CN110155994A - A kind of device and method directly preparing composite patterning graphene - Google Patents
A kind of device and method directly preparing composite patterning graphene Download PDFInfo
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- CN110155994A CN110155994A CN201910272380.7A CN201910272380A CN110155994A CN 110155994 A CN110155994 A CN 110155994A CN 201910272380 A CN201910272380 A CN 201910272380A CN 110155994 A CN110155994 A CN 110155994A
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- 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
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- 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
- C01B32/194—After-treatment
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Abstract
The present invention provides the device and methods that one kind directly prepares composite patterning graphene, including reaction chamber, heating device and laser, the reaction chamber tangential direction is at least provided with 2 inlet ducts, the reaction chamber bottom is equipped with exhaust outlet, for generating the radial air flow of the spiral circulation air-flow and decline that rise；The radial air flow is discharged by exhaust outlet；The indoor radial air flow path is reacted equipped with heating device, and the heating device is for making graphene growth；The laser, which is used to generate laser beam, makes the graphene film of growth generate composite pattern.The present invention does not have to closed container extracting vacuum, effectively saves the time；Methane and hydrogen can be made to be formed in the device simultaneously to circulate, guarantee that the gaseous carbon source in metallic substrates is abundant enough；And composite patterning graphene film can be prepared.
Description
Technical field
The present invention relates to field of preparation of graphene, in particular to a kind of device for directly preparing composite patterning graphene and
Method.
Background technique
The hexagon cellular shape two dimensional crystal that graphene is made of single layer of carbon atom based on sp2 hydridization has very excellent
Electricity, optics and mechanical property.Chemical vapour deposition technique is one of the effective way for obtaining high-quality graphene, and at present
One of the method that industrialization production may be implemented.
Existing process for preparing graphenes by chemical vapour deposition is decomposed under the high temperature conditions using gaseous carbon sources such as methane, acetylene
And dehydrogenation forms carbonaceous active group under substrate catalytic action, when carbonaceous active group has reached a certain concentration on substrate
When just substrate surface forming core grow, formed graphene.Using hydrogen as protective gas, using metals such as copper foil, nickel foils as substrate.
But it is very time-consuming for closed container extracts vacuum.
Since the graphene of chemical vapour deposition technique preparation is the continuous structure of large area, so in the system of graphene device
During standby, how accurately quickly to obtain required graphene pattern, become restraining factors that graphene device develops it
One.The method of existing graphene pattern is mainly divided to two classes:
(1) constituency is carried out to existing graphene to remove to obtain patterned Graphene.Most commonly seen in such method is light
Mask means is carved, but different micro- patterns usually requires different mask plates, efficiency is lower.And in graphene transfer process by
It will cause the destruction of graphene film in the adhesion of mask plate and graphene film.Therefore being highly desirable to can be used for manufacturing graphene
The mask-free method of micro- pattern.
(2) pattern is directly scanned on graphene film using laser.It is small that such method is simple and efficient pollution, but limits to
In preparing single-layer graphene pattern.
Summary of the invention
For the deficiencies in the prior art, the present invention provides the dresses that one kind directly prepares composite patterning graphene
It sets and method without closed container is extracted vacuum effectively saves the time；Methane and hydrogen can be made to be formed in the device simultaneously
It circulates, guarantees that the gaseous carbon source in metallic substrates is abundant enough；And it is thin to prepare composite patterning graphene
Film.
The present invention achieves the above technical objects by the following technical means.
A kind of device directly preparing composite patterning graphene, including reaction chamber, heating device and laser, it is described anti-
Answer room tangential direction at least provided with 2 inlet ducts, the reaction chamber bottom is equipped with exhaust outlet, follows for generating the spiral risen
The radial air flow of ring air-flow and decline；The radial air flow is discharged by exhaust outlet；It reacts on the indoor radial air flow path
Equipped with heating device, the heating device is for making graphene growth；The laser, which is used to generate laser beam, makes the stone of growth
Black alkene film generates composite pattern.
Further, the top of the reaction chamber is taper type, and the lower part of the reaction chamber is divided into cylinder；The cylinder
Surface tangential direction is equipped at least two inlet duct.
It further, further include gas mixer chamber, the gas mixer chamber is connected to exhaust outlet, the gas mixer chamber and every
It is connected between a inlet duct by air pump.
Further, transparent injection port is installed in sealing at the top of the reaction chamber, and the laser beam is injected by transparent injection port
In reaction chamber.
