as a solar cell or a photodetector. Indium Tin Oxide (ITO) is the most widely used transparent electrode of electronic devices, but the manufacturing cost is increasing due to the price rise and depletion of indium (In), which is a main material. have.

Conventional methods for obtaining a graphene film include a micromechanical method and a SiC crystal pyrolysis method. The micromechanical method is to attach a scotch tape to a graphite sample and then remove it to obtain graphene in the form of a sheet separated from graphite on the scotch tape surface. In this case, the peeled off graphene sheet has a constant number of layers, and its shape is not constant due to the tearing of paper. Moreover, there is a disadvantage in that it is extremely difficult to obtain a graphene sheet in a large area. In the SiC crystal pyrolysis method, when SiC single crystal is heated, SiC on the surface is decomposed to remove Si and graphene is generated by the remaining carbon (C). In this method, SiC single crystals used as starting materials are very expensive, and graphene is very difficult to obtain in large areas.

Conventionally, a method of manufacturing a graphene film for transparent electrodes includes a method of obtaining a graphene film by coating a catalyst on graphite attached on a substrate, covering the polymer thereon, and heat treating the graphene to obtain graphene from the graphite, and then removing the substrate. This method produces a high quality graphene film, but the process is rather complicated.

Another method is to oxidize graphene, mix and disperse it in a solution, and then form it directly as an electrode or an electron transport layer through spin coating. The method of using oxidized graphene has advantages of simple and easy formation of large-area graphene film because it can use general polymer process such as spin coating, and it is simpler than the method of refining graphite. . However, since the graphene is oxidized, the electrical characteristics are lower than those of pure graphene, and the transparent electrode is divided into small pieces rather than a single thin film, and thus the characteristics of the transparent electrode are inferior to those of the conventional ITO.

The problem to be solved by the present invention is to provide a method for obtaining a high quality graphene film simply and easily in large area.

In the graphene film production method according to the present invention for solving the above problems it is proposed to produce a graphene by supplying a gaseous carbon source while heating the substrate on which the graphitized metal catalyst is formed by a joule heating. In the present invention, a substrate on which a graphitized metal film is formed is charged into a chamber, and a current is passed through at least one of the graphitized metal film and the substrate in the chamber to heat the graphitized metal film by the heat transfer effect at that time. By supplying a gaseous carbon source into the chamber to solidify a carbon component in the graphitized metal film while the graphitized metal film is heated, the amount of current is controlled to cool the graphitized metal film at a controlled rate. Graphene is deposited on the surface of the graphitized metal film from the solid solution of carbon.

The gaseous carbon source may comprise a CH 4 gas and may further supply hydrogen with the gaseous carbon source. The heating temperature of the graphitized metal film may be 600 to 1000 ° C. when supplying the gaseous carbon source, and the cooling rate of the graphitized metal film may be 1 to 50 ° C. per second when the graphene is deposited. The thickness of the precipitated graphene may be 1 to 1000nm, the graphitized metal film is Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Si, Ta, Ti, It may be at least one selected from the group consisting of W, U, V and Zr.

After the graphene precipitation may be further included by removing the graphitized metal film by an acid treatment, separating the precipitated graphene from the substrate. Graphene separated from the substrate has a film or sheet shape, which can be used as a transparent electrode of devices such as solar cells and photodetectors.

According to the present invention, a current is passed through at least one of the graphitized metal film and the substrate and the graphitized metal film is heated by the heat transfer effect at that time. That is, the heat resistance heating method is used. The electric field formed by the flowing current causes the particle size of the graphitized metal film to be large, thereby making the surface very flat. This makes it possible to obtain a higher quality graphene film.

Cooling, the last step in the graphene process, is the most important factor in controlling the quality of the graphene formed. In the present invention, cooling by adjusting the amount of current flowing in the heat resistance heating method without flowing an inert gas or using natural cooling. Since the thermal resistance can be precisely controlled by the amount of current, it is possible to accurately control the amount of heat generated accordingly, so that it is easy to adjust the cooling rate exactly to the desired cooling rate.

