CN112028059A - Preparation device and application of graphene - Google Patents

Preparation device and application of graphene Download PDF

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Publication number
CN112028059A
CN112028059A CN202010941296.2A CN202010941296A CN112028059A CN 112028059 A CN112028059 A CN 112028059A CN 202010941296 A CN202010941296 A CN 202010941296A CN 112028059 A CN112028059 A CN 112028059A
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reaction
graphene
shell
cooling
pipe
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CN202010941296.2A
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陶汀汀
曹敏杰
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Ningbo Mcc Electronic Technology Co ltd
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Ningbo Mcc Electronic Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • C01B32/186Preparation by chemical vapour deposition [CVD]
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/04Specific amount of layers or specific thickness

Abstract

The embodiment of the invention discloses a preparation device of graphene and application thereof. The graphene preparation device comprises: a reaction housing having a sealed containment chamber; the heating assembly is arranged in the accommodating cavity and forms a reaction area in the accommodating cavity; the reaction gas input pipe is communicated with the reaction shell and extends into the reaction area; the protective gas input pipe is communicated with the reaction shell and extends into the accommodating cavity; the graphene output pipe is communicated with the reaction shell, and a pipe orifice of the graphene output pipe is opposite to the reaction area; and the gas discharge pipe is communicated with the reaction shell and extends into the accommodating cavity. The embodiment of the invention solves the problem that the existing graphene preparation device is complex in structure.