Further, the heating device includes several steel needles and heater strip, and several steel needles are uniformly distributed to be heated at dot matrix
Region, the gap filling high temperature resistant heat insulation material between the adjacent steel needle, heating wire described in any steel needle surface wrap,
By controlling the state of each heating wire, for realizing the heating of different zones.
Further, the heating device bottom is equipped with lifting working platform.
It further, further include master air suction valve, exhaust valve and secondary intake valve；The inlet duct is equipped with master air suction valve, institute
Gas mixer chamber exit installation exhaust valve is stated, time air inlet is installed between the gas mixer chamber and each inlet duct
Valve.
A method of composite patterning graphene is directly prepared, is included the following steps:
Emptying reaction room air: opening master air suction valve and exhaust valve, for that will react room air discharge；
Circulating current in being formed: closing exhaust valve, and booster air pump makes to generate the spiral circulation air-flow risen inside reaction chamber
With the radial air flow of decline；
The heating of metallic substrates: the work by controlling each heating wire makes the metallic substrates temperature of different zones
It is inconsistent, cause the graphene growth of different metal basal region different, realizes that single layer refines pattern；
Laser scanning: patterned surfaces ablation pattern again is refined in former single layer by laser beam, generates composite pattern.
Further, electrothermal wire heating's temperature control is 300-500 DEG C.
Further, further include following steps:
It is quickly cooled down: closing heating wire, close time intake valve, open at least one master air suction valve, allow metallic substrates in gas
Stream effect is lower to be quickly cooled down.
The beneficial effects of the present invention are:
1. the device and method of the present invention for directly preparing composite patterning graphene, without extracting closed container
Vacuum effectively saves the time；Methane and hydrogen can be made to be formed in the device simultaneously to circulate, guarantee the gas in metallic substrates
State carbon source is abundant enough；And composite patterning graphene film can be prepared.
2. the device and method of the present invention for directly preparing composite patterning graphene, by each dot matrix of control
Heating wire positive electrode and negative electrode level, effectively control the energization and power-off in each region, realize the heating of different zones, from
And it realizes and prepares single layer fining pattern on graphene film；By control laser on graphene film surface difference ablation road
Diameter realizes patterning, is finally reached composite patterning effect.
Detailed description of the invention
Fig. 1 is the structure drawing of device of the present invention for directly preparing composite patterning graphene.
Fig. 2 is the device cross-sectional view of the present invention for directly preparing composite patterning graphene.
Fig. 3 is air flow path schematic diagram of the present invention.
Fig. 4 is dot matrix heater schematic diagram of the present invention.
Fig. 5 is that Fluent of the present invention emulates trace diagram.
Speed vector figure on the Fluent emulation section of the present invention of the position Fig. 6.
In figure:
1- reaction chamber；2- gaseous carbon source air inlet；3- hydrogen inlet；41- exhaust outlet；42- gas mixer chamber exhaust outlet；
The first snorkel of 51-；The second snorkel of 52-；The first master air suction valve of 61-；The second master air suction valve of 62-；63- first time intake valve；
Second of intake valve of 64-；65- exhaust valve；The first air pump of 71-；The second air pump of 72-；8- gas mixer chamber；9- workbench；10- high
Spend regulating mechanism；11- heating device；111- steel needle；112- heater strip；113- high temperature resistant heat insulation material；The transparent injection port of 12-；
13- laser；14- methane gas bottle；15- hydrogen cylinder；16- strainer.
Specific embodiment
Present invention will be further explained with reference to the attached drawings and specific examples, but protection scope of the present invention is simultaneously
It is without being limited thereto.
