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WO2014115942A1 - Appareil de synthèse de graphène et procédé associé l'utilisant - Google Patents

Appareil de synthèse de graphène et procédé associé l'utilisant Download PDF

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Publication number
WO2014115942A1
WO2014115942A1 PCT/KR2013/007568 KR2013007568W WO2014115942A1 WO 2014115942 A1 WO2014115942 A1 WO 2014115942A1 KR 2013007568 W KR2013007568 W KR 2013007568W WO 2014115942 A1 WO2014115942 A1 WO 2014115942A1
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Prior art keywords
substrates
auxiliary heating
graphene
heating unit
substrate
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Ceased
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PCT/KR2013/007568
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English (en)
Korean (ko)
Inventor
원동관
윤종혁
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Hanwha Vision Co Ltd
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Samsung Techwin Co Ltd
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Priority to CN201380071641.XA priority Critical patent/CN105246588B/zh
Publication of WO2014115942A1 publication Critical patent/WO2014115942A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B01J4/002—Nozzle-type elements
    • 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
    • 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
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/248—Reactors comprising multiple separated flow channels
    • B01J19/249—Plate-type reactors
    • 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
    • B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00139—Controlling the temperature using electromagnetic heating
    • B01J2219/00146—Infrared radiation
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0869—Feeding or evacuating the reactor
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0871—Heating or cooling of the reactor

Definitions

  • An embodiment of the present invention relates to a graphene synthesis device for synthesizing graphene and a graphene synthesis method using the same.
  • the present invention is derived from a study conducted as part of the industrial source technology development project of the Ministry of Knowledge Economy.
  • Graphene is a material in which carbon is connected to each other in a hexagonal shape to form a honeycomb two-dimensional planar structure, and its thickness is very thin, transparent, and has a very high electrical conductivity. Many attempts have been made to apply graphene to touch panels, transparent displays, or flexible displays by using these characteristics of graphene. As interest in graphene increases, a method for mass production of high quality graphene is required.
  • Graphene is synthesized on the surface of the catalytic metal by chemical vapor deposition (CVD) by introducing a gas containing carbon.
  • CVD chemical vapor deposition
  • a graphene synthesis apparatus that maintains a high temperature environment is required.
  • An embodiment of the present invention provides a graphene synthesis device for synthesizing a large amount of high quality graphene and a graphene synthesis method using the same.
  • a chamber defining an inner space in which a plurality of substrates disposed so that each surface is opposed to each other;
  • a gas supply unit supplying a gas containing carbon to the internal space;
  • a main heating unit radiating radiant heat to the inner space;
  • a first auxiliary heating part disposed to face one surface of the substrate in correspondence with the main heating part, and converting the radiant heat into convective heat and discharging the radiant heat into the inner space;
  • a plurality of second auxiliary heating parts disposed between the plurality of substrates so as to face at least one surface of the substrate and absorbing the radiant heat and the convective heat and then dissipating heat into the inner space. It provides a graphene synthesis device, including.
  • an auxiliary heating unit is provided between the plurality of substrates to evenly transfer heat to each substrate.
  • graphene is synthesized on each of the plurality of substrates, thereby allowing mass production of graphene.
  • the auxiliary heating unit disposed between the plurality of substrates has a feature that it is possible to synthesize high quality graphene by smoothing the flow of heat and gas flow.
  • FIG. 1 is a perspective view schematically showing the graphene referred to herein.
  • FIGS. 2 and 3 are perspective views schematically showing the graphene synthesis apparatus 100 according to an embodiment of the present invention.
  • FIG. 4 schematically illustrates a chamber 101 included in the graphene synthesis apparatus 100 shown in FIGS. 2 and 3.
  • FIG. 5 is a schematic front view of the graphene synthesizing apparatus 100 of FIG. 2.
  • FIG. 6 is a detailed view of portion V of FIG. 5.
  • FIG. 7 relates to a graphene synthesizing apparatus according to another embodiment of the present invention, and shows only the portion V in the front view of the graphene synthesizing apparatus illustrated in FIG. 4.
  • FIG. 8 and 9 illustrate a graphene synthesizing apparatus according to yet another embodiment of the present invention, and shows only the V portion in the front view of the graphene synthesizing apparatus shown in FIG. 4.