In addition, since the present invention can proceed at atmospheric pressure, the process is simple and mass production is possible, and the heater design is not a method of heating the substrate indirectly by the radiant heat of the resistance heater or the lamp, but directly by the heat resistance heating method. No change is necessary, which is advantageous for large area at low cost.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, the present invention is not limited to the embodiments disclosed below, but will be implemented in various forms, and only the present embodiments are intended to complete the disclosure of the present invention and to those skilled in the art to fully understand the scope of the invention. It is provided to inform you.

1 is a flowchart of the present invention, and FIGS. 2 to 4 are schematic implementation views accordingly.

First, a graphite metal film 20 is formed on the substrate 10 as shown in FIG. 2, and charged into the chamber 30 as shown in FIG. 3 (step S1 of FIG. 1).

The chamber 30 here is basically provided with a gas supply mechanism 35 capable of supplying various gases to the substrate 10 side so as to perform CVD. Although the gas supply mechanism 35 can be comprised by the showerhead normally used as the gas supply mechanism of this kind of apparatus, for example, it is not limited to this. After charging the substrate 10 on which the graphitized metal film 20 is formed into the chamber 30, air in the chamber 30 is removed using a pump or the like not shown. Thereafter, while maintaining the vacuum in the chamber 30, an appropriate atmospheric gas such as hydrogen and argon gas is flowed through the gas supply mechanism 35 at a ratio between 1: 1 and 1: 6 to maintain atmospheric pressure.

The substrate 10 is an auxiliary means for forming a graphene film, but the material of the substrate 10 does not matter much, but it must be able to withstand heating to around 1000 ° C. in a subsequent process and has a sheet shape separated from the substrate 10. In order to obtain a graphene film of, it is preferable to select a material that can be easily removed by acid treatment and the like. As the material of the substrate 10 that satisfies these properties and is not expensive and easily available, in this embodiment, a doped or undoped silicon substrate is adopted, and after forming the silicon oxide film 15 thereon, the graphitized metal film 20 ).

The graphitized metal film 20 is a film including a graphitized metal catalyst, the graphitized metal catalyst serves to help the carbon components are bonded to each other to form a hexagonal plate-like structure, for example to synthesize graphite or , A catalyst used to induce a carbonization reaction or to prepare carbon nanotubes can be used. More specifically, at least one metal selected from the group consisting of Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Si, Ta, Ti, W, U, V and Zr Or alloys can be used.

The graphitized metal film 20 may be formed by dissolving such a metal complex or an alkoxide of a metal in a solvent such as alcohol, and then applying the same to the substrate 10 to dry it. Or it may be formed by depositing on the substrate 10 by a metal deposition method such as thermal deposition.

In particular, in the chamber 30 used in the practice of the present invention, the electrode 40 is provided in the vicinity of both ends of the substrate 10, and the electrode 40 has a power source (50, DC or AC power supply) outside the chamber. When the electrode 40 is in contact with the substrate 10 on which the graphitized metal film 20 is formed, as shown in FIG. 3, the graphite is insulated when the substrate 10 is insulated like a undoped silicon substrate. A current may flow through the metallization film 20, and if the substrate 10 is a conductive substrate such as a doped silicon substrate, a current flows through at least one of the graphitized metal film 20 and the substrate 10. Can give The electrode 40 illustrated in FIG. 3 is a pair of electrodes extending along two opposite sides of the substrate 10 at both upper and lower ends of the substrate 10, but the shape of the electrode 40 is illustrated. Any structure can be used as long as it is not limited to the bar and the structure which can electrically conduct the graphitized metal film 20 and / or the board | substrate 10 evenly.

Next, an electric current flows in at least one of the graphitized metal film 20 and the substrate 10 in the chamber 30 while maintaining the atmospheric pressure, thereby heating the graphitized metal film 20 by the heat transfer effect at that time. (Step S2 of FIG. 1). That is, the temperature of the graphitized metal film 20 is raised by using a heat resistance heating method. Preferably the temperature is raised to 600 ~ 1000 ℃. Due to the heating effect at this time, the particle size of the graphitized metal film 20 increases, and the surface of the graphitized metal film 20 becomes flat.