Description

Preparation device and application of graphene
Technical Field
The invention relates to the technical field of graphene preparation, in particular to a graphene preparation device and application of the graphene preparation device.
Background
Graphene is a sheet-like body in which carbon atoms are arranged in a hexagonal ring shape, and is generally composed of a single-layer or multi-layer graphite sheet layer, and can extend infinitely in a two-dimensional space, and can be said to be a two-dimensional structural material in a strict sense. It has the outstanding advantages of large specific surface area, excellent electric and heat conductivity, low thermal expansion coefficient and the like. In particular, its advantages include at least: high specific surface area (theoretical calculation: 2630 m)2(iv)/g); high conductivity and carrier transmission rate (200000 cm)2V · s); high thermal conductivity (50)00W/mK); high strength, high Young's modulus (1100GPa) and breaking strength (125 GPa). Therefore, the material has great application prospect in the fields of energy storage, heat conduction and high-strength materials.
The existing methods for preparing graphene mainly include a micro-mechanical exfoliation method, an ultra-high vacuum graphene epitaxial growth method, an oxidation-reduction method, a Chemical Vapor Deposition (CVD) method, a solvent exfoliation method, and a solvothermal method. Among the methods, the oxidation-reduction method is the most widely used method among the methods for preparing graphene in the largest batch at present.
However, the conventional graphene preparation device has a complicated structure.
Disclosure of Invention
Therefore, the embodiment of the invention provides a graphene preparation device and application of the graphene preparation device, and solves the problem that the existing preparation device is complex in structure.
In one aspect, an apparatus for preparing graphene provided in an embodiment of the present invention includes: a reaction housing having a sealed containment chamber; the heating assembly is arranged in the accommodating cavity and forms a reaction area in the accommodating cavity; the reaction gas input pipe is communicated with the reaction shell and extends into the reaction area; the protective gas input pipe is communicated with the reaction shell and extends into the accommodating cavity; the graphene output pipe is communicated with the reaction shell, and a pipe orifice of the graphene output pipe is opposite to the reaction area; and the gas discharge pipe is communicated with the reaction shell and extends into the accommodating cavity.
In one embodiment of the invention, the heating assembly comprises a plasma electrode module and an electric field electrode module; the plasma electrode module generates a plasma arc under the action of an electromagnetic field generated by the electric field electrode module; wherein the plasma electrode module and the electric field electrode module form the reaction region.
In one embodiment of the present invention, the electric field electrode module includes: a first electric field electrode and a second electric field electrode; the two are oppositely arranged and provided with a gap; the plasma electrode module includes: and the pairs of plasma electrodes are respectively oppositely arranged between the first electric field electrode and the second electric field electrode, and intervals are respectively arranged between each pair of plasma electrodes.
In an embodiment of the present invention, the gas outlet pipe is disposed at a top end of the reaction housing, and the graphene outlet pipe is disposed at an opposite bottom end of the reaction housing.
In an embodiment of the present invention, the apparatus for preparing graphene further includes: and the cooling assembly is arranged outside the reaction shell.
In one embodiment of the invention, the cooling assembly comprises: the cooling shell is sleeved outside the reaction shell and forms a sealed cooling area with the reaction shell; the cooling liquid input pipe is communicated with the cooling shell and extends into the cooling area; and the cooling liquid return pipe is communicated with the cooling shell and extends into the cooling area.
In an embodiment of the present invention, the apparatus for preparing graphene further includes: the first temperature sensor is arranged in the accommodating cavity and used for detecting the temperature of the reaction area; the second temperature sensor is arranged in the accommodating cavity and used for detecting the temperature of the area between the reaction shell and the heating assembly; and the display component is connected with the first temperature sensor and is positioned outside the reaction shell.
In a further aspect, the present invention also provides a use of the apparatus for preparing graphene according to any one of the above embodiments, for preparing a 2-5-layer graphene material; wherein the reaction zone is heated to 3500-3800K by the heating assembly; inert gas is input into the accommodating cavity through the protective gas input pipe, so that the pressure of the accommodating cavity is 1.2-1.5 MPa; inputting methane and/or acetylene gas into the reaction area through the reaction gas input pipe; outputting the graphene material to the outside of the reaction shell through the graphene output pipe; discharging hydrogen gas through the gas discharge pipe.
In one embodiment of the invention, when the heating assembly comprises the plasma electrode module and the electric field electrode module; the current passed by the plasma module is between 70 and 130A.
In one embodiment of the present invention, when the preparation apparatus further comprises the cooling unit, the cooling temperature of the cooling unit is 50 to 70 ℃.
In summary, the above embodiments of the present application may have one or more of the following advantages or benefits: i) the preparation device can prepare graphene; ii) the preparation device has simple structure.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a graphene preparation apparatus 200 according to an embodiment of the present invention.