  • a chamber defining an inner space in which a plurality of substrates disposed so that each surface is opposed to each other;
  • a gas supply unit supplying a gas containing carbon to the internal space;
  • a main heating unit radiating radiant heat to the inner space;
  • a first auxiliary heating part disposed to face one surface of the substrate in correspondence with the main heating part, and converting the radiant heat into convective heat and discharging the radiant heat into the inner space;
  • a plurality of second auxiliary heating parts disposed between the plurality of substrates so as to face at least one surface of the substrate and absorbing the radiant heat and the convective heat and then dissipating heat into the inner space. It provides a graphene synthesis device, including.
  • At least one through hole is formed in at least one of the plurality of second auxiliary heating parts.
  • the second auxiliary heating unit includes a plurality of holes, and when the one side of the second auxiliary heating unit is divided into four quadrants, the holes are arranged such that each of the quadrants is symmetric with each other.
  • At least one of the plurality of second auxiliary heating parts has a mesh shape.
  • the second auxiliary heating unit is made of a material coated with graphite or oxide film.
  • the number of the plurality of second auxiliary heating parts is smaller than the number of the plurality of substrates.
  • At least one surface included in the plurality of substrates and the second auxiliary heating parts is disposed in the direction of gravity.
  • the gas supply unit and the discharge unit may be disposed in a direction crossing or perpendicular to a direction in which the plurality of substrates are arranged.
  • a step of placing a plurality of substrates in the interior space of the chamber; Depressurizing the internal space; Injecting an atmosphere gas into the internal space; Supplying a gas containing carbon to the internal space; And irradiating radiant heat for heating the substrates; And placing the substrates includes providing a plurality of auxiliary heating parts disposed between the plurality of substrates so as to face at least one surface of the substrate. do.
  • FIG. 1 is a perspective view schematically showing the graphene referred to herein.
  • graphene refers to a graphene in which a plurality of carbon atoms are covalently linked to each other to form a polycyclic aromatic molecule, which is formed in a film form.
  • a 6-membered ring is formed as a repeating unit, it is also possible to further include a 5-membered ring and / or a 7-membered ring.
  • the graphene film thus forms a single layer of covalently bonded carbon atoms (C) (usually sp2 bonds).
  • C covalently bonded carbon atoms
  • the graphene film may have various structures, and such a structure may vary depending on the content of 5-membered and / or 7-membered rings that may be included in graphene.
  • the graphene film may be formed of a single layer of graphene as shown, but they may be stacked with each other to form a plurality of layers, and the side end portion of the graphene may be saturated with a hydrogen atom (H). .
  • FIGS. 2 and 3 are perspective views schematically showing the graphene synthesis apparatus 100 according to an embodiment of the present invention. 4 schematically illustrates a chamber included in the graphene synthesizing apparatus 100 illustrated in FIGS. 2 and 3.
  • FIG. 5 is a front view schematically showing the graphene synthesizing apparatus 100 of FIG. 2, and FIG. 6 is a detailed view of part V of FIG. 5.
  • the substrates 1, 2, and 3 placed in the graphene synthesizing apparatus 100 are panel type.
  • the substrates 1a enclosed in the graphene synthesizing apparatus 100 are illustrated. (2a, 3a) is a roll type.
  • the panel type means that the substrate has a discontinuous panel form.
  • the roll type means that the substrate has a roll film form that is continuous in one direction.
  • the panel type has an advantage of easy handling, and the roll type has a feature suitable for a system that produces a large amount of graphene.
  • the substrate referred to herein may be a catalyst thin film for graphene growth, it will be described taking an example having a panel form for convenience.
  • Substrate 1, 2, 3 is copper (Cu), nickel (Ni), cobalt (Co), iron (Fe), platinum (Pt), gold (Au), silver (Ag), aluminum (Al), chromium (Cr), magnesium (Mg), manganese (Mn), molybdenum (Mo), rhodium (Rh), silicon (Si), tantalum (Ta), titanium (Ti), tungsten (W), uranium (U), At least among vanadium (V), palladium (Pd), yttrium (Y), zirconium (Zr), germanium (Ge), brass, bronze, white brass and stainless steel It may include one metal or alloy, but is not limited thereto.
