CN110155994B - Device and method for directly preparing composite patterned graphene - Google Patents
Device and method for directly preparing composite patterned graphene Download PDFInfo
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- CN110155994B CN110155994B CN201910272380.7A CN201910272380A CN110155994B CN 110155994 B CN110155994 B CN 110155994B CN 201910272380 A CN201910272380 A CN 201910272380A CN 110155994 B CN110155994 B CN 110155994B
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- C01B32/186—Preparation by chemical vapour deposition [CVD]
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Abstract
The invention provides a device and a method for directly preparing composite patterned graphene, wherein the device comprises a reaction chamber, a heating device and a laser, wherein at least 2 air inlet devices are arranged in the tangential direction of the reaction chamber, and an exhaust port is arranged at the bottom of the reaction chamber and used for generating ascending spiral circulating airflow and descending radial airflow; the radial gas flow is discharged from a gas outlet; a heating device is arranged on the radial airflow path in the reaction chamber and used for enabling graphene to grow; the laser is used for generating laser beams to enable the grown graphene film to generate composite patterns. The invention does not need to vacuumize the closed container, thus effectively saving time; meanwhile, methane and hydrogen can form circulating flow in the device, so that sufficient gaseous carbon source on the metal substrate is ensured; and the composite patterned graphene film can be prepared.
Description
Technical Field
The invention relates to the field of graphene preparation, in particular to a device and a method for directly preparing composite patterned graphene.
Background
The graphene is a hexagonal honeycomb two-dimensional crystal formed by single-layer carbon atoms based on sp2 hybridization, and has excellent electrical, optical and mechanical properties. The chemical vapor deposition method is one of effective ways to obtain high-quality graphene and is also one of methods which can realize industrial production at present.
In the existing chemical vapor deposition method for preparing graphene, gaseous carbon sources such as methane and acetylene are decomposed at high temperature and dehydrogenated under the catalytic action of a substrate to form carbon-containing active groups, and when the carbon-containing active groups are accumulated on the substrate to reach a certain concentration, nucleation growth is carried out on the surface of the substrate to form graphene. Hydrogen is used as a protective gas, and metal such as copper foil, nickel foil and the like is used as a substrate. But is very time consuming for the closed container to draw a vacuum.
Since the graphene prepared by the chemical vapor deposition method is a large-area continuous structure, how to accurately and quickly obtain a required graphene pattern in the preparation process of a graphene device becomes one of the restricting factors for the development of the graphene device. The existing graphene patterning methods mainly fall into two categories:
(1) And selecting and removing the existing graphene to obtain the patterned graphene. The most common of such methods is photolithographic masking, but different micro-patterns often require different masks, which is inefficient. And the graphene film can be damaged due to the adhesion of the mask plate and the graphene film in the graphene transfer process. There is therefore a great need for a maskless method that can be used to fabricate graphene micropatterns.
(2) And directly scanning a pattern on the graphene film by using laser. The method is simple, efficient and low in pollution, but is limited to preparation of single-layer graphene patterns.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a device and a method for directly preparing composite patterned graphene, wherein a closed container is not required to be vacuumized, so that the time is effectively saved; meanwhile, methane and hydrogen can form circulating flow in the device, so that sufficient and sufficient gaseous carbon source on the metal substrate is ensured; and the composite patterned graphene film can be prepared.
The present invention achieves the above-described object by the following technical means.
A device for directly preparing composite patterned graphene comprises a reaction chamber, a heating device and a laser, wherein at least 2 air inlet devices are arranged in the tangential direction of the reaction chamber, and an air outlet is formed in the bottom of the reaction chamber and used for generating ascending spiral circulating air flow and descending radial air flow; the radial gas flow is discharged from a gas outlet; a heating device is arranged on the radial airflow path in the reaction chamber and used for enabling graphene to grow; the laser is used for generating laser beams to enable the grown graphene film to generate composite patterns.
Furthermore, the upper part of the reaction chamber is in a frustum shape, and the lower part of the reaction chamber is in a cylindrical shape; the cylindrical surface is provided with at least 2 air inlet devices in the tangential direction.
The gas mixing chamber is communicated with the exhaust port, and the gas mixing chamber is communicated with each gas inlet device through a gas pump.
Furthermore, a transparent sample inlet is hermetically arranged at the top of the reaction chamber, and the laser beam is injected into the reaction chamber through the transparent sample inlet.
Further, the heating device comprises a plurality of steel needles and heating wires, the steel needles are uniformly distributed to form a lattice type heating area, a gap between every two adjacent steel needles is filled with a high-temperature-resistant heat insulation material, the surfaces of the steel needles are wound with the heating wires, and the heating devices are used for heating different areas by controlling the state of each heating wire.
Furthermore, a lifting working platform is arranged at the bottom of the heating device.
