Classifications

• • 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
  • B01J19/18—Stationary reactors having moving elements inside
  • B01J19/22—Stationary reactors having moving elements inside in the form of endless belts
• • 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

Definitions

• the present invention relates to graphene, and more particularly, to a method for producing graphene using a tension allol, and a graphene and a manufacturing apparatus thereof.
• Carbon atoms include fullerene, carbon nanotube, graphene and graphite.
• graphene is a structure in which carbon atoms are composed of a single layer of atoms in a two-dimensional plane.
• graphene is not only very stable and excellent in electrical, mechanical, and chemical properties, but also as a good conductive material, it can move electrons much faster than silicon and carry a much larger current than copper.
• a method of separating graphene has been discovered, it has been proved through experiments.
• graphene generally has electrical characteristics that can be changed according to the crystal orientation of graphene having a given thickness, so that the user can express electrical characteristics in a selected direction, and thus the device can be easily designed. . Therefore, graphene can be effectively used for carbon-based electrical or electromagnetic devices.
• the problem to be solved by the present invention is to provide a graphene manufacturing method and a graphene and its manufacturing apparatus capable of producing high quality uniform graphene.
• the present invention provides a method for producing graphene.
• the graphene manufacturing method includes loading a catalyst metal charge into a chamber, applying tension to the catalyst metal charge, and applying the catalyst metal charge to the catalyst metal charge. And supplying a carbon source into the chamber under tension to form graphene on the catalyst metal charge.
• the chamber comprising a gas inlet and outlet, the catalyst metal layer is loaded; And a tensioning device for tensioning the catalytic metal layer loaded into the chamber.
• the grain size of the catalyst metal layer can be increased by applying tension to the catalyst metal charge, and high quality uniform graphene can be grown using the catalyst metal layer.
• the orientation of the catalyst metal layer can be changed to the (111) orientation, and the catalyst metal filling can be used to grow high quality uniform graphene.
• FIG. 1 is a flowchart schematically illustrating a method of manufacturing graphene according to an exemplary embodiment of the present invention.
• FIG. 3 shows images obtained by measuring the orientation of a catalyst metal layer after synthesizing graphene according to Comparative Examples and Preparation Examples.
• FIG. 4 is a schematic view showing an example of a graphene manufacturing apparatus.
• FIG. 5 is a schematic view showing another example of a graphene manufacturing apparatus.
• first and second may be used to describe various elements, components, regions, layers and / or regions, such elements, components, regions, layers and It will be understood that regions should not be limited by these terms.
• FIG. 1 is a flowchart schematically illustrating a method of manufacturing graphene according to an embodiment of the present invention.
• the method for preparing graphene includes loading a catalyst metal charge into a chamber (S1), applying a tension to the catalyst metal layer (S2), and graphene on the catalyst metal layer. Forming step (S3).
• the loading of the catalytic metal layer into the chamber (S1) may use, for example, chambers of various deposition apparatus.
• it may be a horizontal CVD chamber or a vertical CVD chamber which is a chamber of a chemical vapor deposition (CVD) apparatus.
• a catalyst metal layer can be loaded into a horizontal CVD chamber.
• the catalytic metal layer is a metal capable of forming graphene, including nickel (Ni), cobalt (Co), iron (Fe), platinum (Pt), gold (Au), aluminum (A1), and creme (0) , Copper (Cu), Magnesium (Mg), Manganese (Mn), Molybdenum (Mo), Rhodium (Rh), Silicon (Si), Tantalum (Ta), Titanium (Ti), Tungsten Uranium (U), Banarum ( V), any one selected from the group consisting of zirconium (Zr) may be used, and any one of these cases may be used as a single layer or at least two alloys of these cases.
• the catalyst metal layer may be a single metal layer composed only of the catalyst metal, or may be combined with other members.
• the catalytic metal may be in a state disposed on one side of the silicon substrate having silicon oxide (Si0 2 ).
• the catalyst metal layer may be in the form of a wafer or a foil.
• the catalytic metal layer may be a copper foil.
• the thickness of the catalyst metal charge may be 10 to 50. If the thickness of the catalyst metal layer is less than 10, the magnitude of the tension applied to the catalyst metal layer cannot be sufficiently increased.
• the thickness of the catalyst metal layer exceeds 50, the area of contact with the carbon source is constant, and the economical efficiency may be reduced because the thickness of the catalyst metal layer is increased.