As mentioned above, the electrode 40 in the chamber 30 is brought into contact with the substrate 10 so that the graphitized metal film 20 and / or the substrate 10 can be fed to the substrate 10 and the electrothermal effect at this time. The graphitized metal film 20 is heated. When the substrate 10 is insulative, the temperature is increased by direct heating of the graphitized metal film 20 while the graphitized metal film 20 is energized. Since the metal catalyst is formed in the form of a film and the electrode 40 is in contact with both ends of the substrate 10, the current can flow almost uniformly over the entire surface of the graphitized metal film 20. In this way, only the current is flowed through the graphitized metal film 20, and the entire graphitized metal film 20 is heated almost uniformly by the heat transfer effect without raising complicated control. When the substrate 10 is conductive, when the substrate 10 is energized, the substrate 10 generates heat and the graphitized metal film 20 formed thereon is easily heated.

In this step peculiar to the present invention, the graphitized metal film 20 becomes larger due to the heating effect as well as the additional effect of the electric field formed by the flowing current, thereby increasing the size of the metal particles constituting the graphitized metal film 20. As a result, the surface of the graphitized metal film 20 becomes very flat. In a subsequent process, the graphene is formed on the graphitized metal film 20 thus flattened so that the quality thereof is excellent.

Next, a gaseous carbon source is supplied into the chamber 30 through the gas supply mechanism 35 while the graphitized metal film 20 is heated to solidify a carbon component in the graphitized metal film 20 (FIG. 1). Step S3).

The gaseous carbon source may use a hydrocarbon gas family such as ethane, ethylene, ethanol, acetylene, propane, propylene, butane, butadiene, pentane, hexanes, and in particular may include CH 4 gas, You can supply more. In other words, CH 4 gas, which is a gaseous carbon source, can be supplied at this stage while continuously supplying a mixed gas of hydrogen-argon gas for maintaining the atmospheric pressure in the chamber 30. It is possible to adjust the amount of carbon component dissolved in the graphitized metal film 20 by adjusting the heating temperature, the time, the supply amount of the gaseous carbon source, etc. in this step. Increasing the amount of carbon component dissolved by increasing the time and supply amount may result in increasing the thickness of the graphene film, and conversely, decreasing the amount of carbon component by reducing the time and supply amount decreases the thickness of the graphene film. can do. If the supply is small, lengthening the time allows for the desired amount of carbon content to be dissolved.

In the processing of the substrate which normally requires heating, a method of heating the substrate indirectly by radiant heat of a resistance heater or a lamp is mainly used. In recent years, due to the increase in the size of a thin film display, the increase in the demand for inexpensive solar panels, and the like, it is required to increase the size of the graphene film for transparent electrodes. In order to obtain such a large graphene film, the substrate 10 as a substrate on which the graphene film is formed should be large. In the method of indirectly heating by radiation using a conventional resistance heater or lamp, the size of the heater is also increased. Since there is a need to do so, an increase in manufacturing cost is concerned.

However, in the present invention, since the substrate 10 and / or the graphitized metal film 20 are directly energized and heated by using a heat resistance heating method, the substrate 10 and / or the graphitized metal film 20 can be efficiently heated by a simple configuration and there is no increase in manufacturing cost, and the substrate 10 It is possible to heat the graphitized metal film 20 not only when the insulation layer is insulating but also when it is conductive.

Next, the supply of the gaseous carbon source is stopped and the amount of current flowing in the heat resistance heating method is reduced to cool the graphitized metal film 20 at a controlled rate (step S4 of FIG. 20, graphene is deposited on the surface of the graphitized metal film 20 from the carbon component dissolved in 20, thereby forming a graphene film 60. As shown in FIG.

This cooling process is an important step to obtain high quality by uniformly depositing graphene, and rapid cooling can lead to obtaining graphene that is less than the desired thickness or to causing cracks in the resulting graphene film. Since the thickness is too thick or the productivity is impaired, it is desirable to cool it at a controlled constant rate if possible. The ideal cooling rate is 1 to 50 ° C per second, and most ideally 10 ° C per second.

Cooling after normal film formation is mainly performed by flowing inert gas or natural cooling. However, if the cooling using an inert gas after the production of the graphene as in the present invention, since the temperature is indirectly controlled by the inert gas, accurate temperature control is difficult. Natural cooling is a method that does not control the temperature at all, so if natural cooling is performed after the production of graphene as in the present invention, the process becomes simple, but the quality of graphene may be greatly degraded.