  • the substrates 1, 2, and 3 may have a multilayer structure in which a catalyst metal film (not shown) is formed on a base layer (not shown).
  • the base layer may be formed of inorganic materials such as silicon (Si), glass, gallium nitride (GaN), silica, or metals such as nickel (Ni), copper (Cu), and tungsten (W).
  • the catalytic metal film can be formed on the base layer using a sputtering apparatus, an electron beam evaporation apparatus, or the like.
  • a plurality of substrates 1, 2, and 3 are disposed inside the graphene synthesis apparatus 100 to synthesize graphene in a large amount.
  • three substrates 1, 2, and 3 are shown in the drawing, the present invention is not limited thereto, and four or more substrates may be placed inside the graphene synthesis apparatus.
  • each substrate is referred to as a first substrate 1, a second substrate 2, and a third substrate 3 along the X-axis direction.
  • the graphene synthesizing apparatus 100 includes a chamber 101, a main heating unit 130, a first auxiliary heating unit 110, and a second auxiliary heating unit 120.
  • the gas supply unit 140, the discharge unit 150, a pressure reducing unit (not shown) and a gate (not shown) may be further provided.
  • FIG. 4 schematically illustrates a chamber 101 included in the graphene synthesis apparatus 100 shown in FIGS. 2 and 3.
  • 2 and 3 exemplarily show that the chamber 101 is a hexahedron. Therefore, each side of the cube required for the description below will be referred to as A1 to A6 plane as shown in FIG.
  • the shape of the chamber 101 is not limited to the illustrated hexahedron, for example, the chamber 101 may be provided in addition to the hexahedron, other polyhedrons, polygonal pillars, polygonal pyramids, or spheres.
  • the chamber 101 defines an internal space I in which the plurality of substrates 1, 2, 3 are seated.
  • the chamber 101 may be provided integrally, or may be a form in which a plurality of modules are assembled.
  • An inner space I may be provided with a support (not shown) for fixing the plurality of substrates 1, 2, and 3.
  • the main heating unit 130 irradiates radiant heat to the internal space I for the purpose of heating the plurality of substrates 1, 2, 3.
  • the radiant heat may be light including a near infrared wavelength band, but is not limited thereto and may be light of a mid infrared ray and a visible ray wavelength band. Light in the near infrared wavelength band may heat the substrate, and light in the mid-infrared or visible wavelength band may heat a gas including carbon supplied into the chamber 101.
  • the main heating unit 130 may be disposed on the surface of the chamber 101 facing the surface of the substrate 1, 2, 3 to maximize the area of radiant heat applied to the substrates 1, 2, 3. For example, when the substrates 1, 2, 3 are disposed in the internal space I in a state of gravity as shown in FIGS. 2 and 3, the main heating part 130 is formed on the A5 surface of the chamber 101 and And / or on the A6 side.
  • the main heating unit 130 may include a first main heating unit 131 and a second main heating unit 132.
  • the first main heating unit 131 may be disposed on the A6 surface of the chamber 101
  • the second main heating unit 132 may be disposed on the A5 surface of the chamber.
  • the present invention is not limited thereto, and only one main heating unit may be disposed, or three or more main heating units may be disposed on the surfaces of three or more chambers 101 different from each other.
  • the main heating unit 130 may include a halogen lamp, the halogen lamp may be arranged in a plurality of spaced apart a predetermined interval. Halogen lamps) emit light of near-infrared, mid-infrared and / or visible light.
  • the main heating unit 130 may further include a window (not shown), and the window may be disposed to surround the outer circumference of the halogen lamp, or may be disposed on one side of the halogen lamps arranged in parallel in one direction.
  • the window may comprise a transparent material, for example quartz. The window protects the halogen lamp and can enhance the light efficiency.
  • the substrates 1, 2, and 3 may reflect most of the radiant heat supplied from the main heating unit 130. In this case, the substrates 1, 2, and 3 may not be heated easily, which may take a long time to reach the temperature conditions required for graphene synthesis.