As shown in Figure 1, Figure 2 and Figure 3, the device of the present invention for directly preparing composite patterning graphene, including it is anti-
Answer room 1, heating device 11 and laser 14；The reaction chamber 1 uses upright conical barrel chamber body, and the top of cylinder is divided into circular cone
The lower part of body, cylinder is divided into cylindrical body.Cylindrical body tangential direction is each side equipped with a gas inlet pipe, respectively gaseous carbon
Source air inlet 2 and hydrogen inlet 3, the gaseous carbon source air inlet 2 are connected to methane gas bottle 14；The hydrogen inlet 3
It is connected to hydrogen cylinder 15；First master air suction valve 61 is installed between the gaseous carbon source air inlet 2 and methane gas bottle 14；The hydrogen
Second master air suction valve 62 is installed between gas air inlet 3 and hydrogen cylinder 15；1 bottom of reaction chamber is equipped with exhaust outlet 41；Exhaust outlet
41 are connected with gas mixer chamber 8, and the gas mixer chamber 8 is equipped with the first snorkel 51, the second snorkel 52 and gas mixing
Room exhaust outlet 42；First snorkel 51 is for being connected to gas mixer chamber 8 and gaseous carbon source air inlet 2；Second ventilation
Pipe 52 is for being connected to gas mixer chamber 8 and hydrogen inlet 3；First air pump 71 and first time are installed on first snorkel 51
Intake valve 63；Second air pump 72 and second of intake valve 64 are installed on second snorkel 52；The row of installation on gas mixer chamber 8
Air valve 65.The first master air suction valve 61, the second master air suction valve 62 and exhaust valve 65 are opened when air inlet, and two kinds of gas flows are set
Speed is passed through gas certain time with the air in venting cone reaction chamber 1；Exhaust valve 65 is closed later, continues to be passed through first
Alkane and hydrogen close the first master air suction valve 61 and the second master air suction valve 62 after a certain period of time；Start the first air pump 71 and the second air pump
72, so that gas is formed circulation in entire interworking unit.Air-flow becomes circular motion, swirling eddy from linear motion in the device
It is twist flowed up towards cone along wall cylinder.The outer rotational gas flow risen is rotated, constantly to separation in uphill process
The central part of device flows into, and forms centripetal radial air flow, this fraction, which constitutes, rotates downward inward eddy.It can be effective
Recycle two kinds of gases sufficiently in the device, to guarantee that the gaseous carbon source in metallic substrates is abundant enough.
1 inside center of reaction chamber has a workbench 9, and the workbench passes through height adjustment mechanism 10 and hollow cavity bottom
It is connected.Heating device 11 is placed on the workbench 9, as shown in figure 4, the heating device 11 includes several steel needles 111 and adds
Heated filament 112, several steel needles 111 are uniformly distributed at dot matrix heating region, the resistance to height of gap filling between the adjacent steel needle 111
Warm heat-barrier material, heating wire 112 described in any 111 surface wrap of steel needle pass through the shape of each heating wire 112 of control
State, for realizing the heating of different zones.Dot matrix heating region is formed by 128 × 128 steel needles 111, is wound on steel needle 111
Carbon fibre electrothermal wire 112.Each 111 gap filling high temperature resistant heat insulation material 113 of steel needle, each heating wire 112 is according to certain side
Formula connection line, it is whole using single-chip microcontroller as core, it, can by the level of the positive electrode and negative electrode of each heating wire 112 of programming Control
Effectively to control the energization and power-off of each heating wire, the heating of different zones is realized.Using metallic substrates such as nickel foil or copper foils
As growth substrate, it is placed on heating wire.The heated difference of nickel foil different zones, thus gaseous carbon source by thermal decomposition situation not
Together, cause the graphene growth of different zones different, reach single layer fining pattern effect.Laser 13 is located at whole device
Surface forms pattern by laser ablation path, the graphene film of growth can be made to reach composite patterning effect.Resistance to height
Warm heat-barrier material is ceramic material.Strainer 16 is equipped between the exhaust outlet 41 and gas mixer chamber 8, for filtering sundries.
It is transparency silica glass injection port 12 at the top of the reaction chamber 1, takes sample from the position.The height of table
Height of the adjustable workbench of regulating mechanism 10 relative to bottom of device, compares the growing state of graphene.
Fig. 5 is that Fluent of the present invention emulates trace diagram.The draft speed of two blow vents is respectively 200mm/s and 400mm/
S, mixed gas rotates again after twist rising in the device is formed down inward eddy, to guarantee that two kinds of gases fill in the device
Tap touching mixing.
Fig. 6 is the speed vector figure on Fluent of the present invention emulation section.Outer ring helical flow on section as seen from the figure
Speed is high and inner ring helical flow speed is low.