Further, the air conditioner also comprises a main air inlet valve, an exhaust valve and a secondary air inlet valve; the air inlet device is provided with a main air inlet valve, an outlet of the air mixing chamber is provided with an exhaust valve, and a secondary air inlet valve is arranged between the air mixing chamber and each air inlet device.
A method for directly preparing composite patterned graphene comprises the following steps:
evacuating the air in the reaction chamber: opening a main air inlet valve and an exhaust valve for exhausting air in the reaction chamber;
forming an internal circulation airflow: closing the exhaust valve, starting the air pump, and enabling the interior of the reaction chamber to generate ascending spiral circulating airflow and descending radial airflow;
heating of the metal substrate: by controlling the work of each heating wire, the temperatures of the metal substrates in different areas are inconsistent, so that the growth of graphene in different metal substrate areas is different, and single-layer refined patterns are realized;
laser scanning: and (3) ablating the pattern again on the surface of the original single-layer refined pattern by using a laser beam to generate a composite pattern.
Further, the heating temperature of the electric heating wire is controlled to be 300-500 ℃.
Further, the method also comprises the following steps:
and (3) rapid cooling: and closing the electric heating wire, closing the secondary air inlet valve, and opening at least one main air inlet valve to rapidly cool the metal substrate under the action of air flow.
The invention has the beneficial effects that:
1. according to the device and the method for directly preparing the composite patterned graphene, the closed container is not required to be vacuumized, so that the time is effectively saved; meanwhile, methane and hydrogen can form circulating flow in the device, so that sufficient and sufficient gaseous carbon source on the metal substrate is ensured; and the composite patterned graphene film can be prepared.
2. According to the device and the method for directly preparing the composite patterned graphene, disclosed by the invention, the power-on and power-off of each area are effectively controlled by controlling the levels of the positive electrode and the negative electrode of the electric heating wire on each point array, so that the heating of different areas is realized, and the preparation of a single-layer refined pattern on a graphene film is realized; the patterning is realized by controlling different ablation paths of the laser on the surface of the graphene film, and finally, the composite patterning effect is achieved.
Drawings
Fig. 1 is a structural diagram of an apparatus for directly preparing composite patterned graphene according to the present invention.
Fig. 2 is a cross-sectional view of an apparatus for directly preparing composite patterned graphene according to the present invention.
Fig. 3 is a schematic view of the gas flow path according to the present invention.
Fig. 4 is a schematic view of the lattice heater of the present invention.
FIG. 5 is a Fluent simulation trace diagram according to the present invention.
FIG. 6 is a velocity vector diagram on the Fluent simulation profile of the present invention.
In the figure:
1-a reaction chamber; 2-a gaseous carbon source inlet; 3-hydrogen inlet; 41-exhaust port; 42-gas mixing chamber exhaust; 51-a first vent pipe; 52-a second vent; 61-a first main inlet valve; 62-a second main intake valve; 63-first intake valve; 64-a second intake valve; 65-exhaust valves; 71-a first air pump; 72-a second air pump; 8-a gas mixing chamber; 9-a workbench; 10-a height adjustment mechanism; 11-a heating device; 111-steel needle; 112-heating wires; 113-high temperature resistant insulation; 12-a transparent sample inlet; 13-a laser; 14-a methane gas bottle; 15-hydrogen gas cylinder; 16-a filter screen.
Detailed Description
The invention will be further described with reference to the following figures and specific examples, without limiting the scope of the invention thereto.
As shown in fig. 1, 2 and 3, the apparatus for directly preparing composite patterned graphene according to the present invention includes a reaction chamber 1, a heating device 11 and a laser 14; the reaction chamber 1 adopts a vertical conical cylinder cavity, the upper part of the cylinder is a cone, and the lower part of the cylinder is a cylinder. The left side and the right side of the cylinder in the tangential direction are respectively provided with a gas inlet pipe which is a gaseous carbon source inlet 2 and a hydrogen inlet 3, and the gaseous carbon source inlet 2 is communicated with a methane gas bottle 14; the hydrogen inlet 3 is communicated with a hydrogen cylinder 15; a first main air inlet valve 61 is arranged between the gaseous carbon source air inlet 2 and the methane gas bottle 14; a second main air inlet valve 62 is arranged between the hydrogen inlet 3 and the hydrogen cylinder 15; the bottom of the reaction chamber 1 is provided with an exhaust port 41; the exhaust port 41 is connected with the gas mixing chamber 8, and a first vent pipe 51, a second vent pipe 52 and a gas mixing chamber exhaust port 42 are arranged on the gas mixing chamber 8; the first breather pipe 51 is used for communicating the gas mixing chamber 8 with the gaseous carbon source inlet 2; the second vent pipe 52 is used for communicating the gas mixing chamber 8 with the hydrogen gas inlet 3; the first breather pipe 51 is provided with a first air pump 71 and a first air inlet valve 63; the second vent pipe 52 is provided with a second air pump 72 and a second secondary air inlet valve 64; the gas mixing chamber 8 is provided with a gas discharge valve 65. When in air intake, the first main air inlet valve 61, the second main air inlet valve 62 and the exhaust valve 65 are opened, the air flow speed of two kinds of air is set, and the air is introduced for a certain time to exhaust the air in the conical reaction chamber 1; then closing the exhaust valve 65, continuing to introduce methane and hydrogen for a certain time, and closing the first main intake valve 61 and the second main intake valve 62; the first air pump 71 and the second air pump 72 are activated to circulate air throughout the intercommunicating apparatus. The air flow changes from linear motion to circular motion in the device, and the rotating air flow spirally flows upwards along the wall cylinder towards the cone. The rotating and rising outer cyclone air flow continuously flows into the central part of the separator in the rising process to form centripetal radial air flow, and the centripetal radial air flow forms a rotating and downward inner cyclone. The two gases can be effectively and fully circulated in the device to ensure that the gaseous carbon source on the metal substrate is sufficient.