  • the substrates 1, 2, 3 when the plurality of substrates 1, 2, 3 are arranged in the internal space I, the substrate disposed inside, for example, the second substrate 2, and the substrate disposed outside, for example, the first substrate 1. ) And the third substrate 3, because it receives a small amount of radiant heat, there is a problem that the heating is not sufficiently. Therefore, in order to uniformly heat the plurality of substrates 1, 2, 3 in a faster time, the graphene synthesis apparatus 100 includes a first auxiliary heating unit 110 and a second auxiliary heating unit 120. do.
  • the first auxiliary heating unit 110 converts the radiant heat of the main heating unit 130 into convective heat and releases it into the internal space I to heat the substrate and the gas.
  • the temperature of the first auxiliary heating unit 110 may be increased by radiant heat emitted from the main heating unit 130.
  • the first auxiliary heating unit 110 may be any type of material that can be raised in temperature by radiant heat.
  • the first auxiliary heating unit 110 may include a material coated with graphite or an oxide film. This is because the material may be, for example, a metal, and by coating an oxide film on the metal, the reflectance may be lowered and the absorption rate of radiant heat may be increased.
  • the material is not limited to metals.
  • the first auxiliary heating unit 110 is disposed to face one of the one or the other surfaces of the substrates 1, 2, and 3 in correspondence with the main heating unit 130. That is, the first auxiliary heating unit 110 is disposed to be parallel to the surface of the chamber 101 in which the main heating unit 130 is disposed, for example, the A5 surface and / or the A6 surface, and the substrates 1, 2, and 3 It may be arranged to be parallel to any one side or the other side of the.
  • the first auxiliary heating unit 110 may include a first-first auxiliary heating unit 111 and a second-second auxiliary heating unit 112 disposed at both sides with the substrates 1, 2, and 3 interposed therebetween. have. However, this is exemplary and the first auxiliary heating unit 110 may include only one of the first-first auxiliary heating unit 111 or the 1-2 second auxiliary heating unit 112.
  • the first-first auxiliary heating unit 111 and the second-second auxiliary heating unit 112 are disposed to face each other while being spaced apart from each other.
  • the first-first auxiliary heating part 111 is disposed to face one surface of the first substrate 1
  • the second-second auxiliary heating part 112 is disposed to face the other surface of the third substrate 3. Can be.
  • the first auxiliary heating unit 110 emits convective heat to heat both the substrate and the gas to convert the internal space I to a high temperature optimized for graphene synthesis in a short time.
  • the first-first auxiliary heating unit 111 and the second-second auxiliary heating unit 112 are provided to serve to confine heat generated in the internal space I to maintain a high temperature.
  • the substrate when one or two substrates are used, the substrate may be heated to a temperature required for graphene synthesis in a short time with only the main heating unit 130 and the first auxiliary heating unit 110.
  • the substrate disposed inside, for example, the second substrate 2 may be arranged on the outside, for example, the first substrate 1 and the third substrate 3. ) May interfere with heat flow or block heat, resulting in insufficient heating.
  • the second auxiliary heating unit 120 is disposed between the plurality of substrates 1, 2, and 3 to evenly heat the substrate disposed inside, for example, the second substrate 2.
  • the second auxiliary heating unit 120 may be raised in temperature by radiant heat emitted from the main heating unit 130 and convective heat emitted from the first auxiliary heating unit 110, and may be coated with graphite or oxide film. It may be made of a material.
  • the second auxiliary heating unit 120 is arranged to apply heat to the largest area of the substrate and to face at least one of one or the other surfaces of the substrates 1, 2 and 3 in consideration of spatial efficiency.
  • the area of one surface of the second auxiliary heating unit 120 is preferably about 60% or more of the area of the main heating unit 130.
  • the second auxiliary heating part 120 is not heated evenly.
  • the temperature of the edge of one surface of the second auxiliary heating part 120 is lower than that of the center part, so that the overall temperature of the second auxiliary heating part 120 is uneven.
  • the heat flow and the gas flow of the internal space are not smooth, so that the probability of defects in graphene synthesis increases, and the process time required for graphene synthesis may increase.
  • the number of second auxiliary heating units 120 is determined according to the number of substrates.
  • the number of second auxiliary heating units 120 may be (number of substrates-1).