Fig. 2 is a schematic front sectional view of the graphene preparation apparatus 200 shown in fig. 1.
Fig. 3 is a schematic top sectional view of the apparatus 200 for preparing graphene shown in fig. 1.
Fig. 4 is a schematic structural diagram of the heating assembly 210 in fig. 2.
Fig. 5 is a schematic structural diagram of the first temperature sensor 220, the second temperature sensor 221 and the display module 222 in fig. 2.
Description of the main element symbols:
200 is a graphene preparation device; 201 is a reaction shell; 202 is a reaction gas input pipe; 203 is a protective gas input pipe; 204 is a graphene output pipe; 205 is a gas discharge pipe; 206 is a cooling liquid input pipe; 207 is a cooling liquid return pipe; 208 is a cooling housing; 209 is a cooling zone; 210 is a heating element; 211 is a first plasma electrode; 212 is a second plasma electrode; 213 is a first electric field electrode; 214 is a second electric field electrode; 215 is a reaction zone; 216 is a waterproof jacket; 220 is a first temperature sensor; 221 is a second temperature sensor; 222 is a display element.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1 and fig. 2, which are schematic structural diagrams of a graphene preparation apparatus 200 according to an embodiment of the present invention, the graphene preparation apparatus 200 includes: the reactor comprises a reaction shell 201, a heating assembly 210, a reaction gas input pipe 202, a protective gas input pipe 203, a graphene output pipe 204 and a gas discharge pipe 205. The reaction housing 201 has a sealed accommodating chamber (not labeled), the heating element 210 is disposed in the accommodating chamber, and a reaction region 215 is formed in the accommodating chamber; the reaction gas input pipe 202 is communicated with the reaction shell 201 and extends into the reaction area 215; the protective gas input pipe 203 is communicated with the reaction shell 201 and extends into the accommodating cavity; the graphene output pipe 204 is communicated with the reaction shell 201, and a pipe orifice of the graphene output pipe is opposite to the reaction area 215 and is arranged at the opposite bottom end of the reaction shell 201; the gas outlet pipe 205 is communicated with the reaction shell 201, extends into the accommodating cavity, and is arranged at the top end of the reaction shell 201.
Specifically, the reaction gas input pipe 202, the protective gas input pipe 203, the graphene output pipe 204, and the gas discharge pipe 205 are all sleeved with gas valves for controlling gas flow.
Specifically, referring to fig. 3 and 4, the heating assembly 210 includes a plasma electrode module (not shown) and an electric field electrode module (not shown), wherein the plasma electrode module generates a plasma arc under the action of an electromagnetic field generated by the electric field electrode module; the plasma electrode module and the electric field electrode module form a reaction region 215. Specifically, the electric field electrode module includes: a first electric field electrode 213 and a second electric field electrode 214, the first electric field electrode 213 and the second electric field electrode 214 being disposed opposite to each other with a space therebetween; the plasma electrode module includes: a plurality of pairs of plasma electrodes (not shown), wherein one pair of plasma electrodes comprises: a first plasma electrode 211 and a second plasma electrode 212; the pairs of plasma electrodes are oppositely disposed between the first electric field electrode 213 and the second electric field electrode 214, and a space is disposed between each pair of plasma electrodes.
Preferably, referring to fig. 2, the apparatus 200 for preparing graphene further includes: and the cooling assembly (not marked in the figure) is arranged outside the reaction shell 201 and used for cooling the accommodating cavity, so that the reaction rate of the reaction gas is improved, and the graphene with excellent performance is obtained. The cooling assembly includes: a cooling housing 208, a coolant inlet line 206 and a coolant return line 207. The cooling shell 208 is sleeved outside the reaction shell 201 and forms a sealed cooling area 209 with the reaction shell 201, the cooling liquid input pipe 206 is communicated with the cooling shell 208 and extends into the cooling area 209, the cooling liquid return pipe 207 is communicated with the cooling shell 208 and extends into the cooling area 209, and the cooling liquid input pipe 206 and the cooling liquid return pipe 207 are both sleeved with hydraulic valves for controlling the flow of cooling liquid.
Specifically, the reaction shell 201 and the cooling shell 208 may be, for example, spherical structures or square structures, and the spherical structures are favorable for uniform pressure distribution of the gas and the cooling liquid in the accommodating cavity, so as to increase the stressed areas of the gas and the reaction shell 201, the cooling liquid and the cooling shell 208, and thus reduce the stress on the reaction shell 201 and the cooling shell 208.
Specifically, referring to fig. 3 and 4, input wires (not shown) connected to the first plasma electrode 211, the second plasma electrode 212, the first electric field electrode 213, and the second electric field electrode 214 close to the reaction housing are all sleeved with a waterproof jacket 216 in the cooling region 209 and extend out of the cooling housing 208, so as to prevent the input wires from contacting with the cooling liquid and avoid the danger caused by electric sparks due to short circuit of the electrodes.
Preferably, referring to fig. 2 and 5, the graphene preparation apparatus 200 further includes: a first temperature sensor 220, a second temperature sensor 221, and a display assembly 222. The first temperature sensor 220 is disposed in the accommodating cavity for detecting the temperature of the reaction region 215, the second temperature sensor 221 is disposed in the accommodating cavity for detecting the temperature of the region between the reaction housing 201 and the heating element 210, and the display element 222 is connected to the first temperature sensor 220 and located outside the reaction housing 201.