• the catalyst metal layer may be tensioned by using a component capable of applying tension to the catalyst metal layer.
• tension may be applied to the catalyst metal layer vertically or horizontally.
• a catalyst metal layer is loaded in a vertical CVD chamber, and the loaded catalyst metal layer can be hanged in a batch type, and by connecting a component capable of applying tension to the lower portion of the catalyst metal layer.
• tension can be applied to the catalyst metal layer up and down.
• the size of the tension may be 0.1 kg / m to 5 kg / m. If the magnitude of the tension is less than 0.1 kg / m, the grain size of the catalyst metal layer cannot be increased as desired, and if the magnitude of the tension exceeds 5 kg / m, the catalyst metal layer cannot tolerate the force and is torn. Damage may occur.
• This tension can increase the grain size of the catalyst metal layer.
• the average grain size of this tensioned catalytic metal layer may be between 100 urn and 500.
• the tension may change the orientation of the catalyst metal layer. For example, when tension is applied to a copper foil having a (001) orientation, it may be changed to a (111) orientation.
• the step of applying all the tension to the catalyst metal filling (S2) may further comprise the step of heat-treating the catalyst metal layer.
• This heat treatment temperature may be 3 (xrc or more).
• the addition of heat treatment under tension to the catalyst metal charge helps to change the orientation of the catalyst metal layer and allows the catalyst metal layer to have a more single orientation structure. As the orientation of the catalyst metal layer has more unit orientation, high quality uniform graphene may be synthesized.
• the graphene may be formed on the catalyst metal charge by supplying a carbon source into the chamber while applying tension to the catalyst metal layer.
• graphene may be formed on the catalyst metal layer using various deposition methods.
• graphene may be synthesized by chemical vapor deposition using a catalytic metal.
• chemical vapor deposition for example, high temperature chemical vapor deposition (T-CVD), inductively coupled plasma chemical vapor deposition (ICP-CVD), and plasma chemical vapor deposition Chemical vapor deposition (Plasma Enhanced Chemical Vapor Deposition, PE-CVD), microwave CVD (Microwave CVD) can be used.
• various methods such as rapid thermal annealing (RTA), atomic layer deposition (ALD), and physical vapor deposition (PVD) may be used.
• Examples of carbon sources can be supplied in the form of gases such as methane (CH 4 ), acetylene (C 2 3 ⁇ 4), solid forms such as powders and polymers, and liquid forms such as bubbling alcohols. Supply is possible.
• gases such as methane (CH 4 ), acetylene (C 2 3 ⁇ 4), solid forms such as powders and polymers, and liquid forms such as bubbling alcohols. Supply is possible.
• various carbon sources such as ethane, ethylene, ethanol, acetylene, propane, butane, butadiene, pentane pentene, cyclopentadiene, nucleic acid, cyclonucleic acid, benzene and toluene may be used.
• Methane gas is introduced in a hydrogen atmosphere while maintaining a suitable temperature on the copper catalyst metal layer.
• methane gas is separated into carbon atoms and hydrogen atoms, and the separated carbon atoms are absorbed or deposited on the surface of the catalytic metal.
• the separated carbon atoms diffuse into the grains of the catalytic metal.
• the temperature in the chamber may be made at a silver condition of approximately 300 V to 1500 ° C.
• graphene is formed by remarking the catalytic metal charge in which carbon atoms are absorbed or deposited on the surface. Carbon atoms absorbed on the surface of the catalyst metal layer are synthesized on the surface of the catalyst metal charge as the catalyst metal layer cools.
• the angle of the catalyst metal layer can be carried out within a relatively short time.
• the cooling of the catalyst metal layer may be performed inside the chamber, or may be performed outside the chamber after removing the catalyst metal layer from the chamber.
• copper has a low solubility in carbon, and thus may be advantageous for forming a mono-layer grapheneol.
• the method may further include removing the catalyst metal charge (not shown).
• the catalytic metal layer can be removed by a method such as etching. If desired, for example, the nickel catalyst metal layer can be removed using a FeCl 3 etching solution.
• the catalyst metal layer may be removed after laminating the carrier member on the graphene.
• the catalyst metal layer may be removed using polydimethylsiloxane (PDMS).
• the orientation of the catalyst metal charge is changed to the (111) orientation by applying tension to the catalyst metal layer, and high quality uniform graphene can be grown using the catalytic metal layer which has been changed to the (111) orientation.
• Graphene was synthesized using a vertical CVD apparatus. A copper catalyst metal layer was loaded into the vertical CVD chamber and a carbon source was fed into the chamber to form graphene with a tension of about 1 kg / m applied up and down the catalyst metal charge.