  • the second auxiliary heating part 120 is the second-first auxiliary heating part 121 disposed between the first substrate 1 and the second substrate 2.
  • the second auxiliary heating unit 122 may be disposed between the second substrate 2 and the third substrate 3.
  • the 2-1 sub-heater 121 and the 2-2 sub-heater 122 are disposed between the substrates 1, 2, and 3 to emit heat, and thus, are disposed inside the substrate.
  • the second substrate 2 can also be sufficiently heated.
  • the internal space can be converted to a high temperature optimized for graphene synthesis in a short time.
  • the gas supply unit 140 includes a plurality of nozzles and supplies a gas containing carbon to the internal space I.
  • Gases containing carbon are reaction gases for graphene formation, such as 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 Carbon atoms such as H 10 ), cyclopentadiene (C 5 H 6 ), hexane (C 6 H 14 ), cyclohexane (C 6 H 12 ), benzene (C 6 H 6 ), toluene (C 7 H 8 )
  • One or more selected from the group may be used.
  • the gas containing carbon is separated into carbon atoms
  • the gas supply unit 140 may supply not only the gas containing carbon but also the atmospheric gas to the internal space (I).
  • the atmosphere gas may include an inert gas such as helium or argon, and an unreacted gas such as hydrogen to keep the surface of the substrate clean.
  • one gas supply unit 140 supplies both a gas containing carbon and an atmosphere gas
  • the present invention is not limited thereto.
  • a gas supply unit supplying a gas containing carbon and a gas supply unit supplying an atmosphere gas may be provided, respectively, and the gas containing carbon and the atmosphere gas may be supplied to the internal space I, respectively.
  • the gas supply unit 140 is disposed on the A3 surface, but is not limited thereto.
  • the gas supply unit 140 may be disposed on the other surface.
  • the plurality of gas supply units 140 may be disposed on a plurality of different surfaces.
  • the discharge part 150 is used for graphene synthesis in the internal space (I) and then exhausts the remaining residual gases to the outside.
  • Discharge unit 150 may be disposed on the surface facing the gas supply unit 140, for example, A4 surface in order to maximize the discharge effect.
  • this is merely an example, and the arrangement structure and the number of the discharge parts 150 may be variously implemented without being limited to those illustrated.
  • the graphene synthesis apparatus 100 may further include a decompression unit (not shown) that decompresses the internal space I of the chamber 101.
  • a decompression unit (not shown) that decompresses the internal space I of the chamber 101.
  • the gas in the internal space I is drawn out to the outside through the decompression unit so that the internal space I of the chamber 101 may be decompressed to about several torr to 10 ⁇ 3 torr.
  • the graphene synthesizing apparatus 100 may further include a gate (not shown) for inserting and unloading a substrate.
  • a gate for inserting and unloading a substrate.
  • There may be a plurality of gates, and the specific shape, arrangement structure, and number of gates may vary depending on whether the substrate is a panel type or a roll type.
  • FIG. 6 shows only the V portion in detail in the front view of the graphene synthesizing apparatus 100 shown in FIG. 5.
  • 7 to 9 are related to the graphene synthesizing apparatus 100 according to another embodiment of the present invention, and shows only the portion V in the front view of the graphene synthesizing apparatus 100 illustrated in FIG. 5.
  • the interval between the substrates 1, 2, 3 and the second auxiliary heating unit 120 becomes narrower.
  • the substrates 1, 2, 3 and the second auxiliary heating unit 120 interfere with the heat flow and the flow of the gas, so that the substrate may not be heated evenly or the gas may not reach the substrate uniformly. Occurs. Therefore, graphene is not partially synthesized on the surface of the substrate, or the quality of graphene is degraded.
  • the aforementioned problem may be solved by forming the hole H in the second auxiliary heating unit 120a.
  • the second auxiliary heating part 120a includes a plurality of the second auxiliary heating part 121a and the second auxiliary heating part 122a, a plurality of second auxiliary heating parts 120a are formed, thereby forming heat. Flow and gas flow can be smoothed.
  • the shape of the hole H may be circular or polygonal, but is not limited thereto.
  • the size of the hole H, the number of holes H, and the like are not limited to those illustrated in FIG. 7, and may be variously implemented.