The center of the interior of the reaction chamber 1 is provided with a workbench 9, and the workbench is connected with the bottom of the hollow cavity through a height adjusting mechanism 10. Placing heating device 11 on workstation 9, as shown in fig. 4, heating device 11 includes a plurality of steel needles 111 and heater strip 112, and a plurality of steel needle 111 equipartition becomes dot matrix heating region, and is adjacent the clearance between steel needle 111 is filled with high temperature resistant insulation material, arbitrary steel needle 111 surface winding heater strip 112, through controlling every the state of heater strip 112 for realize the heating in different regions. A lattice type heating area is composed of 128 x 128 steel needles 111, and carbon fiber heating wires 112 are wound on the steel needles 111. Each steel needle 111 gap is filled with high temperature resistant heat insulation material 113, each heating wire 112 is connected with a circuit in a certain mode, the whole single chip microcomputer is used as a core, the level of the anode and the level of the cathode of each heating wire 112 are controlled through programming, the electrification and the outage of each heating wire can be effectively controlled, and the heating of different areas is realized. A metal substrate such as nickel foil or copper foil is used as a growth substrate and is arranged on the electric heating wire. Different areas of the nickel foil are heated differently, so that the conditions of thermal decomposition of the gaseous carbon source are different, the growth of graphene in different areas is different, and the effect of single-layer refined patterns is achieved. The laser 13 is positioned right above the whole device, and patterns are formed through a laser ablation path, so that the grown graphene film can achieve a composite patterning effect. The high-temperature resistant heat-insulating material is a ceramic material. And a filter screen 16 is arranged between the exhaust port 41 and the gas mixing chamber 8 and is used for filtering impurities.
The top of the reaction chamber 1 is provided with a transparent quartz glass sample inlet 12, and a sample is taken from the position. The height of the workbench relative to the bottom of the device can be adjusted by the workbench height adjusting mechanism 10, so that the growth condition of graphene can be compared.
FIG. 5 is a Fluent simulation trace diagram according to the present invention. The aeration speeds of the two air vents are respectively 200mm/s and 400mm/s, and the mixed gas spirally rises in the device and then rotates downwards to form an internal rotational flow so as to ensure that the two gases are sufficiently contacted and mixed in the device.
FIG. 6 is a velocity vector diagram on the Fluent simulation profile of the present invention. It can be seen that in the cross section, the outer spiral air flow velocity is high and the inner spiral air flow velocity is low.
A method for directly preparing composite patterned graphene comprises the following steps:
s01: placing the sample on a workbench and fixing;
s02: opening the first main air inlet valve 61, the second main air inlet valve 62 and the exhaust valve 65, setting the flow speed of two gases, and introducing the gases for a certain time to exhaust the air in the conical reaction chamber 1;
s03: opening the first and second intake valves 63 and 64 for a certain time for exhausting the air in the first and second air pipes 51 and 52;
s04: closing the exhaust valve 65, and closing the first main intake valve 61 and the second main intake valve 62 after continuing to introduce the methane and the hydrogen for a certain time;
s05: the first air pump 71 and the second air pump 72 are activated to circulate the air throughout the intercommunicating apparatus. The air flow changes from linear motion to circular motion in the device, and the rotating air flow spirally flows upwards along the wall cylinder towards the cone. The rotating and rising outer cyclone air flow continuously flows into the central part of the separator in the rising process to form centripetal radial air flow, and the centripetal radial air flow forms a rotating and downward inner cyclone. The two gases can be effectively and fully circulated in the device to ensure that the gaseous carbon source on the metal substrate is sufficient.