In the present invention, since the calorific value can be controlled by adjusting the amount of current, it is very easy to accurately control the cooling rate of the graphitized metal film 20 by changing the amount of current. Therefore, by using the cooling method as in the present invention it is possible to grow high quality graphene. The thickness of the graphene film 60 may be 1 to 1000nm, it is also possible to thicker than this. That is, the graphene film 60 may be formed of a thin film or a thick film.

Next, the graphene film 60 may be separated from the substrate 10 by removing the graphitized metal film 20 by acid treatment. In the embodiment, when the substrate 10 on which the graphene film 60 is formed is sequentially immersed in HF and TFG solutions, the silicon oxide film 15 and the graphitized metal film 20 are sequentially removed to remove the sheet-like graphene film 60. It can be extracted completely from the substrate 10.

As described above, according to the present invention, it is possible to raise the temperature of the graphitized metal film easily by using a heat resistance heating method, to flatten the surface of the graphitized metal film, and to form a high-quality graphene film by controlling the temperature during cooling. . In addition, since the present invention can proceed at atmospheric pressure, the process is simple and mass production is possible, and the heater design of the chamber is not required, and thus, it is advantageous for large area.

Experimental Example

The p-type silicon substrate on which SiO 2 was formed was sonicated with acetone and ethanol and then washed with deionized water (DI-water). The washed substrate was dried with N 2 gas and a Ni film was thermally evaporated at least 200 nm as a graphitized metal film on the substrate.

In order to carry out the method according to the present invention, a Ni film-deposited substrate was placed in a chamber for CVD rules, and the air was evacuated to create a vacuum state, and then filled with atmospheric pressure with a gas of 1: 4 mixed with hydrogen and argon. An electric current was made to flow through the board | substrate and Ni film | membrane in the state which maintained the normal pressure, and the temperature of the Ni film | membrane was raised to 800 degreeC, and Ni surface was made flat.

When heating using the heat resistance heating method, there are differences in current and voltage conditions depending on the size of the specimen and the doping concentration of the silicon substrate. Usually, a p-type silicon substrate, which is readily available, can be heated to 800-900 ° C by applying a voltage of 5-10V and a current of 10-20A when the specimen size is 1cm x 6cm. When the size of the specimen is 2.5cm x 6cm, it can be heated to 800 ~ 900 ℃ by flowing a voltage of 10 ~ 15V, current 20 ~ 30A.

While maintaining the surface of the Ni film at 800 ° C., CH 4 gas and hydrogen-argon mixed gas were respectively flowed at a rate of 50 sccm and 200 to 300 sccm for 30 seconds, and then cooled down to room temperature by 10 ° C. per second by reducing the amount of current.

FIG. 5A is a SEM photograph of a Ni-film thermally-deposited state (as-depo) as a graphitized metal film. The Ni film in the thermally evaporated state is a polycrystalline film made of particles of very small size, as shown in FIG. 5 (a), and the surface roughness is poor because it occupies a large portion of the interface between the particles.

Figure 5 (b) is a SEM photograph when the Ni film is simply heat-treated at 900 ℃ for 15 minutes in the furnace for comparison with the present invention, Figure 5 (c) is a Ni film and a substrate according to the present invention It is a SEM photograph when a Ni film is heat-treated by passing an electric current. At this time, the size of the specimen was 1cm x 5cm and a voltage of 10V and a current of 15A were flowed.

5 (b) and 5 (c) show that the particle size of Ni is increased and surface roughness is also improved as compared with FIG. It can be seen that even when the heat treatment at the same time and the same temperature (c), which is the case of applying heat treatment by applying the heat transfer effect at that time, does not use a current, the particle size becomes larger and the surface becomes flat. According to the present invention, since graphene is produced by supplying a gaseous carbon source on the Ni film having a flat surface in the state (c), graphene is formed in high quality.

Figure 6 is a SEM photograph showing that the graphene is grown on the Ni film by the heat resistance heating method according to the experimental example of the present invention. Graphene was formed by supplying a source of CH 4 gas on a Ni film having a flat surface, and the cooling rate was controlled to be constant. Thus, the graphene film formed was formed along the flat surface state of the Ni film and has excellent surface quality. You can see that.