  • the four quadrants provided with respect to the vertical axis Q1 and the horizontal axis Q2 passing through the center point of the second auxiliary heating part 120b are symmetrical. It is preferable to arrange the hole H. Only then can the heat flow and gas flow in the interior space be smooth to synthesize high quality graphene. As described above, the shape, size, number, and the like of the holes H are not limited to those illustrated in FIG. 8, and may be variously implemented.
  • the number and area of through holes may be maximally formed in the second auxiliary heating part 120c in order to facilitate the heat flow and the gas flow in the internal space.
  • the second auxiliary heating unit 120c may be manufactured in a mesh form.
  • At least one of each of the 2-1 sub-heaters 121c and the 2-2 sub-heaters 122c included in the second sub-heater 120c of FIG. 9 may be manufactured in a mesh form.
  • another graphene synthesizing apparatus of the present invention may further include an additional main heating unit and an additional auxiliary heating unit.
  • This additional auxiliary heating portion is arranged to intersect, for example vertically, with each side of the plurality of substrates, and the additional main heating portion is disposed corresponding to the additional auxiliary heating portion.
  • the additional main heating unit may be disposed on at least one of the A1 side, the A2 side, the A3 side, and the A4 side of FIG. 4, and the additional auxiliary heating unit may be disposed to be parallel to each side of the chamber in which the additional main heating unit is formed. have.
  • the additional main heating unit and the additional auxiliary heating unit thus arranged may supply radiant heat and convective heat in a direction perpendicular to the plane vectors of the plurality of substrates. Therefore, radiant heat and convective heat can be effectively applied between the substrates, thereby increasing the temperature of the substrate and the internal space more quickly.
  • the plurality of substrates 1, 2, and 3 are seated in the internal space I, and then a gas contained in the internal space I is transferred through a decompression unit (not shown) using a vacuum pump (not shown). Pull it out.
  • the internal space I may have a pressure lower than atmospheric pressure, for example several hundred torr to 10 ⁇ 6 torr.
  • the second auxiliary heating unit 120 is disposed between the plurality of substrates (1, 2, 3).
  • the second auxiliary heating unit 120 is disposed to face one of the one surface or the other surface of the substrate.
  • the direction in which the plurality of substrates 1, 2, 3 and the second auxiliary heating unit 120 are arranged may be a direction that crosses, for example, a direction of gravity (-Y direction). Can be.
  • the sheet resistance of the synthesized graphene may be more excellent.
  • the grain of the substrate increases due to the high temperature atmosphere. For example, when copper is used as the substrate, the grain of copper increases, and it is determined that the environment in which graphene is uniformly synthesized due to the increase in grain of copper is created.
  • the outermost substrates are disposed to face the first auxiliary heating unit 110.
  • an atmosphere gas for example, an inert gas such as helium or argon and / or a non-reactive gas such as hydrogen for maintaining the surface of the metal thin plate may be injected through the gas supply unit 140.
  • the gas supply unit 140 is disposed in the direction in which the substrate is erected so that the gas can be effectively supplied between the plurality of substrates (1, 2, 3).
  • the substrates 1, 2, 3 and the first and second auxiliary heaters 110, 120 are heated using the main heater 130.
  • the temperatures of the first and second auxiliary heating parts 110 and 120 and the substrates 1, 2 and 3 are sufficiently high by the radiant heat emitted from the main heating part 130, the substrates 1, 2 and 3 and the first 2, a temperature sufficient for synthesizing graphene is formed in the internal space I by the heat emitted from the auxiliary heating units 110 and 120.
  • the temperature of the interior space I and the substrates 1, 2, 3 may be about 300 degrees Celsius or about 1000 degrees Celsius or more.
  • a gas containing carbon that is, a reaction gas
  • a gas containing carbon that is, a reaction gas
  • the discharge part 150 provided on the side opposite to the gas supply part 140 is also disposed in the direction in which the substrate is placed, that is, the plurality of substrates are arranged in the direction crossing the direction in which the substrates are arranged, while supplying the reaction gas to the supply unit 140, the other side may exhaust the gas using the discharge unit 150 so that the reaction gas may effectively flow through the space between the substrates.