S06: the electrical level of the anode and the cathode of the electric heating wire 112 on each dot matrix is controlled by programming the single chip microcomputer, so that the electrification and the outage of each area are effectively controlled, the heating of different areas is realized, and the heating temperature of the carbon fiber electric heating wire is controlled to be 300-500 ℃;
s07: starting the laser 13, adjusting the laser power density, and continuing for a certain time; the laser is a solid laser, the emission wavelength of the laser is 532nm, and the power of the laser is 10W;
s08: closing the heating device 11, closing the first secondary air inlet valve 63 and the second secondary air inlet valve 64, and opening the second main air inlet valve 62 to allow the nickel foil to be rapidly cooled at a certain speed under the hydrogen flow;
s09: and adjusting the scanning speed of a laser, heating and patterning at the scanning speed of 2000-3000mm/s, ablating a pattern on the surface of the graphene film according to a scanning path, and ablating the pattern on the surface of the original single-layer refined pattern again to achieve a composite patterning effect.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (10)
1. The device for directly preparing the composite patterned graphene is characterized by comprising a reaction chamber (1), a heating device (11) and a laser (14), wherein at least 2 air inlet devices are arranged in the tangential direction of the reaction chamber, and an air outlet (41) is formed in the bottom of the reaction chamber (1) and used for generating ascending spiral circulating airflow and descending radial airflow; the radial gas flow is discharged from a gas outlet (41); a heating device (11) is arranged on the radial airflow path in the reaction chamber (1), and the heating device (11) is used for enabling graphene to grow; the laser (14) is used for generating laser beams to enable the grown graphene film to generate composite patterns.
2. The apparatus for directly preparing composite patterned graphene according to claim 1, wherein the upper portion of the reaction chamber (1) has a frustum shape, and the lower portion of the reaction chamber (1) has a cylindrical shape; the cylindrical surface is provided with at least 2 air inlet devices in the tangential direction.
3. The apparatus for directly preparing composite patterned graphene according to claim 1, further comprising a gas mixing chamber (8), wherein the gas mixing chamber (8) is communicated with the gas outlet (41), and the gas mixing chamber (8) is communicated with each gas inlet device through a gas pump (71, 72).
4. The apparatus for directly preparing composite patterned graphene according to claim 2, wherein a transparent injection port (12) is hermetically installed on the top of the reaction chamber (1), and the laser beam is injected into the reaction chamber (1) through the transparent injection port (12).
5. The apparatus for directly preparing composite patterned graphene according to claim 3, wherein the heating apparatus (11) comprises a plurality of steel needles (111) and heating wires (112), the plurality of steel needles (111) are uniformly distributed into a lattice type heating region, a gap between adjacent steel needles (111) is filled with a high temperature resistant heat insulating material, and the heating wires (112) are wound on the surface of any one of the steel needles (111) for realizing heating of different regions by controlling the state of each heating wire (112).
6. The apparatus for directly preparing composite patterned graphene according to claim 5, wherein a liftable working platform (9) is arranged at the bottom of the heating apparatus (11).
7. The apparatus for directly preparing composite patterned graphene according to claim 5, further comprising a main intake valve (61, 62), an exhaust valve (65), and a sub-intake valve (63, 64); be equipped with main admission valve (61, 62) on the air inlet unit, gas mixing chamber (8) exit installation discharge valve (65), gas mixing chamber (8) and every install time admission valve (63, 64) between the air inlet unit.
8. A method for directly preparing composite patterned graphene by using the apparatus for directly preparing composite patterned graphene according to claim 7, comprising the following steps:
evacuating the air inside the reaction chamber (1): opening main intake valves (61, 62) and exhaust valves (65) for exhausting air in the reaction chamber (1);
forming an internal circulation airflow: closing the exhaust valve (65), and starting the air pumps (71, 72) to generate ascending spiral circulating airflow and descending radial airflow in the reaction chamber (1);
heating of the metal substrate: by controlling the work of each heating wire (112), the temperatures of the metal bases in different areas are inconsistent, so that the graphene in different metal base areas grows differently, and a single-layer refined pattern is realized;
laser scanning: and (3) ablating the pattern again on the surface of the original single-layer refined pattern by using a laser beam to generate a composite pattern.
9. The method for directly preparing composite patterned graphene according to claim 8, wherein the heating temperature of the heating wire (112) is controlled to be 300-500 ℃.
10. The method for directly preparing composite patterned graphene according to claim 8, further comprising the steps of:
and (3) quick cooling: the heating wire (112) is closed, the secondary air inlet valves (63, 64) are closed, and at least one primary air inlet valve (61, 62) is opened, so that the metal substrate is rapidly cooled under the action of the air flow.
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| US5204145A (en) * | 1991-03-04 | 1993-04-20 | General Electric Company | Apparatus for producing diamonds by chemical vapor deposition and articles produced therefrom |
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