Specifically, the using process of the graphene preparation apparatus 200 for preparing 2 to 5 layers of graphene includes, for example: the heating assembly 210 is used to heat the reaction region 215 to 3500-3800K (3226.85-3526.85 ℃) and inert gas is input into the holding chamber through the protective gas input pipe 203, so that the pressure of the holding chamber is 1.2-1.5MPa (i.e. the pressure in the reaction shell 201 is 1.2-1.5 MPa). Methane and/or acetylene gas is input into the reaction region 215 through the reaction gas input pipe 202, the graphene material is output to the outside of the reaction housing 201 through the graphene output pipe 204, and hydrogen is discharged through the gas discharge pipe 205. When the heating assembly 210 includes the plasma electrode module and the electric field electrode module, the current introduced by the plasma module is between 70 and 130A, and when the graphene preparation apparatus 200 further includes the cooling assembly, the cooling temperature of the cooling assembly is between 50 and 70 ℃.
Specifically, the graphene prepared by the graphene preparation device can be applied to the fields of water purification, air purification, medical treatment and clothing.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A preparation device of graphene is characterized by comprising:
a reaction housing having a sealed containment chamber;
the heating assembly is arranged in the accommodating cavity and forms a reaction area in the accommodating cavity;
the reaction gas input pipe is communicated with the reaction shell and extends into the reaction area;
the protective gas input pipe is communicated with the reaction shell and extends into the accommodating cavity;
the graphene output pipe is communicated with the reaction shell, and a pipe orifice of the graphene output pipe is opposite to the reaction area;
and the gas discharge pipe is communicated with the reaction shell and extends into the accommodating cavity.
2. The graphene manufacturing apparatus according to claim 1, wherein the heating assembly includes a plasma electrode module and an electric field electrode module; the plasma electrode module generates a plasma arc under the action of an electromagnetic field generated by the electric field electrode module;
wherein the plasma electrode module and the electric field electrode module form the reaction region.
3. The apparatus for preparing graphene according to claim 2,
the electric field electrode module includes: a first electric field electrode and a second electric field electrode; the two are oppositely arranged and provided with a gap;
the plasma electrode module includes: and the pairs of plasma electrodes are respectively oppositely arranged between the first electric field electrode and the second electric field electrode, and intervals are respectively arranged between each pair of plasma electrodes.
4. The apparatus according to claim 1, wherein the gas outlet pipe is disposed at a top end of the reaction housing, and the graphene outlet pipe is disposed at an opposite bottom end of the reaction housing.
5. The apparatus for preparing graphene according to claim 1, further comprising:
and the cooling assembly is arranged outside the reaction shell.
6. The apparatus of claim 5, wherein the cooling assembly comprises:
the cooling shell is sleeved outside the reaction shell and forms a sealed cooling area with the reaction shell;
the cooling liquid input pipe is communicated with the cooling shell and extends into the cooling area;
and the cooling liquid return pipe is communicated with the cooling shell and extends into the cooling area.
7. The apparatus for preparing graphene according to claim 1, further comprising:
the first temperature sensor is arranged in the accommodating cavity and used for detecting the temperature of the reaction area;
the second temperature sensor is arranged in the accommodating cavity and used for detecting the temperature of the area between the reaction shell and the heating assembly;
and the display component is connected with the first temperature sensor and is positioned outside the reaction shell.
8. Use of the apparatus for preparing graphene according to any one of claims 1 to 7,
using the preparation device for preparing 2-5 layers of graphene materials;
wherein the reaction zone is heated to 3500-3800K by the heating assembly; inert gas is input into the accommodating cavity through the protective gas input pipe, so that the pressure of the accommodating cavity is 1.2-1.5 MPa; inputting methane and/or acetylene gas into the reaction area through the reaction gas input pipe; outputting the graphene material to the outside of the reaction shell through the graphene output pipe; discharging hydrogen gas through the gas discharge pipe.
9. The use of claim 8, wherein the heating assembly comprises the plasma electrode module and the electric field electrode module; the current passed by the plasma module is between 70 and 130A.
10. Use according to claim 8, wherein the cooling temperature of the cooling assembly is between 50 and 70 ℃ when the preparation device further comprises the cooling assembly.
CN202010941296.2A 2020-09-09 2020-09-09 Preparation device and application of graphene Pending CN112028059A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112010292A (en) * 2020-09-09 2020-12-01 宁波中冶电子科技有限公司 Preparation method and application of graphene material
CN114620716A (en) * 2022-03-25 2022-06-14 西南交通大学 Fluorinated graphene and preparation method and application thereof

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CN104773725A (en) * 2015-04-09 2015-07-15 厦门大学 Method for preparing graphene by using low-temperature plasmas
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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN112010292A (en) * 2020-09-09 2020-12-01 宁波中冶电子科技有限公司 Preparation method and application of graphene material
CN114620716A (en) * 2022-03-25 2022-06-14 西南交通大学 Fluorinated graphene and preparation method and application thereof
CN114620716B (en) * 2022-03-25 2023-02-28 西南交通大学 Fluorinated graphene and preparation method and application thereof

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