  • a nozzle of the gas supply unit 140 may be present between the plurality of substrates to facilitate gas flow .
  • the reaction gas is energized in the auxiliary space (I) and decomposed into a state required for graphene synthesis.
  • the substrates 1, 2, and 3 which are in contact with the surface of the activated substrate, are absorbed by the surface-activated substrate. Pin crystals grow.
  • the substrates 1, 2, and 3 are heated by the main heating unit 130, and then the gas containing carbon is supplied.
  • the main heating unit 130 may supply a gas containing carbon before emitting radiant heat, or at the same time as emitting radiant heat, or after radiating radiant heat. That is, when the main heating unit 130 is operated before supplying the gas containing carbon or when the main heating unit 130 is operated while supplying the gas containing carbon, or after the gas is supplied, the main heating unit is operated. 130 may be operated.
  • the substrates 1, 2, 3 and the first and second auxiliary heating units 110 and 120 are heated, and the heated substrate 1, 2,3) and the case in which the internal space I is warmed and the gas containing carbon is decomposed by the heat emitted from the first and second auxiliary heating parts 110 and 120, but the present invention is not limited thereto.
  • the main heating unit 130 may emit light including the near infrared wavelength band and / or the visible wavelength band as well as the near infrared wavelength band.
  • the light of the near infrared wavelength band emitted from the main heating unit 130 supplies energy to the substrates 1, 2 and 3 and the first and second auxiliary heating units 10 and 120, as described above.
  • the internal space I may be heated by the substrates 1, 2, 3 and the first and second auxiliary heating parts 110 and 120.
  • the gas containing the carbon supplied to the internal space I may be heated by the light of the mid-infrared and / or visible light wavelength band emitted from the main heating unit 130.
  • the gas containing carbon is heat and mid-infrared or / and visible light wavelength band of the internal space I warmed by the substrates 1, 2, 3 and the first and second auxiliary heating parts 110, 120. It can be decomposed by receiving energy from light. Therefore, the graphene synthesis reaction in the internal space (I) can be performed more actively in a short time.
  • Embodiments of the present invention can be applied to an active layer and a display device, an electronic device, an optoelectronic device, a battery, and a solar cell including the same.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Toxicology (AREA)
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  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
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Abstract

Cette invention concerne un appareil de synthèse de graphène, comprenant : une chambre comportant des espaces intérieurs dans laquelle une pluralité de substrats dont les surfaces sont orientées de façon à être en regard les uns des autres est chargée ; une unité d'injection de gaz pour injecter, dans lesdits espaces intérieurs, un gaz contenant du carbone ; une unité de chauffage principale pour exposer lesdits espaces intérieurs à une chaleur rayonnante ; une première unité de chauffage auxiliaire placée de façon à être en regard d'une surface des substrats correspondant à l'unité de chauffage principale, pour convertir la chaleur rayonnante en chaleur de convection, et diffuser la chaleur de convection convertie dans les espaces intérieurs ; et une pluralité de secondes unités de chauffage auxiliaires placées pour être en regard d'au moins une surface du substrat parmi la pluralité de substrats, chauffée par absorption de la chaleur rayonnante et de la chaleur de convection, et qui diffuse la chaleur dans les espaces intérieurs.
PCT/KR2013/007568 2013-01-28 2013-08-26 Appareil de synthèse de graphène et procédé associé l'utilisant Ceased WO2014115942A1 (fr)

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KR101812208B1 (ko) 2016-03-15 2017-12-27 해성디에스 주식회사 그래핀 합성 장치 및 이를 이용한 그래핀 합성 방법
KR101956175B1 (ko) * 2016-11-29 2019-03-08 (주) 세츠 대면적 그래핀 성장 장치
KR102037990B1 (ko) * 2019-04-18 2019-10-29 세종대학교산학협력단 그래핀 제조장치 및 그래핀 제조방법
CN111892042A (zh) * 2020-08-07 2020-11-06 河南墨特石墨烯科技有限公司 一种生产石墨烯的装置及利用该装置生产石墨烯的方法

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KR20140096648A (ko) 2014-08-06
KR101842027B1 (ko) 2018-03-26
CN105246588B (zh) 2020-04-24

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