A method of composite patterning graphene is directly prepared, is included the following steps:
S01: sample is put on workbench and is fixed；
S02: opening the first master air suction valve 61, the second master air suction valve 62 and exhaust valve 65, two kinds of gas flow speed be arranged,
Gas certain time is passed through with the air in venting cone reaction chamber 1；
S03: opening first time intake valve 63 and second of 64 certain time of intake valve, is used for 51 He of the first snorkel of venting
Air in second snorkel 52；
S04: closing exhaust valve 65, continues to be passed through methane and hydrogen and closes the first master air suction valve 61 and second after a certain period of time
Master air suction valve 62；
S05: the first air pump 71 of starting and the second air pump 72 make gas form circulation in entire interworking unit.Air-flow exists
Circular motion is become from linear motion in device, swirling eddy is twist flowed up towards cone along wall cylinder.Rotation
The outer rotational gas flow risen constantly flows into the central part of separator in uphill process, forms centripetal radial air flow, this portion
Divide air-flow to constitute and rotates downward inward eddy.Two kinds of gases can be made sufficiently to recycle in the device, effectively to guarantee Metal Substrate
Gaseous carbon source on bottom is abundant enough.
S06: the level by controlling mcu programming the positive electrode and negative electrode of the heating wire 112 on each dot matrix, effectively
The energization and power-off in each region are controlled, to realize the heating of different zones, the control of carbon fibre electrothermal wire heating temperature is 300-
500℃；
S07: opening laser 13, adjusts laser power density, certain time；The laser is Solid State Laser
Device, launch wavelength 532nm, power 10W；
S08: closing heating device 11, closes first time intake valve 63 and second of intake valve 64, opens the second main air inlet
Valve 62 allows nickel foil to be quickly cooled down under hydrogen stream with certain speed；
S09: adjusting the scanning speed of laser, is heated and is patterned with 2000-3000mm/s scanning speed, is allowed to
Go out pattern according to scan path ablation on graphene film surface, ablation pattern reaches again in former single layer fining patterned surfaces
Composite patterning effect.
The embodiment is a preferred embodiment of the present invention, but present invention is not limited to the embodiments described above, not
In the case where substantive content of the invention, any conspicuous improvement that those skilled in the art can make, replacement
Or modification all belongs to the scope of protection of the present invention.
Claims (10)
1. the device that one kind directly prepares composite patterning graphene, which is characterized in that including reaction chamber (1), heating device
(11) it is equipped with laser (14), the reaction chamber tangential direction at least provided with 2 inlet ducts, reaction chamber (1) bottom
Exhaust outlet (41), for generating the radial air flow of the spiral circulation air-flow and decline that rise；The radial air flow is by exhaust outlet
(41) it is discharged；The radial air flow path in reaction chamber (1) is equipped with heating device (11), and the heating device (11) is used for
Make graphene growth；The laser (14), which is used to generate laser beam, makes the graphene film of growth generate composite pattern.
2. the device according to claim 1 for directly preparing composite patterning graphene, which is characterized in that the reaction chamber
(1) top is taper type, and the lower part of the reaction chamber (1) is divided into cylinder；The cylindrical surface tangential direction is equipped with extremely
Few 2 inlet ducts.
3. the device according to claim 1 for directly preparing composite patterning graphene, which is characterized in that further include gas
Mixing chamber (8), the gas mixer chamber (8) are connected to exhaust outlet (41), and the gas mixer chamber (8) and each air inlet fill
It is connected between setting by air pump (71,72).
4. the device according to claim 2 for directly preparing composite patterning graphene, which is characterized in that the reaction chamber
(1) transparent injection port (12) is installed in top sealing, and the laser beam is injected in reaction chamber (1) by transparent injection port (12).
5. the device according to claim 3 for directly preparing composite patterning graphene, which is characterized in that the heating dress
Setting (11) includes several steel needles (111) and heater strip (112), and several steel needles (111) are uniformly distributed at dot matrix heating region, phase
Gap filling high temperature resistant heat insulation material between the adjacent steel needle (111), electric heating described in any steel needle (111) surface wrap
Silk (112), by controlling the state of each heating wire (112), for realizing the heating of different zones.
6. the device according to claim 5 for directly preparing composite patterning graphene, which is characterized in that the heating dress
(11) bottom is set equipped with lifting working platform (9).
7. the device according to claim 5 for directly preparing composite patterning graphene, which is characterized in that further include it is main into
Air valve (61,62), exhaust valve (65) and time intake valve (63,64)；The inlet duct is equipped with master air suction valve (61,62), institute
Gas mixer chamber (8) exit installation exhaust valve (65) is stated, is pacified between the gas mixer chamber (8) and each inlet duct
Fill time intake valve (63,64).