• FIG. 2 is a graph illustrating grain size of a catalyst metal layer after synthesis of graphene according to Comparative Examples and Preparation Examples.
• FIG. 2 (a) is a graph illustrating grain mapping of a catalyst metal charge after synthesizing graphene according to a comparative example.
• FIG. 2 (b) is a graph showing grain mapping of the catalyst metal layer after synthesis of graphene according to the preparation example, and graphene was synthesized in a state in which tension was applied to the catalyst metal charge.
• 3 (a) and 3 (b) are images obtained by orientation mapping of a catalyst metal layer after synthesizing graphene according to a comparative example.
• 3 (a) and 3 (b) are the same image, and FIG. 3 (b) is colored according to the direction.
• 3 (c) and 3 (d) are images obtained by orientation mapping of a catalyst metal charge after synthesizing graphene according to a preparation example. 3 (c) and 3 (d) are the same image, and FIG. 3 (d) is displayed in color according to the direction.
• 4 and 5 are examples of a manufacturing apparatus for synthesizing graphene according to the preparation example of the present invention.
• FIG. 4 shows an apparatus in which the catalyst metal layer 20 is vertically loaded into the chamber 10
• FIG. 5 shows that the catalyst metal layer 10 is loaded in a roll-t method.
• 10 shows a device to be supplied.
• the graphene manufacturing apparatus includes a chamber 10 in which the catalyst metal filling 20 is vertically disposed and loaded, and the chamber 10 is equipped with a gas inlet 11 and a gas outlet 12.
• a support 13 is disposed to provide the catalyst metal layer 20. Support so that the catalytic metal layer 20 can be loaded vertically.
• tension portion 30 may be connected to the opposite side of the catalyst metal packed 20 supported by the support 13.
• tension unit 30 may be a weight weight having a predetermined weight.
• Another example may be an elastic member having elasticity.
• One example of such an elastic member may be a spring member. At this time, one end of the spring member may be connected to the catalyst metal layer 20 and the other end may be fixed to the chamber 10.
• the tension applied to the catalyst metal layer 20 may be adjusted to a fixed value by using the tension unit 30 exemplified as the weight member or the spring member fixed as described above. '
• the tension applied to the catalytic metal charge 20 is also possible to configure the tension applied to the catalytic metal charge 20 to be variable. That is, the tension can be adjusted.
• the other end of the tension portion 30, such as the weight or spring member is connected to the tension control portion 40 that is installed to be movable, by the operation of such a tension control portion 40 It may be possible to control the tension applied to the catalytic metal layer 20.
• the catalyst metal layer 20 is released from the supply roll 50 and supplied to the chamber 10 in the A direction, and wound around the winding rule 60.
• the chamber 10 is provided with a gas inlet 11 and a gas outlet 12.
• tension part 31 can be configured using a lor.
• tension control unit 41 which can adjust the tension allol so that the tension allotted to the catalyst metal layer 20 can be varied.
• the tension section 31 is connected to a tension control section 41 in which the tension section 31 is movable so that the catalyst metal layer 20 can be operated by the operation of the tension control section 41. You can adjust the tension on).
• the tension applied to the catalyst metal layer 20 by the tension section 31 can be measured.
• the tension measuring unit 42 may be further provided. Therefore, the tension adjusting unit 41 can more precisely adjust the tension to be applied to the catalyst metal layer 20 according to the measured value of the tension measuring unit 42, and this process can be made automatically.
• the tension portion 31 may be provided with an elastic structure such as a spring therein to be elastically and in contact with the catalytic metal layer 20.
• the tension unit 31 and the tension control unit 41 may be connected by using a separate elastic member.
• the tension portion 31 shows an example in which the tension portion 31 is located at the inlet side of the chamber 10 into which the catalyst metal layer 20 is introduced. In some cases, the catalyst metal layer 20 It is also possible to provide in the position of the exit side discharged from this chamber 10.
• both the inlet and the outlet side of the chamber 10 may be provided, and in some cases, it may be provided inside the chamber 10.
• high-quality uniform graphene can be grown by applying tension to the catalyst metal layer.
• Such high quality graphene has excellent electrical and physical properties and may be used in various electronic devices such as display devices.

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Citations (5)

• 2013
  • 2013-08-01 WO PCT/KR2013/006955 patent/WO2014035068A1/fr not_active Ceased

Patent Citations (5)

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