The graphene-grown substrate was placed in an HF solution to etch SiO 2 , and then the Ni film was etched in a TFG solution to finally extract only a sheet-like graphene film. The graphene film was evaluated to have excellent mechanical and electrical properties such that it can be used as a transparent electrode of a device such as a solar cell or a photodetector.

Although the preferred embodiments of the present invention have been shown and described above, the present invention is not limited to the specific preferred embodiments described above, and the present invention belongs to the present invention without departing from the gist of the present invention as claimed in the claims. Various modifications can be made by those skilled in the art, and such changes are within the scope of the claims.

1 is a flow chart of the present invention.

2 to 4 are schematic implementation figures in accordance with the present invention.

Figure 5 is a SEM image of the surface of the Ni film in the thermally evaporated state, the Ni film heat-treated for comparison with the present invention, and the Ni film heat-treated by the heat resistance heating method according to the present invention.

6 is a SEM photograph showing the growth of graphene on the Ni film according to the experimental example of the present invention.

<Explanation of symbols for the main parts of the drawings>

10 ... substrate 15 ... silicon oxide

20 ... graphitized metal film 30 ... chamber

35 Gas supply mechanism 40 Electrode

50 ... power 60 ... graphene

Claims (8)

Charging a substrate in which a graphitized metal film is formed into a chamber; Heating the graphitized metal film by a heat resistance heating method by directly flowing a current to at least one of the graphitized metal film and the substrate in the chamber; Supplying a gaseous carbon source into the chamber while the graphitized metal film is heated to solidify a carbon component in the graphitized metal film; And Controlling the amount of current to cool the graphitized metal film at a controlled rate, thereby depositing graphene on the surface of the graphitized metal film from the solid solution carbon component. The method of claim 1, wherein the gaseous carbon source comprises CH 4 gas. The method of claim 1, further supplying hydrogen together with the gaseous carbon source. The method of claim 1, wherein the heating temperature of the graphitized metal film is 600 to 1000 ° C. while the gaseous carbon source is supplied. The method of claim 1, wherein the cooling rate of the graphitized metal film is 1 to 50 ° C. per second while depositing the graphene. The method of claim 1, wherein the deposited graphene has a thickness of 1 to 1000 nm. The method of claim 1, wherein the graphitized metal film is made of Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Si, Ta, Ti, W, U, V and Zr Graphene film production method characterized in that at least one selected from the group. The method of claim 1, further comprising separating the precipitated graphene from the substrate by removing the graphitized metal film by acid treatment.
KR20090078057A 2009-08-24 2009-08-24 Fabrication method of graphene film by using joule heating KR101093657B1 (en)

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US20120234240A1 (en) 2011-03-17 2012-09-20 Nps Corporation Graphene synthesis chamber and method of synthesizing graphene by using the same
CN103534204A (en) * 2011-03-29 2014-01-22 国立大学法人蔚山科学技术大学校产学协力团 Graphene sheet, transparent electrode including graphene sheet, active layer, and display device, electronic device, photovoltaic device, battery, solar cell, and dye-sensitized solar cell employing transparent electrode
WO2012150761A1 (en) * 2011-05-03 2012-11-08 한국과학기술원 Method for manufacturing graphene and device for manufacturing graphene
KR101188988B1 (en) * 2011-05-23 2012-10-08 한양대학교 산학협력단 Method for seperating of graphene thin film
JP5862080B2 (en) * 2011-07-06 2016-02-16 ソニー株式会社 Graphene production method and graphene production apparatus
KR101878735B1 (en) * 2011-07-29 2018-07-17 삼성전자주식회사 Process for preparing graphene sheet
KR101465419B1 (en) * 2012-12-17 2014-12-01 (주)우주일렉트로닉스 Pruducing method for graphite sheet
KR102650379B1 (en) 2017-09-28 2024-03-25 아톰 드레드즈 코퍼레이션 Graphene fiber manufactured by joule heating and fabricating method of the same
CN112678808B (en) * 2020-12-24 2021-08-03 广东工业大学 Device and method for producing graphene by electric impact method
KR102477237B1 (en) * 2022-07-05 2022-12-14 (주)스피너스 Method for mamufacturing graphene

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