8. it is a kind of directly prepared using the device for directly preparing composite patterning graphene as claimed in claim 7 it is composite patterning
The method of graphene, which comprises the steps of:
It empties reaction chamber (1) interior air: opening master air suction valve (61,62) and exhaust valve (65), be used for reaction chamber (1) interior air
Discharge；
Circulating current in being formed: closing exhaust valve (65), booster air pump (71,72), makes to generate the spiral shell risen inside reaction chamber (1)
Revolve the radial air flow of circulating current and decline；
The heating of metallic substrates: the work by controlling each heating wire (112) makes the metallic substrates temperature of different zones
It is inconsistent, cause the graphene growth of different metal basal region different, realizes that single layer refines pattern；
Laser scanning: patterned surfaces ablation pattern again is refined in former single layer by laser beam, generates composite pattern.
9. the method according to claim 8 for directly preparing composite patterning graphene, which is characterized in that the heating wire
(112) heating temperature control is 300-500 DEG C.
10. the method according to claim 8 for directly preparing composite patterning graphene, which is characterized in that further include as
Lower step:
It is quickly cooled down: closing heating wire (112), close time intake valve (63,64), open at least one master air suction valve (61,62),
Metallic substrates are allowed to be quickly cooled down under airflow function.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910272380.7A CN110155994B (en) | 2019-04-04 | 2019-04-04 | Device and method for directly preparing composite patterned graphene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910272380.7A CN110155994B (en) | 2019-04-04 | 2019-04-04 | Device and method for directly preparing composite patterned graphene |
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| Publication Number | Publication Date |
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| CN110155994A true CN110155994A (en) | 2019-08-23 |
| CN110155994B CN110155994B (en) | 2023-01-17 |
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Citations (8)
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| US2942043A (en) * | 1955-01-03 | 1960-06-21 | Hoechst Ag | Process for carrying out endothermic chemical reactions |
| US5204145A (en) * | 1991-03-04 | 1993-04-20 | General Electric Company | Apparatus for producing diamonds by chemical vapor deposition and articles produced therefrom |
| WO2012036537A2 (en) * | 2010-09-17 | 2012-03-22 | 한국과학기술원 | Apparatus and method for manufacturing graphene using a flash lamp or laser beam, and graphene manufactured by same |
| US20140205763A1 (en) * | 2013-01-22 | 2014-07-24 | Nutech Ventures | Growth of graphene films and graphene patterns |
| CN104264130A (en) * | 2014-09-25 | 2015-01-07 | 北矿磁材科技股份有限公司 | Preparation method and preparation device of graphene |
| CN105369347A (en) * | 2015-11-03 | 2016-03-02 | 电子科技大学 | Device and method for preparing large-area graphene single crystal by controlling nucleus formation |
| CN105399082A (en) * | 2015-07-22 | 2016-03-16 | 李雪松 | Chemical vapor deposition equipment and method for preparing graphene film |
| CN108545725A (en) * | 2018-05-14 | 2018-09-18 | 南京航空航天大学 | A kind of graphene preparation facilities and the method using the long graphene of device pattern metaplasia |
-
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Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2942043A (en) * | 1955-01-03 | 1960-06-21 | Hoechst Ag | Process for carrying out endothermic chemical reactions |
| US5204145A (en) * | 1991-03-04 | 1993-04-20 | General Electric Company | Apparatus for producing diamonds by chemical vapor deposition and articles produced therefrom |
| WO2012036537A2 (en) * | 2010-09-17 | 2012-03-22 | 한국과학기술원 | Apparatus and method for manufacturing graphene using a flash lamp or laser beam, and graphene manufactured by same |
| US20140205763A1 (en) * | 2013-01-22 | 2014-07-24 | Nutech Ventures | Growth of graphene films and graphene patterns |
| CN104264130A (en) * | 2014-09-25 | 2015-01-07 | 北矿磁材科技股份有限公司 | Preparation method and preparation device of graphene |
| CN105399082A (en) * | 2015-07-22 | 2016-03-16 | 李雪松 | Chemical vapor deposition equipment and method for preparing graphene film |
| CN105369347A (en) * | 2015-11-03 | 2016-03-02 | 电子科技大学 | Device and method for preparing large-area graphene single crystal by controlling nucleus formation |
| CN108545725A (en) * | 2018-05-14 | 2018-09-18 | 南京航空航天大学 | A kind of graphene preparation facilities and the method using the long graphene of device pattern metaplasia |
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